# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jian-Ping Lang' _publ_contact_author_email JPLANG@SUDA.EDU.CN _publ_section_title ; From trans-[(?5-C5Me5)2Mo2S2(?-S)2] to [(?5-C5Me5)2Mo2(?3-S)4(CuMeCN)2]2+ to [(?5-C5Me5)2Mo2(?3-S)4Cu2]-Based Polymeric and Dimeric Clusters: Syntheses, Structures and Enhanced Third-Order Nolinear Optical Performances ; loop_ _publ_author_name 'Jian-Ping Lang' 'Yang Chen' 'Ni-Ya Li' 'Hong-Xi Li' 'Zhi-Gang Ren' ; Ying-Lin Song ; 'Jun-Yi Yang' 'Yong Zhang' # Attachment 'JPLangCIF_revised_.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 679376' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H36 Cu2 Mo2 N2 S4, 2(Cl O4)' _chemical_formula_sum 'C24 H36 Cl2 Cu2 Mo2 N2 O8 S4' _chemical_formula_weight 998.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.678(3) _cell_length_b 21.782(4) _cell_length_c 14.036(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.39(3) _cell_angle_gamma 90.00 _cell_volume 3633.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 14353 _cell_measurement_theta_min 3.0957 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour Dark-red _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 2.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3018 _exptl_absorpt_correction_T_max 0.4308 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35034 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6633 _reflns_number_gt 6242 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+4.7085P] 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 6633 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 0.41053(2) 0.142779(11) 0.109175(18) 0.02281(8) Uani 1 1 d . . . Mo2 Mo 0.19474(2) 0.134035(11) 0.129268(19) 0.02251(8) Uani 1 1 d . . . Cu1 Cu 0.23262(4) 0.08345(2) -0.03539(3) 0.03896(12) Uani 1 1 d . . . Cu2 Cu 0.34419(4) 0.038364(19) 0.18688(4) 0.04174(12) Uani 1 1 d . . . S1 S 0.41883(8) 0.04768(4) 0.05346(7) 0.0397(2) Uani 1 1 d . . . S2 S 0.15551(8) 0.03655(4) 0.07700(7) 0.0402(2) Uani 1 1 d . . . S3 S 0.24157(6) 0.18483(3) 0.00334(5) 0.02565(16) Uani 1 1 d . . . S4 S 0.36992(6) 0.13317(3) 0.25813(6) 0.02690(17) Uani 1 1 d . . . N1 N 0.1837(3) 0.06741(14) -0.1785(2) 0.0424(7) Uani 1 1 d . . . N2 N 0.4190(3) -0.02211(15) 0.2862(3) 0.0529(8) Uani 1 1 d . . . C1 C 0.5181(2) 0.23127(14) 0.1645(2) 0.0295(7) Uani 1 1 d . . . C2 C 0.4962(3) 0.22696(16) 0.0583(2) 0.0329(7) Uani 1 1 d . . . C3 C 0.5502(3) 0.17297(18) 0.0405(3) 0.0377(8) Uani 1 1 d . . . C4 C 0.6069(3) 0.14472(16) 0.1358(3) 0.0348(8) Uani 1 1 d . . . C5 C 0.5868(2) 0.18024(15) 0.2126(2) 0.0303(7) Uani 1 1 d . . . C6 C 0.4867(3) 0.28337(16) 0.2189(3) 0.0406(8) Uani 1 1 d . . . H6A H 0.4658 0.2672 0.2751 0.061 Uiso 1 1 calc R . . H6B H 0.4229 0.3057 0.1715 0.061 Uiso 1 1 calc R . . H6C H 0.5510 0.3112 0.2459 0.061 Uiso 1 1 calc R . . C7 C 0.4393(3) 0.2748(2) -0.0185(3) 0.0514(10) Uani 1 1 d . . . H7A H 0.3822 0.2957 0.0021 0.077 Uiso 1 1 calc R . . H7B H 0.4032 0.2553 -0.0849 0.077 Uiso 1 1 calc R . . H7C H 0.4951 0.3047 -0.0231 0.077 Uiso 1 1 calc R . . C8 C 0.5537(4) 0.1517(2) -0.0600(3) 0.0614(12) Uani 1 1 d . . . H8A H 0.6152 0.1725 -0.0741 0.092 Uiso 1 1 calc R . . H8B H 0.4821 0.1615 -0.1137 0.092 Uiso 1 1 calc R . . H8C H 0.5660 0.1072 -0.0578 0.092 Uiso 1 1 calc R . . C9 C 0.6832(3) 0.0902(2) 0.1537(4) 0.0572(11) Uani 1 1 d . . . H9A H 0.7590 0.1037 0.1597 0.086 Uiso 1 1 calc R . . H9B H 0.6546 0.0616 0.0965 0.086 Uiso 1 1 calc R . . H9C H 0.6860 0.0696 0.2166 0.086 Uiso 1 1 calc R . . C10 C 0.6416(3) 0.17077(19) 0.3244(3) 0.0446(9) Uani 1 1 d . . . H10A H 0.6494 0.1267 0.3392 0.067 Uiso 1 1 calc R . . H10B H 0.5952 0.1894 0.3598 0.067 Uiso 1 1 calc R . . H10C H 0.7162 0.1900 0.3478 0.067 Uiso 1 1 calc R . . C11 C 0.1298(3) 0.21612(15) 0.2003(3) 0.0313(7) Uani 1 1 d . . . C12 C 0.0538(2) 0.20942(14) 0.0990(2) 0.0272(6) Uani 1 1 d . . . C13 C -0.0012(2) 0.15210(15) 0.0911(3) 0.0314(7) Uani 1 1 d . . . C14 C 0.0398(3) 0.12317(16) 0.1881(3) 0.0369(8) Uani 1 1 d . . . C15 C 0.1214(3) 0.16221(18) 0.2554(3) 0.0376(8) Uani 1 1 d . . . C16 C 0.1977(3) 0.27249(18) 0.2437(3) 0.0515(10) Uani 1 1 d . . . H16A H 0.2239 0.2911 0.1924 0.077 Uiso 1 1 calc R . . H16B H 0.2627 0.2612 0.3034 0.077 Uiso 1 1 calc R . . H16C H 0.1509 0.3020 0.2637 0.077 Uiso 1 1 calc R . . C17 C 0.0254(3) 0.25760(16) 0.0186(3) 0.0423(9) Uani 1 1 d . . . H17A H -0.0408 0.2805 0.0193 0.063 Uiso 1 1 calc R . . H17B H 0.0092 0.2382 -0.0480 0.063 Uiso 1 1 calc R . . H17C H 0.0893 0.2857 0.0317 0.063 Uiso 1 1 calc R . . C18 C -0.0926(3) 0.12939(19) -0.0017(4) 0.0558(11) Uani 1 1 d . . . H18A H -0.1647 0.1472 -0.0045 0.084 Uiso 1 1 calc R . . H18B H -0.0969 0.0845 0.0010 0.084 Uiso 1 1 calc R . . H18C H -0.0764 0.1416 -0.0623 0.084 Uiso 1 1 calc R . . C19 C -0.0027(4) 0.0641(2) 0.2152(4) 0.0634(13) Uani 1 1 d . . . H19A H 0.0609 0.0397 0.2586 0.095 Uiso 1 1 calc R . . H19B H -0.0425 0.0411 0.1530 0.095 Uiso 1 1 calc R . . H19C H -0.0543 0.0727 0.2518 0.095 Uiso 1 1 calc R . . C20 C 0.1768(4) 0.1511(3) 0.3670(3) 0.0633(13) Uani 1 1 d . . . H20A H 0.1262 0.1641 0.4024 0.095 Uiso 1 1 calc R . . H20B H 0.2469 0.1747 0.3926 0.095 Uiso 1 1 calc R . . H20C H 0.1935 0.1073 0.3791 0.095 Uiso 1 1 calc R . . C21 C 0.1391(5) 0.0615(3) -0.3719(3) 0.0715(14) Uani 1 1 d . . . H21A H 0.0576 0.0647 -0.4071 0.107 Uiso 1 1 calc R . . H21B H 0.1659 0.0223 -0.3894 0.107 Uiso 1 1 calc R . . H21C H 0.1769 0.0954 -0.3929 0.107 Uiso 1 1 calc R . . C22 C 0.1643(3) 0.06432(17) -0.2627(3) 0.0434(8) Uani 1 1 d . . . C23 C 0.5344(4) -0.08056(19) 0.4489(4) 0.0630(12) Uani 1 1 d . . . H23A H 0.5885 -0.0523 0.4952 0.095 Uiso 1 1 calc R . . H23B H 0.5750 -0.1148 0.4320 0.095 Uiso 1 1 calc R . . H23C H 0.4833 -0.0965 0.4817 0.095 Uiso 1 1 calc R . . C24 C 0.4699(3) -0.04811(16) 0.3564(3) 0.0482(9) Uani 1 1 d . . . Cl1 Cl 0.21554(11) -0.06406(5) 0.44460(11) 0.0707(3) Uani 1 1 d . . . Cl2 Cl 0.31917(8) 0.22512(5) -0.32512(7) 0.0488(2) Uani 1 1 d . . . O1 O 0.2637(3) -0.11914(17) 0.4321(3) 0.0866(11) Uani 1 1 d . A . O2 O 0.1177(10) -0.0657(6) 0.3400(8) 0.126(5) Uani 0.483(14) 1 d P A 1 O3 O 0.1442(9) -0.0784(6) 0.5117(9) 0.064(3) Uani 0.483(14) 1 d P A 1 O4 O 0.2650(15) -0.0142(6) 0.445(2) 0.175(12) Uani 0.483(14) 1 d P A 1 O2A O 0.2095(17) -0.0155(8) 0.3872(14) 0.195(12) Uani 0.517(14) 1 d P A 2 O3A O 0.1419(18) -0.0630(8) 0.479(2) 0.182(10) Uani 0.517(14) 1 d P A 2 O4A O 0.3156(10) -0.0403(5) 0.5403(9) 0.119(4) Uani 0.517(14) 1 d P A 2 O5 O 0.2610(4) 0.2322(3) -0.4266(3) 0.159(3) Uani 1 1 d . . . O6 O 0.3510(4) 0.2856(2) -0.2858(4) 0.1040(14) Uani 1 1 d . . . O7 O 0.4185(3) 0.19095(19) -0.3078(3) 0.0836(11) Uani 1 1 d . . . O8 O 0.2550(3) 0.20136(17) -0.2689(4) 0.0928(13) 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 0.01996(14) 0.02628(14) 0.02234(14) -0.00329(9) 0.00755(10) 0.00381(9) Mo2 0.02064(14) 0.02186(14) 0.02494(14) -0.00163(9) 0.00784(11) 0.00027(9) Cu1 0.0437(3) 0.0376(2) 0.0333(2) -0.01415(18) 0.01046(19) -0.00379(18) Cu2 0.0486(3) 0.0263(2) 0.0500(3) 0.00475(18) 0.0167(2) 0.00891(18) S1 0.0416(5) 0.0327(4) 0.0469(5) -0.0114(4) 0.0180(4) 0.0085(4) S2 0.0431(5) 0.0265(4) 0.0516(5) -0.0083(4) 0.0172(4) -0.0077(3) S3 0.0215(3) 0.0302(4) 0.0242(4) -0.0001(3) 0.0067(3) 0.0012(3) S4 0.0244(4) 0.0323(4) 0.0236(4) 0.0008(3) 0.0078(3) 0.0042(3) N1 0.0446(17) 0.0417(17) 0.0396(18) -0.0152(13) 0.0132(14) -0.0070(14) N2 0.056(2) 0.0361(18) 0.069(2) 0.0155(17) 0.0246(18) 0.0112(15) C1 0.0214(15) 0.0316(16) 0.0365(17) -0.0022(13) 0.0113(13) -0.0042(12) C2 0.0196(15) 0.047(2) 0.0331(17) 0.0043(14) 0.0102(13) -0.0041(13) C3 0.0225(16) 0.060(2) 0.0347(18) -0.0062(16) 0.0152(14) -0.0017(15) C4 0.0172(15) 0.047(2) 0.0397(18) -0.0065(15) 0.0088(14) 0.0054(13) C5 0.0181(14) 0.0408(18) 0.0287(16) -0.0047(13) 0.0039(12) -0.0022(12) C6 0.0362(19) 0.0335(18) 0.056(2) -0.0097(16) 0.0202(17) -0.0052(14) C7 0.039(2) 0.065(3) 0.048(2) 0.0240(19) 0.0111(18) -0.0047(18) C8 0.048(2) 0.106(4) 0.040(2) -0.015(2) 0.028(2) -0.005(2) C9 0.0302(19) 0.064(3) 0.071(3) -0.014(2) 0.0094(19) 0.0203(18) C10 0.0333(18) 0.060(2) 0.0319(18) -0.0015(16) 0.0009(15) -0.0006(17) C11 0.0233(15) 0.0353(17) 0.0403(18) -0.0103(14) 0.0174(14) 0.0028(13) C12 0.0252(15) 0.0250(15) 0.0353(16) -0.0003(12) 0.0154(13) 0.0065(12) C13 0.0190(15) 0.0297(16) 0.0438(19) -0.0004(14) 0.0087(14) 0.0055(12) C14 0.0236(16) 0.0374(18) 0.056(2) 0.0146(16) 0.0213(16) 0.0053(14) C15 0.0275(16) 0.058(2) 0.0341(17) 0.0069(16) 0.0199(14) 0.0100(15) C16 0.040(2) 0.047(2) 0.070(3) -0.032(2) 0.0211(19) -0.0052(17) C17 0.048(2) 0.0345(19) 0.051(2) 0.0114(16) 0.0266(18) 0.0162(16) C18 0.031(2) 0.044(2) 0.074(3) -0.010(2) -0.005(2) 0.0012(16) C19 0.046(2) 0.052(3) 0.102(4) 0.034(2) 0.038(2) 0.0067(19) C20 0.049(2) 0.115(4) 0.033(2) 0.011(2) 0.0225(19) 0.026(2) C21 0.087(4) 0.088(4) 0.038(2) -0.014(2) 0.020(2) -0.001(3) C22 0.049(2) 0.039(2) 0.043(2) -0.0106(16) 0.0166(17) -0.0010(16) C23 0.073(3) 0.034(2) 0.070(3) 0.013(2) 0.010(2) 0.002(2) C24 0.052(2) 0.0251(18) 0.068(3) 0.0076(18) 0.021(2) 0.0046(16) Cl1 0.0734(8) 0.0440(6) 0.1006(10) 0.0128(6) 0.0379(7) 0.0165(5) Cl2 0.0343(5) 0.0693(6) 0.0457(5) -0.0065(4) 0.0178(4) 0.0016(4) O1 0.095(3) 0.066(2) 0.101(3) -0.008(2) 0.037(2) 0.023(2) O2 0.117(9) 0.114(9) 0.104(8) 0.030(6) -0.016(6) 0.019(7) O3 0.057(5) 0.058(6) 0.087(6) 0.017(4) 0.039(5) 0.004(4) O4 0.130(13) 0.061(9) 0.39(4) -0.086(15) 0.155(18) -0.060(9) O2A 0.23(2) 0.134(16) 0.181(15) 0.121(13) 0.018(14) 0.072(15) O3A 0.227(16) 0.087(10) 0.35(3) -0.002(12) 0.244(19) -0.003(9) O4A 0.123(8) 0.064(6) 0.129(9) -0.004(5) -0.006(7) -0.034(5) O5 0.098(3) 0.296(8) 0.053(2) -0.033(4) -0.011(2) 0.075(4) O6 0.124(4) 0.083(3) 0.129(4) -0.025(3) 0.074(3) -0.037(2) O7 0.062(2) 0.113(3) 0.090(3) 0.031(2) 0.046(2) 0.037(2) O8 0.082(2) 0.071(2) 0.162(4) 0.000(2) 0.088(3) -0.0086(19) _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 S1 2.2296(9) . ? Mo1 S3 2.3273(11) . ? Mo1 S4 2.3302(9) . ? Mo1 C1 2.333(3) . ? Mo1 C5 2.347(3) . ? Mo1 C2 2.365(3) . ? Mo1 C3 2.385(3) . ? Mo1 C4 2.386(3) . ? Mo1 Cu1 2.7722(10) . ? Mo1 Cu2 2.7765(7) . ? Mo1 Mo2 2.8527(7) . ? Mo2 S2 2.2450(9) . ? Mo2 S4 2.3248(12) . ? Mo2 S3 2.3307(9) . ? Mo2 C11 2.333(3) . ? Mo2 C15 2.349(3) . ? Mo2 C12 2.354(3) . ? Mo2 C13 2.385(3) . ? Mo2 C14 2.393(3) . ? Mo2 Cu2 2.7420(7) . ? Mo2 Cu1 2.7495(7) . ? Cu1 N1 1.916(3) . ? Cu1 S3 2.2676(10) . ? Cu1 S2 2.3584(11) . ? Cu1 S1 2.3840(12) . ? Cu2 N2 1.913(3) . ? Cu2 S4 2.2680(9) . ? Cu2 S2 2.3518(13) . ? Cu2 S1 2.3829(11) . ? N1 C22 1.122(5) . ? N2 C24 1.124(5) . ? C1 C2 1.420(5) . ? C1 C5 1.428(5) . ? C1 C6 1.498(5) . ? C2 C3 1.426(5) . ? C2 C7 1.492(5) . ? C3 C4 1.420(5) . ? C3 C8 1.499(5) . ? C4 C5 1.420(5) . ? C4 C9 1.496(5) . ? C5 C10 1.493(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.420(5) . ? C11 C15 1.430(5) . ? C11 C16 1.502(5) . ? C12 C13 1.415(4) . ? C12 C17 1.490(4) . ? C13 C14 1.424(5) . ? C13 C18 1.494(5) . ? C14 C15 1.416(5) . ? C14 C19 1.495(5) . ? C15 C20 1.497(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.454(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 C24 1.454(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? Cl1 O3A 1.189(16) . ? Cl1 O4 1.253(10) . ? Cl1 O2A 1.316(12) . ? Cl1 O1 1.385(4) . ? Cl1 O3 1.548(11) . ? Cl1 O2 1.558(10) . ? Cl1 O4A 1.579(10) . ? Cl2 O5 1.365(4) . ? Cl2 O7 1.409(3) . ? Cl2 O8 1.415(3) . ? Cl2 O6 1.430(4) . ? 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 S1 Mo1 S3 106.69(4) . . ? S1 Mo1 S4 106.46(3) . . ? S3 Mo1 S4 99.56(3) . . ? S1 Mo1 C1 142.26(8) . . ? S3 Mo1 C1 100.88(8) . . ? S4 Mo1 C1 93.56(8) . . ? S1 Mo1 C5 112.88(8) . . ? S3 Mo1 C5 136.42(9) . . ? S4 Mo1 C5 86.37(8) . . ? C1 Mo1 C5 35.55(11) . . ? S1 Mo1 C2 122.13(9) . . ? S3 Mo1 C2 85.39(8) . . ? S4 Mo1 C2 127.50(9) . . ? C1 Mo1 C2 35.19(11) . . ? C5 Mo1 C2 58.58(11) . . ? S1 Mo1 C3 88.97(9) . . ? S3 Mo1 C3 106.33(9) . . ? S4 Mo1 C3 144.57(9) . . ? C1 Mo1 C3 58.41(11) . . ? C5 Mo1 C3 58.21(11) . . ? C2 Mo1 C3 34.94(12) . . ? S1 Mo1 C4 84.10(9) . . ? S3 Mo1 C4 140.47(9) . . ? S4 Mo1 C4 113.94(9) . . ? C1 Mo1 C4 58.38(11) . . ? C5 Mo1 C4 34.91(11) . . ? C2 Mo1 C4 57.97(12) . . ? C3 Mo1 C4 34.64(12) . . ? S1 Mo1 Cu1 55.66(3) . . ? S3 Mo1 Cu1 51.91(3) . . ? S4 Mo1 Cu1 103.71(3) . . ? C1 Mo1 Cu1 149.45(8) . . ? C5 Mo1 Cu1 166.28(8) . . ? C2 Mo1 Cu1 118.86(8) . . ? C3 Mo1 Cu1 111.22(8) . . ? C4 Mo1 Cu1 131.41(8) . . ? S1 Mo1 Cu2 55.56(3) . . ? S3 Mo1 Cu2 103.63(3) . . ? S4 Mo1 Cu2 51.84(2) . . ? C1 Mo1 Cu2 140.20(8) . . ? C5 Mo1 Cu2 113.28(8) . . ? C2 Mo1 Cu2 170.98(8) . . ? C3 Mo1 Cu2 138.93(9) . . ? C4 Mo1 Cu2 113.29(9) . . ? Cu1 Mo1 Cu2 67.98(2) . . ? S1 Mo1 Mo2 97.86(3) . . ? S3 Mo1 Mo2 52.29(2) . . ? S4 Mo1 Mo2 52.12(3) . . ? C1 Mo1 Mo2 119.48(8) . . ? C5 Mo1 Mo2 134.54(8) . . ? C2 Mo1 Mo2 129.70(8) . . ? C3 Mo1 Mo2 158.61(9) . . ? C4 Mo1 Mo2 165.95(9) . . ? Cu1 Mo1 Mo2 58.50(2) . . ? Cu2 Mo1 Mo2 58.282(16) . . ? S2 Mo2 S4 106.82(3) . . ? S2 Mo2 S3 106.68(3) . . ? S4 Mo2 S3 99.62(3) . . ? S2 Mo2 C11 142.52(8) . . ? S4 Mo2 C11 93.31(8) . . ? S3 Mo2 C11 100.45(9) . . ? S2 Mo2 C15 113.11(10) . . ? S4 Mo2 C15 86.42(9) . . ? S3 Mo2 C15 136.01(10) . . ? C11 Mo2 C15 35.56(12) . . ? S2 Mo2 C12 122.20(8) . . ? S4 Mo2 C12 127.27(8) . . ? S3 Mo2 C12 84.82(8) . . ? C11 Mo2 C12 35.28(11) . . ? C15 Mo2 C12 58.61(11) . . ? S2 Mo2 C13 89.30(8) . . ? S4 Mo2 C13 144.51(9) . . ? S3 Mo2 C13 105.78(9) . . ? C11 Mo2 C13 58.27(11) . . ? C15 Mo2 C13 58.09(12) . . ? C12 Mo2 C13 34.75(11) . . ? S2 Mo2 C14 84.50(9) . . ? S4 Mo2 C14 114.03(9) . . ? S3 Mo2 C14 139.93(8) . . ? C11 Mo2 C14 58.25(12) . . ? C15 Mo2 C14 34.72(13) . . ? C12 Mo2 C14 57.90(11) . . ? C13 Mo2 C14 34.68(12) . . ? S2 Mo2 Cu2 55.19(3) . . ? S4 Mo2 Cu2 52.40(2) . . ? S3 Mo2 Cu2 104.59(3) . . ? C11 Mo2 Cu2 140.10(9) . . ? C15 Mo2 Cu2 112.99(9) . . ? C12 Mo2 Cu2 170.57(8) . . ? C13 Mo2 Cu2 138.63(8) . . ? C14 Mo2 Cu2 112.89(8) . . ? S2 Mo2 Cu1 55.25(3) . . ? S4 Mo2 Cu1 104.56(3) . . ? S3 Mo2 Cu1 52.23(2) . . ? C11 Mo2 Cu1 149.04(9) . . ? C15 Mo2 Cu1 165.64(9) . . ? C12 Mo2 Cu1 118.14(8) . . ? C13 Mo2 Cu1 110.53(9) . . ? C14 Mo2 Cu1 130.93(10) . . ? Cu2 Mo2 Cu1 68.78(2) . . ? S2 Mo2 Mo1 98.15(3) . . ? S4 Mo2 Mo1 52.29(2) . . ? S3 Mo2 Mo1 52.18(3) . . ? C11 Mo2 Mo1 119.00(8) . . ? C15 Mo2 Mo1 134.58(9) . . ? C12 Mo2 Mo1 129.00(8) . . ? C13 Mo2 Mo1 157.92(8) . . ? C14 Mo2 Mo1 166.29(9) . . ? Cu2 Mo2 Mo1 59.468(16) . . ? Cu1 Mo2 Mo1 59.28(3) . . ? N1 Cu1 S3 113.55(10) . . ? N1 Cu1 S2 124.32(10) . . ? S3 Cu1 S2 105.02(3) . . ? N1 Cu1 S1 112.86(10) . . ? S3 Cu1 S1 103.60(3) . . ? S2 Cu1 S1 94.26(4) . . ? N1 Cu1 Mo2 150.05(10) . . ? S3 Cu1 Mo2 54.34(2) . . ? S2 Cu1 Mo2 51.45(3) . . ? S1 Cu1 Mo2 97.04(4) . . ? N1 Cu1 Mo1 137.37(10) . . ? S3 Cu1 Mo1 53.88(2) . . ? S2 Cu1 Mo1 97.67(3) . . ? S1 Cu1 Mo1 50.56(3) . . ? Mo2 Cu1 Mo1 62.21(2) . . ? N2 Cu2 S4 110.30(12) . . ? N2 Cu2 S2 126.83(11) . . ? S4 Cu2 S2 105.16(3) . . ? N2 Cu2 S1 113.55(11) . . ? S4 Cu2 S1 103.50(3) . . ? S2 Cu2 S1 94.46(4) . . ? N2 Cu2 Mo2 148.73(11) . . ? S4 Cu2 Mo2 54.30(3) . . ? S2 Cu2 Mo2 51.61(3) . . ? S1 Cu2 Mo2 97.26(3) . . ? N2 Cu2 Mo1 135.18(11) . . ? S4 Cu2 Mo1 53.89(2) . . ? S2 Cu2 Mo1 97.72(3) . . ? S1 Cu2 Mo1 50.50(2) . . ? Mo2 Cu2 Mo1 62.250(18) . . ? Mo1 S1 Cu2 73.93(3) . . ? Mo1 S1 Cu1 73.78(3) . . ? Cu2 S1 Cu1 81.19(4) . . ? Mo2 S2 Cu2 73.20(3) . . ? Mo2 S2 Cu1 73.30(3) . . ? Cu2 S2 Cu1 82.38(4) . . ? Cu1 S3 Mo1 74.20(3) . . ? Cu1 S3 Mo2 73.43(3) . . ? Mo1 S3 Mo2 75.53(3) . . ? Cu2 S4 Mo2 73.30(3) . . ? Cu2 S4 Mo1 74.27(3) . . ? Mo2 S4 Mo1 75.59(3) . . ? C22 N1 Cu1 170.7(3) . . ? C24 N2 Cu2 166.7(4) . . ? C2 C1 C5 108.0(3) . . ? C2 C1 C6 126.6(3) . . ? C5 C1 C6 125.1(3) . . ? C2 C1 Mo1 73.64(18) . . ? C5 C1 Mo1 72.78(18) . . ? C6 C1 Mo1 124.6(2) . . ? C1 C2 C3 108.0(3) . . ? C1 C2 C7 125.5(3) . . ? C3 C2 C7 126.1(3) . . ? C1 C2 Mo1 71.17(18) . . ? C3 C2 Mo1 73.29(19) . . ? C7 C2 Mo1 127.0(2) . . ? C4 C3 C2 108.0(3) . . ? C4 C3 C8 125.5(3) . . ? C2 C3 C8 126.4(4) . . ? C4 C3 Mo1 72.73(19) . . ? C2 C3 Mo1 71.76(17) . . ? C8 C3 Mo1 124.4(3) . . ? C3 C4 C5 108.3(3) . . ? C3 C4 C9 126.0(3) . . ? C5 C4 C9 125.5(3) . . ? C3 C4 Mo1 72.63(18) . . ? C5 C4 Mo1 71.04(17) . . ? C9 C4 Mo1 126.2(3) . . ? C4 C5 C1 107.8(3) . . ? C4 C5 C10 125.6(3) . . ? C1 C5 C10 126.1(3) . . ? C4 C5 Mo1 74.05(18) . . ? C1 C5 Mo1 71.68(17) . . ? C10 C5 Mo1 126.6(2) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 107.8(3) . . ? C12 C11 C16 125.7(3) . . ? C15 C11 C16 126.3(3) . . ? C12 C11 Mo2 73.18(17) . . ? C15 C11 Mo2 72.86(18) . . ? C16 C11 Mo2 124.2(2) . . ? C13 C12 C11 108.2(3) . . ? C13 C12 C17 125.5(3) . . ? C11 C12 C17 125.9(3) . . ? C13 C12 Mo2 73.81(17) . . ? C11 C12 Mo2 71.55(17) . . ? C17 C12 Mo2 126.6(2) . . ? C12 C13 C14 108.1(3) . . ? C12 C13 C18 124.9(3) . . ? C14 C13 C18 126.9(3) . . ? C12 C13 Mo2 71.44(17) . . ? C14 C13 Mo2 72.99(17) . . ? C18 C13 Mo2 124.9(2) . . ? C15 C14 C13 108.1(3) . . ? C15 C14 C19 126.3(4) . . ? C13 C14 C19 125.5(4) . . ? C15 C14 Mo2 70.95(17) . . ? C13 C14 Mo2 72.33(18) . . ? C19 C14 Mo2 125.8(3) . . ? C14 C15 C11 107.9(3) . . ? C14 C15 C20 124.6(4) . . ? C11 C15 C20 127.1(4) . . ? C14 C15 Mo2 74.33(19) . . ? C11 C15 Mo2 71.58(17) . . ? C20 C15 Mo2 125.6(2) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C21 179.0(4) . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 C23 178.3(5) . . ? O3A Cl1 O2A 110.2(13) . . ? O3A Cl1 O4A 99.3(13) . . ? O2A Cl1 O4A 96.6(9) . . ? O2A Cl1 O1 123.6(10) . . ? O3A Cl1 O1 120.7(9) . . ? O1 Cl1 O4A 97.7(5) . . ? O4 Cl1 O1 120.7(6) . . ? O4 Cl1 O3 124.5(10) . . ? O1 Cl1 O3 106.2(5) . . ? O4 Cl1 O2 105.0(13) . . ? O1 Cl1 O2 95.8(5) . . ? O3 Cl1 O2 97.3(6) . . ? O5 Cl2 O7 111.4(3) . . ? O5 Cl2 O8 114.6(3) . . ? O7 Cl2 O8 111.3(2) . . ? O5 Cl2 O6 106.0(4) . . ? O7 Cl2 O6 107.8(3) . . ? O8 Cl2 O6 105.2(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.823 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.080 #===END #============================================================================== data_4MeCN _database_code_depnum_ccdc_archive 'CCDC 679377' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H38 Cu2 Mo2 N2 S4, 2(PF6), CH3CN' _chemical_formula_sum 'C32 H41 Cu2 F12 Mo2 N3 P2 S4' _chemical_formula_weight 1204.88 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.178(15) _cell_length_b 9.0683(18) _cell_length_c 23.821(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.27(3) _cell_angle_gamma 90.00 _cell_volume 9096(4) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8138 _cell_measurement_theta_min 3.0724 _cell_measurement_theta_max 25.3491 _exptl_crystal_description flake _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4783 _exptl_absorpt_coefficient_mu 1.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5269 _exptl_absorpt_correction_T_max 0.9001 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23743 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8068 _reflns_number_gt 5904 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1600P)^2^+10.0000P] 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 8068 _refine_ls_number_parameters 449 _refine_ls_number_restraints 111 _refine_ls_R_factor_all 0.1549 _refine_ls_R_factor_gt 0.1254 _refine_ls_wR_factor_ref 0.3447 _refine_ls_wR_factor_gt 0.3229 _refine_ls_goodness_of_fit_ref 1.331 _refine_ls_restrained_S_all 1.326 _refine_ls_shift/su_max 0.004 _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 0.83439(2) 0.57092(12) 0.87076(4) 0.0297(3) Uani 1 1 d . . . Mo2 Mo 0.90123(3) 0.51673(14) 0.87556(5) 0.0413(4) Uani 1 1 d . . . Cu1 Cu 0.85982(4) 0.33992(19) 0.93133(7) 0.0429(5) Uani 1 1 d . . . Cu2 Cu 0.85922(4) 0.3523(2) 0.80757(7) 0.0426(5) Uani 1 1 d . . . S1 S 0.81594(8) 0.3402(4) 0.86581(14) 0.0384(8) Uani 1 1 d . . . S2 S 0.90108(9) 0.2712(4) 0.87252(15) 0.0467(9) Uani 1 1 d . . . S3 S 0.86985(9) 0.5798(4) 0.94914(14) 0.0426(8) Uani 1 1 d . . . S4 S 0.86908(8) 0.5971(4) 0.79871(14) 0.0397(8) Uani 1 1 d . . . N1 N 0.8571(3) 0.2093(14) 0.9956(4) 0.045(3) Uani 1 1 d . A . C1 C 0.8190(3) 0.8184(13) 0.8745(5) 0.035(3) Uani 1 1 d . . . C2 C 0.8034(3) 0.7570(13) 0.8237(5) 0.032(3) Uani 1 1 d . . . C3 C 0.7827(3) 0.6458(16) 0.8395(5) 0.039(3) Uani 1 1 d . . . C4 C 0.7831(3) 0.6359(14) 0.8996(5) 0.035(3) Uani 1 1 d . . . C5 C 0.8046(3) 0.7453(15) 0.9208(5) 0.039(3) Uani 1 1 d . . . C6 C 0.8399(4) 0.9475(16) 0.8770(8) 0.063(5) Uani 1 1 d . A . H6A H 0.8562 0.9364 0.8494 0.095 Uiso 1 1 calc R . . H6B H 0.8502 0.9558 0.9148 0.095 Uiso 1 1 calc R . . H6C H 0.8274 1.0365 0.8684 0.095 Uiso 1 1 calc R . . C7 C 0.8080(4) 0.8210(18) 0.7665(6) 0.057(4) Uani 1 1 d . . . H7A H 0.7931 0.7744 0.7388 0.085 Uiso 1 1 calc R A . H7B H 0.8298 0.8029 0.7561 0.085 Uiso 1 1 calc R . . H7C H 0.8040 0.9275 0.7672 0.085 Uiso 1 1 calc R . . C8 C 0.7601(3) 0.5607(18) 0.7996(6) 0.052(4) Uani 1 1 d . A . H8A H 0.7416 0.6223 0.7890 0.078 Uiso 1 1 calc R . . H8B H 0.7531 0.4711 0.8183 0.078 Uiso 1 1 calc R . . H8C H 0.7710 0.5338 0.7659 0.078 Uiso 1 1 calc R . . C9 C 0.7621(3) 0.5404(17) 0.9337(6) 0.048(4) Uani 1 1 d . . . H9A H 0.7727 0.5219 0.9708 0.072 Uiso 1 1 calc R A . H9B H 0.7582 0.4464 0.9142 0.072 Uiso 1 1 calc R . . H9C H 0.7419 0.5907 0.9383 0.072 Uiso 1 1 calc R . . C10 C 0.8098(4) 0.7863(18) 0.9807(5) 0.057(4) Uani 1 1 d . . . H10A H 0.7999 0.7123 1.0041 0.086 Uiso 1 1 calc R A . H10B H 0.8002 0.8829 0.9870 0.086 Uiso 1 1 calc R . . H10C H 0.8326 0.7910 0.9907 0.086 Uiso 1 1 calc R . . C21 C 0.8306(4) 0.1949(16) 1.0229(6) 0.050(4) Uani 1 1 d . . . H21 H 0.8123 0.2478 1.0091 0.060 Uiso 1 1 calc R A . C22 C 0.8279(3) 0.1087(17) 1.0698(6) 0.046(4) Uani 1 1 d . A . H22 H 0.8080 0.0962 1.0860 0.055 Uiso 1 1 calc R . . C25 C 0.8544(3) 0.0419(15) 1.0923(5) 0.039(3) Uani 1 1 d . . . C24 C 0.8830(3) 0.0543(17) 1.0635(5) 0.045(4) Uani 1 1 d . A . H24 H 0.9018 0.0045 1.0770 0.054 Uiso 1 1 calc R . . C23 C 0.8829(4) 0.1387(18) 1.0166(6) 0.051(4) Uani 1 1 d . . . H23 H 0.9021 0.1481 0.9978 0.061 Uiso 1 1 calc R A . P1 P 0.73176(9) 1.0373(5) 0.88422(17) 0.0480(10) Uani 1 1 d . . . F1 F 0.7584(4) 1.042(2) 0.9279(6) 0.154(7) Uani 1 1 d . . . F2 F 0.7317(4) 0.8699(14) 0.8954(9) 0.147(7) Uani 1 1 d . . . F3 F 0.7046(3) 1.0461(16) 0.9278(6) 0.118(5) Uani 1 1 d . . . F4 F 0.7043(3) 1.0270(16) 0.8348(5) 0.109(4) Uani 1 1 d . . . F5 F 0.7315(3) 1.2057(13) 0.8724(7) 0.124(5) Uani 1 1 d . . . F6 F 0.7595(3) 1.0257(14) 0.8423(6) 0.102(4) Uani 1 1 d . . . F7 F 0.9392(5) 0.276(3) 1.0703(9) 0.331(17) Uiso 1 1 d D . . F8 F 0.9914(5) 0.273(3) 1.0668(8) 0.331(17) Uiso 1 1 d D . . P2 P 0.9674(3) 0.247(2) 1.1149(6) 0.245(8) Uiso 0.645(11) 1 d PD A 1 F9 F 0.9675(6) 0.077(2) 1.1011(13) 0.245(8) Uiso 0.645(11) 1 d PD A 1 F10 F 0.9414(5) 0.221(4) 1.1592(9) 0.245(8) Uiso 0.645(11) 1 d PD A 1 F11 F 0.9678(7) 0.417(2) 1.1295(13) 0.245(8) Uiso 0.645(11) 1 d PD A 1 F12 F 0.9952(5) 0.221(4) 1.1606(9) 0.245(8) Uiso 0.645(11) 1 d PD A 1 P2A P 0.9673(4) 0.185(2) 1.1015(7) 0.162(9) Uiso 0.355(11) 1 d PD A 2 F9A F 0.9625(8) 0.067(3) 1.0526(13) 0.162(9) Uiso 0.355(11) 1 d PD A 2 F10A F 0.9430(6) 0.101(4) 1.1376(13) 0.162(9) Uiso 0.355(11) 1 d PD A 2 F11A F 0.9713(7) 0.307(3) 1.1487(9) 0.162(9) Uiso 0.355(11) 1 d PD A 2 F12A F 0.9956(6) 0.091(4) 1.1292(14) 0.162(9) Uiso 0.355(11) 1 d PD A 2 C11 C 0.9354(3) 0.7132(18) 0.8472(7) 0.075(3) Uani 0.645(11) 1 d PGU . 1 C12 C 0.9349(4) 0.7130(19) 0.9102(7) 0.075(3) Uani 0.645(11) 1 d PGU . 1 C13 C 0.9462(4) 0.579(2) 0.9327(8) 0.075(3) Uani 0.645(11) 1 d PGU . 1 C14 C 0.9583(4) 0.5095(19) 0.8884(8) 0.075(3) Uani 0.645(11) 1 d PGU . 1 C15 C 0.9498(4) 0.5774(18) 0.8392(7) 0.075(3) Uani 0.645(11) 1 d PGU . 1 C16 C 0.9298(4) 0.831(3) 0.8132(9) 0.075(3) Uani 0.645(11) 1 d PGU . 1 H16A H 0.9464 0.8381 0.7863 0.112 Uiso 0.645(11) 1 calc PR A 1 H16B H 0.9296 0.9210 0.8359 0.112 Uiso 0.645(11) 1 calc PR A 1 H16C H 0.9091 0.8192 0.7927 0.112 Uiso 0.645(11) 1 calc PR A 1 C17 C 0.9240(6) 0.849(3) 0.9475(13) 0.075(3) Uani 0.645(11) 1 d PU . 1 H17A H 0.9291 0.8277 0.9873 0.112 Uiso 0.645(11) 1 calc PR A 1 H17B H 0.9011 0.8632 0.9413 0.112 Uiso 0.645(11) 1 calc PR A 1 H17C H 0.9352 0.9382 0.9366 0.112 Uiso 0.645(11) 1 calc PR A 1 C18 C 0.9497(6) 0.538(3) 0.9985(12) 0.075(3) Uani 0.645(11) 1 d PU . 1 H18A H 0.9720 0.5153 1.0091 0.112 Uiso 0.645(11) 1 calc PR A 1 H18B H 0.9366 0.4511 1.0056 0.112 Uiso 0.645(11) 1 calc PR A 1 H18C H 0.9427 0.6211 1.0207 0.112 Uiso 0.645(11) 1 calc PR A 1 C19 C 0.9755(6) 0.360(3) 0.8887(14) 0.075(3) Uani 0.645(11) 1 d PU . 1 H19A H 0.9683 0.3033 0.8552 0.112 Uiso 0.645(11) 1 calc PR A 1 H19B H 0.9707 0.3046 0.9225 0.112 Uiso 0.645(11) 1 calc PR A 1 H19C H 0.9985 0.3759 0.8884 0.112 Uiso 0.645(11) 1 calc PR A 1 C20 C 0.9558(6) 0.544(4) 0.7836(13) 0.075(3) Uani 0.645(11) 1 d PU . 1 H20A H 0.9698 0.6185 0.7689 0.112 Uiso 0.645(11) 1 calc PR A 1 H20B H 0.9357 0.5418 0.7608 0.112 Uiso 0.645(11) 1 calc PR A 1 H20C H 0.9660 0.4466 0.7822 0.112 Uiso 0.645(11) 1 calc PR A 1 C11A C 0.9435(14) 0.626(7) 0.826(3) 0.074(6) Uiso 0.355(11) 1 d PU . 2 C12A C 0.9415(13) 0.702(7) 0.871(2) 0.074(6) Uiso 0.355(11) 1 d PU . 2 C13A C 0.9482(15) 0.607(7) 0.923(3) 0.074(6) Uiso 0.355(11) 1 d PU . 2 C14A C 0.9579(15) 0.483(7) 0.897(3) 0.074(6) Uiso 0.355(11) 1 d PU . 2 C15A C 0.9527(14) 0.502(7) 0.844(3) 0.074(6) Uiso 0.355(11) 1 d PU . 2 C16A C 0.9356(13) 0.703(6) 0.777(2) 0.074(6) Uiso 0.355(11) 1 d PU . 2 H16D H 0.9294 0.8038 0.7861 0.111 Uiso 0.355(11) 1 calc PR A 2 H16E H 0.9178 0.6539 0.7560 0.111 Uiso 0.355(11) 1 calc PR A 2 H16F H 0.9539 0.7059 0.7533 0.111 Uiso 0.355(11) 1 calc PR A 2 C17A C 0.9291(4) 0.853(2) 0.8860(9) 0.074(6) Uiso 0.355(11) 1 d PGU . 2 H17D H 0.9161 0.8923 0.8541 0.111 Uiso 0.355(11) 1 calc PR A 2 H17E H 0.9470 0.9194 0.8947 0.111 Uiso 0.355(11) 1 calc PR A 2 H17F H 0.9163 0.8444 0.9188 0.111 Uiso 0.355(11) 1 calc PR A 2 C18A C 0.9484(6) 0.640(3) 0.9801(10) 0.074(6) Uiso 0.355(11) 1 d PGU . 2 H18D H 0.9312 0.5874 0.9971 0.111 Uiso 0.355(11) 1 calc PR A 2 H18E H 0.9455 0.7469 0.9849 0.111 Uiso 0.355(11) 1 calc PR A 2 H18F H 0.9688 0.6107 0.9984 0.111 Uiso 0.355(11) 1 calc PR A 2 C19A C 0.9709(7) 0.358(3) 0.9275(12) 0.074(6) Uiso 0.355(11) 1 d PGU . 2 H19D H 0.9648 0.2668 0.9074 0.111 Uiso 0.355(11) 1 calc PR A 2 H19E H 0.9628 0.3556 0.9652 0.111 Uiso 0.355(11) 1 calc PR A 2 H19F H 0.9942 0.3654 0.9305 0.111 Uiso 0.355(11) 1 calc PR A 2 C20A C 0.9655(8) 0.395(3) 0.8008(12) 0.074(6) Uiso 0.355(11) 1 d PGU . 2 H20D H 0.9731 0.3053 0.8201 0.111 Uiso 0.355(11) 1 calc PR A 2 H20E H 0.9831 0.4416 0.7822 0.111 Uiso 0.355(11) 1 calc PR A 2 H20F H 0.9485 0.3700 0.7727 0.111 Uiso 0.355(11) 1 calc PR A 2 C31 C 0.6235(7) 1.061(3) 0.8708(13) 0.142(7) Uiso 1 1 d D . . C32 C 0.6150(13) 0.920(4) 0.891(2) 0.142(7) Uiso 0.645(11) 1 d PD A 1 N3 N 0.6081(9) 0.809(4) 0.9112(16) 0.142(7) Uiso 0.645(11) 1 d PD A 1 C32A C 0.5982(13) 0.958(8) 0.876(4) 0.142(7) Uiso 0.355(11) 1 d PD A 2 N3A N 0.5753(11) 0.888(7) 0.878(3) 0.142(7) Uiso 0.355(11) 1 d PD A 2 N2 N 0.8570(3) -0.2220(14) 1.2415(4) 0.041(3) Uani 1 1 d . . . C28 C 0.8313(3) -0.2252(16) 1.2042(5) 0.045(4) Uani 1 1 d . A . H28 H 0.8139 -0.2873 1.2114 0.053 Uiso 1 1 calc R . . C27 C 0.8301(3) -0.1426(15) 1.1576(5) 0.038(3) Uani 1 1 d . . . H27 H 0.8122 -0.1501 1.1316 0.046 Uiso 1 1 calc R A . C26 C 0.8551(3) -0.0442(16) 1.1463(5) 0.038(3) Uani 1 1 d . A . C29 C 0.8800(4) -0.0496(19) 1.1839(6) 0.054(4) Uani 1 1 d . . . H29 H 0.8982 0.0078 1.1769 0.065 Uiso 1 1 calc R A . C30 C 0.8806(3) -0.1343(16) 1.2322(6) 0.045(4) Uani 1 1 d . A . H30 H 0.8983 -0.1285 1.2587 0.055 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 0.0420(6) 0.0281(6) 0.0192(6) -0.0007(4) 0.0028(4) -0.0020(5) Mo2 0.0400(7) 0.0458(8) 0.0379(7) 0.0024(6) -0.0003(5) -0.0036(5) Cu1 0.0700(12) 0.0352(10) 0.0237(9) 0.0041(7) 0.0032(7) -0.0017(8) Cu2 0.0637(11) 0.0409(11) 0.0236(9) -0.0050(7) 0.0063(7) 0.0012(8) S1 0.0474(19) 0.0325(19) 0.0354(18) -0.0017(14) 0.0036(14) -0.0063(14) S2 0.061(2) 0.047(2) 0.0324(19) 0.0035(16) 0.0006(15) 0.0088(18) S3 0.056(2) 0.045(2) 0.0250(17) -0.0027(15) -0.0064(14) -0.0049(16) S4 0.0474(19) 0.043(2) 0.0293(17) 0.0083(15) 0.0111(14) -0.0044(15) N1 0.053(7) 0.056(8) 0.025(6) 0.001(6) 0.009(5) 0.009(6) C1 0.057(8) 0.010(6) 0.037(7) -0.002(5) 0.006(6) -0.006(5) C2 0.053(7) 0.021(6) 0.024(6) 0.001(5) 0.014(5) 0.008(5) C3 0.041(7) 0.047(9) 0.030(7) -0.005(6) 0.001(5) 0.014(6) C4 0.038(7) 0.034(7) 0.034(7) -0.001(6) 0.016(5) 0.002(6) C5 0.070(9) 0.034(8) 0.015(6) -0.007(5) 0.009(6) -0.007(6) C6 0.090(12) 0.027(8) 0.074(12) 0.000(8) 0.012(10) 0.005(8) C7 0.070(10) 0.058(11) 0.045(9) 0.019(8) 0.017(7) 0.023(8) C8 0.046(8) 0.067(11) 0.043(9) -0.020(8) 0.000(6) -0.028(7) C9 0.047(8) 0.052(9) 0.047(9) 0.020(7) 0.016(6) -0.004(7) C10 0.097(12) 0.050(10) 0.024(7) -0.016(7) 0.001(7) 0.022(9) C21 0.063(9) 0.038(9) 0.047(9) 0.002(7) 0.001(7) 0.006(7) C22 0.042(7) 0.057(10) 0.039(8) 0.013(7) 0.013(6) 0.010(7) C25 0.065(9) 0.030(7) 0.022(7) -0.002(5) 0.009(6) -0.015(6) C24 0.046(8) 0.064(10) 0.023(7) 0.018(7) -0.005(5) 0.001(7) C23 0.056(9) 0.064(11) 0.034(8) -0.002(7) 0.018(7) -0.017(8) P1 0.054(2) 0.055(3) 0.035(2) -0.0015(19) 0.0069(16) 0.0074(19) F1 0.134(13) 0.24(2) 0.087(11) 0.016(12) -0.040(9) 0.010(13) F2 0.123(12) 0.065(9) 0.26(2) 0.044(11) 0.051(12) 0.027(8) F3 0.143(12) 0.124(11) 0.096(10) 0.019(9) 0.077(9) 0.032(9) F4 0.095(9) 0.145(13) 0.083(9) 0.009(9) -0.026(7) -0.024(8) F5 0.098(9) 0.055(8) 0.220(17) -0.028(9) 0.005(10) 0.003(6) F6 0.101(9) 0.107(10) 0.104(10) 0.022(8) 0.054(7) 0.025(7) C11 0.043(5) 0.085(8) 0.095(8) 0.013(6) -0.006(5) -0.008(5) C12 0.043(5) 0.085(8) 0.095(8) 0.013(6) -0.006(5) -0.008(5) C13 0.043(5) 0.085(8) 0.095(8) 0.013(6) -0.006(5) -0.008(5) C14 0.043(5) 0.085(8) 0.095(8) 0.013(6) -0.006(5) -0.008(5) C15 0.043(5) 0.085(8) 0.095(8) 0.013(6) -0.006(5) -0.008(5) C16 0.043(5) 0.085(8) 0.095(8) 0.013(6) -0.006(5) -0.008(5) C17 0.043(5) 0.085(8) 0.095(8) 0.013(6) -0.006(5) -0.008(5) C18 0.043(5) 0.085(8) 0.095(8) 0.013(6) -0.006(5) -0.008(5) C19 0.043(5) 0.085(8) 0.095(8) 0.013(6) -0.006(5) -0.008(5) C20 0.043(5) 0.085(8) 0.095(8) 0.013(6) -0.006(5) -0.008(5) N2 0.049(7) 0.055(8) 0.020(5) 0.005(5) 0.001(4) -0.006(6) C28 0.054(8) 0.050(9) 0.030(7) 0.004(7) 0.009(6) -0.018(7) C27 0.047(7) 0.038(8) 0.028(7) 0.012(6) -0.006(5) -0.015(6) C26 0.052(8) 0.043(8) 0.020(6) 0.006(6) 0.005(5) 0.000(6) C29 0.060(9) 0.072(11) 0.029(8) -0.003(7) -0.001(6) -0.039(8) C30 0.050(8) 0.043(9) 0.042(8) 0.010(7) -0.007(6) -0.019(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 S1 2.233(4) . ? Mo1 S3 2.326(3) . ? Mo1 S4 2.330(3) . ? Mo1 C1 2.340(12) . ? Mo1 C3 2.363(13) . ? Mo1 C2 2.375(12) . ? Mo1 C5 2.382(13) . ? Mo1 C4 2.383(12) . ? Mo1 Cu1 2.728(2) . ? Mo1 Cu2 2.734(2) . ? Mo1 Mo2 2.8575(18) . ? Mo2 S2 2.228(4) . ? Mo2 S3 2.327(4) . ? Mo2 S4 2.332(4) . ? Mo2 C15 2.334(17) . ? Mo2 C13 2.338(19) . ? Mo2 C15A 2.35(6) . ? Mo2 C13A 2.37(6) . ? Mo2 C12 2.395(17) . ? Mo2 C12A 2.40(6) . ? Mo2 C14 2.410(18) . ? Mo2 C11A 2.41(6) . ? Mo2 C11 2.414(14) . ? Cu1 N1 1.944(12) . ? Cu1 S3 2.252(4) . ? Cu1 S1 2.352(4) . ? Cu1 S2 2.379(4) . ? Cu1 Cu2 2.949(2) . ? Cu2 N2 1.966(11) 6 ? Cu2 S4 2.270(4) . ? Cu2 S1 2.357(4) . ? Cu2 S2 2.396(4) . ? N1 C21 1.333(18) . ? N1 C23 1.337(19) . ? C1 C5 1.449(17) . ? C1 C2 1.454(17) . ? C1 C6 1.466(19) . ? C2 C3 1.399(19) . ? C2 C7 1.506(17) . ? C3 C4 1.434(18) . ? C3 C8 1.518(18) . ? C4 C5 1.418(18) . ? C4 C9 1.507(17) . ? C5 C10 1.479(17) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C21 C22 1.372(19) . ? C21 H21 0.9500 . ? C22 C25 1.353(19) . ? C22 H22 0.9500 . ? C25 C24 1.427(18) . ? C25 C26 1.503(17) . ? C24 C23 1.355(19) . ? C24 H24 0.9500 . ? C23 H23 0.9500 . ? P1 F1 1.489(14) . ? P1 F2 1.541(13) . ? P1 F5 1.553(14) . ? P1 F6 1.584(11) . ? P1 F3 1.592(11) . ? P1 F4 1.607(12) . ? F7 P2 1.569(9) . ? F7 P2A 1.593(9) . ? F8 P2A 1.568(9) . ? F8 P2 1.589(9) . ? P2 F12 1.571(9) . ? P2 F11 1.580(9) . ? P2 F9 1.583(9) . ? P2 F10 1.584(9) . ? P2A F10A 1.572(9) . ? P2A F12A 1.577(9) . ? P2A F11A 1.578(9) . ? P2A F9A 1.583(9) . ? C11 C16 1.353(9) . ? C11 C15 1.390(10) . ? C11 C12 1.504(10) . ? C12 C13 1.402(10) . ? C12 C17 1.60(3) . ? C13 C14 1.353(9) . ? C13 C18 1.61(3) . ? C14 C15 1.353(9) . ? C14 C19 1.54(4) . ? C15 C20 1.40(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C11A C15A 1.26(7) . ? C11A C12A 1.29(8) . ? C11A C16A 1.38(7) . ? C12A C17A 1.51(6) . ? C12A C13A 1.53(8) . ? C13A C14A 1.37(8) . ? C13A C18A 1.38(7) . ? C14A C15A 1.29(8) . ? C14A C19A 1.44(7) . ? C15A C20A 1.53(7) . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C31 C32 1.419(9) . ? C31 C32A 1.424(10) . ? C32 N3 1.160(9) . ? C32A N3A 1.162(9) . ? N2 C30 1.304(17) . ? N2 C28 1.361(16) . ? N2 Cu2 1.966(11) 6_556 ? C28 C27 1.338(17) . ? C28 H28 0.9500 . ? C27 C26 1.418(18) . ? C27 H27 0.9500 . ? C26 C29 1.343(19) . ? C29 C30 1.384(19) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? 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 S1 Mo1 S3 106.32(14) . . ? S1 Mo1 S4 106.73(13) . . ? S3 Mo1 S4 100.70(13) . . ? S1 Mo1 C1 143.5(3) . . ? S3 Mo1 C1 95.9(3) . . ? S4 Mo1 C1 96.8(3) . . ? S1 Mo1 C3 86.6(4) . . ? S3 Mo1 C3 141.5(3) . . ? S4 Mo1 C3 110.2(3) . . ? C1 Mo1 C3 58.9(5) . . ? S1 Mo1 C2 117.4(3) . . ? S3 Mo1 C2 131.7(3) . . ? S4 Mo1 C2 86.1(3) . . ? C1 Mo1 C2 35.9(4) . . ? C3 Mo1 C2 34.4(5) . . ? S1 Mo1 C5 117.2(3) . . ? S3 Mo1 C5 84.8(3) . . ? S4 Mo1 C5 132.3(3) . . ? C1 Mo1 C5 35.7(4) . . ? C3 Mo1 C5 57.5(5) . . ? C2 Mo1 C5 58.2(4) . . ? S1 Mo1 C4 85.8(3) . . ? S3 Mo1 C4 108.2(3) . . ? S4 Mo1 C4 143.7(3) . . ? C1 Mo1 C4 59.5(4) . . ? C3 Mo1 C4 35.2(4) . . ? C2 Mo1 C4 58.4(4) . . ? C5 Mo1 C4 34.6(4) . . ? S1 Mo1 Cu1 55.52(10) . . ? S3 Mo1 Cu1 52.18(10) . . ? S4 Mo1 Cu1 102.91(10) . . ? C1 Mo1 Cu1 144.9(3) . . ? C3 Mo1 Cu1 135.7(4) . . ? C2 Mo1 Cu1 169.7(3) . . ? C5 Mo1 Cu1 116.6(3) . . ? C4 Mo1 Cu1 111.9(3) . . ? S1 Mo1 Cu2 55.57(10) . . ? S3 Mo1 Cu2 102.60(11) . . ? S4 Mo1 Cu2 52.54(10) . . ? C1 Mo1 Cu2 146.4(3) . . ? C3 Mo1 Cu2 114.2(3) . . ? C2 Mo1 Cu2 118.2(3) . . ? C5 Mo1 Cu2 170.7(3) . . ? C4 Mo1 Cu2 136.2(3) . . ? Cu1 Mo1 Cu2 65.35(6) . . ? S1 Mo1 Mo2 100.43(10) . . ? S3 Mo1 Mo2 52.13(10) . . ? S4 Mo1 Mo2 52.23(9) . . ? C1 Mo1 Mo2 116.0(3) . . ? C3 Mo1 Mo2 162.3(3) . . ? C2 Mo1 Mo2 131.0(3) . . ? C5 Mo1 Mo2 129.9(3) . . ? C4 Mo1 Mo2 160.3(3) . . ? Cu1 Mo1 Mo2 59.31(5) . . ? Cu2 Mo1 Mo2 59.28(5) . . ? S2 Mo2 S3 105.64(14) . . ? S2 Mo2 S4 106.63(14) . . ? S3 Mo2 S4 100.61(13) . . ? S2 Mo2 C15 103.0(4) . . ? S3 Mo2 C15 140.4(4) . . ? S4 Mo2 C15 96.8(4) . . ? S2 Mo2 C13 105.1(5) . . ? S3 Mo2 C13 88.9(5) . . ? S4 Mo2 C13 142.9(4) . . ? C15 Mo2 C13 57.3(4) . . ? S2 Mo2 C15A 86.2(14) . . ? S3 Mo2 C15A 146.5(15) . . ? S4 Mo2 C15A 105.8(15) . . ? C15 Mo2 C15A 17.2(15) . . ? C13 Mo2 C15A 57.7(16) . . ? S2 Mo2 C13A 111.2(15) . . ? S3 Mo2 C13A 92.8(15) . . ? S4 Mo2 C13A 134.4(15) . . ? C15 Mo2 C13A 51.0(16) . . ? C13 Mo2 C13A 8.6(16) . . ? C15A Mo2 C13A 54(2) . . ? S2 Mo2 C12 139.0(4) . . ? S3 Mo2 C12 84.8(4) . . ? S4 Mo2 C12 110.2(4) . . ? C15 Mo2 C12 55.7(4) . . ? C13 Mo2 C12 34.4(3) . . ? C15A Mo2 C12 67.1(15) . . ? C13A Mo2 C12 27.7(16) . . ? S2 Mo2 C12A 134.4(14) . . ? S3 Mo2 C12A 107.3(14) . . ? S4 Mo2 C12A 97.3(14) . . ? C15 Mo2 C12A 34.7(15) . . ? C13 Mo2 C12A 45.9(14) . . ? C15A Mo2 C12A 49.6(19) . . ? C13A Mo2 C12A 37.3(19) . . ? C12 Mo2 C12A 24.0(14) . . ? S2 Mo2 C14 88.7(4) . . ? S3 Mo2 C14 121.2(5) . . ? S4 Mo2 C14 129.8(4) . . ? C15 Mo2 C14 33.1(3) . . ? C13 Mo2 C14 33.1(3) . . ? C15A Mo2 C14 26.2(16) . . ? C13A Mo2 C14 31.6(16) . . ? C12 Mo2 C14 53.7(4) . . ? C12A Mo2 C14 47.1(14) . . ? S2 Mo2 C11A 113.3(15) . . ? S3 Mo2 C11A 137.6(16) . . ? S4 Mo2 C11A 84.1(14) . . ? C15 Mo2 C11A 14.4(14) . . ? C13 Mo2 C11A 65.9(15) . . ? C15A Mo2 C11A 30.6(18) . . ? C13A Mo2 C11A 58(2) . . ? C12 Mo2 C11A 54.8(15) . . ? C12A Mo2 C11A 31.1(18) . . ? C14 Mo2 C11A 46.6(15) . . ? S2 Mo2 C11 136.8(4) . . ? S3 Mo2 C11 113.9(4) . . ? S4 Mo2 C11 83.1(3) . . ? C15 Mo2 C11 34.0(3) . . ? C13 Mo2 C11 60.5(4) . . ? C15A Mo2 C11 51.0(14) . . ? C13A Mo2 C11 51.9(15) . . ? C12 Mo2 C11 36.4(3) . . ? C12A Mo2 C11 14.7(14) . . ? C14 Mo2 C11 56.4(4) . . ? C11A Mo2 C11 24.2(15) . . ? N1 Cu1 S3 117.3(4) . . ? N1 Cu1 S1 116.3(4) . . ? S3 Cu1 S1 104.85(14) . . ? N1 Cu1 S2 112.5(4) . . ? S3 Cu1 S2 103.18(16) . . ? S1 Cu1 S2 100.59(14) . . ? N1 Cu1 Mo1 147.7(3) . . ? S3 Cu1 Mo1 54.68(10) . . ? S1 Cu1 Mo1 51.50(9) . . ? S2 Cu1 Mo1 99.69(11) . . ? N1 Cu1 Mo2 143.0(4) . . ? S3 Cu1 Mo2 54.09(10) . . ? S1 Cu1 Mo2 100.09(10) . . ? S2 Cu1 Mo2 50.63(11) . . ? Mo1 Cu1 Mo2 62.67(5) . . ? N1 Cu1 Cu2 144.4(4) . . ? S3 Cu1 Cu2 98.18(11) . . ? S1 Cu1 Cu2 51.31(10) . . ? S2 Cu1 Cu2 52.11(10) . . ? Mo1 Cu1 Cu2 57.41(5) . . ? Mo2 Cu1 Cu2 57.82(6) . . ? N2 Cu2 S4 120.9(4) 6 . ? N2 Cu2 S1 116.1(3) 6 . ? S4 Cu2 S1 104.61(13) . . ? N2 Cu2 S2 109.4(3) 6 . ? S4 Cu2 S2 103.18(15) . . ? S1 Cu2 S2 99.94(14) . . ? N2 Cu2 Mo1 150.9(3) 6 . ? S4 Cu2 Mo1 54.55(9) . . ? S1 Cu2 Mo1 51.38(9) . . ? S2 Cu2 Mo1 99.11(11) . . ? N2 Cu2 Mo2 142.4(3) 6 . ? S4 Cu2 Mo2 54.06(10) . . ? S1 Cu2 Mo2 99.91(10) . . ? S2 Cu2 Mo2 50.49(11) . . ? Mo1 Cu2 Mo2 62.59(5) . . ? N2 Cu2 Cu1 140.8(4) 6 . ? S4 Cu2 Cu1 97.99(11) . . ? S1 Cu2 Cu1 51.15(10) . . ? S2 Cu2 Cu1 51.60(10) . . ? Mo1 Cu2 Cu1 57.23(5) . . ? Mo2 Cu2 Cu1 57.78(6) . . ? Mo1 S1 Cu1 72.98(11) . . ? Mo1 S1 Cu2 73.04(11) . . ? Cu1 S1 Cu2 77.54(12) . . ? Mo2 S2 Cu1 73.73(12) . . ? Mo2 S2 Cu2 73.44(12) . . ? Cu1 S2 Cu2 76.29(12) . . ? Cu1 S3 Mo1 73.14(11) . . ? Cu1 S3 Mo2 74.31(13) . . ? Mo1 S3 Mo2 75.77(11) . . ? Cu2 S4 Mo1 72.90(11) . . ? Cu2 S4 Mo2 73.91(12) . . ? Mo1 S4 Mo2 75.60(11) . . ? C21 N1 C23 117.3(13) . . ? C21 N1 Cu1 122.2(10) . . ? C23 N1 Cu1 120.2(9) . . ? C5 C1 C2 105.6(10) . . ? C5 C1 C6 127.8(13) . . ? C2 C1 C6 125.6(13) . . ? C5 C1 Mo1 73.7(7) . . ? C2 C1 Mo1 73.4(7) . . ? C6 C1 Mo1 126.8(10) . . ? C3 C2 C1 108.2(10) . . ? C3 C2 C7 129.5(13) . . ? C1 C2 C7 122.1(12) . . ? C3 C2 Mo1 72.3(7) . . ? C1 C2 Mo1 70.7(7) . . ? C7 C2 Mo1 127.3(9) . . ? C2 C3 C4 110.0(12) . . ? C2 C3 C8 125.3(12) . . ? C4 C3 C8 124.3(13) . . ? C2 C3 Mo1 73.3(7) . . ? C4 C3 Mo1 73.2(7) . . ? C8 C3 Mo1 125.9(10) . . ? C5 C4 C3 106.4(11) . . ? C5 C4 C9 126.4(12) . . ? C3 C4 C9 126.9(13) . . ? C5 C4 Mo1 72.6(7) . . ? C3 C4 Mo1 71.6(7) . . ? C9 C4 Mo1 125.7(9) . . ? C4 C5 C1 109.7(11) . . ? C4 C5 C10 125.1(13) . . ? C1 C5 C10 125.1(13) . . ? C4 C5 Mo1 72.7(7) . . ? C1 C5 Mo1 70.5(7) . . ? C10 C5 Mo1 126.7(10) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C21 C22 124.3(14) . . ? N1 C21 H21 117.9 . . ? C22 C21 H21 117.9 . . ? C25 C22 C21 118.3(13) . . ? C25 C22 H22 120.9 . . ? C21 C22 H22 120.9 . . ? C22 C25 C24 118.5(12) . . ? C22 C25 C26 123.1(12) . . ? C24 C25 C26 118.4(12) . . ? C23 C24 C25 118.5(13) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? N1 C23 C24 122.9(13) . . ? N1 C23 H23 118.5 . . ? C24 C23 H23 118.5 . . ? F1 P1 F2 85.3(10) . . ? F1 P1 F5 95.4(10) . . ? F2 P1 F5 179.3(11) . . ? F1 P1 F6 83.6(9) . . ? F2 P1 F6 93.0(8) . . ? F5 P1 F6 87.0(7) . . ? F1 P1 F3 94.9(9) . . ? F2 P1 F3 85.9(8) . . ? F5 P1 F3 94.1(8) . . ? F6 P1 F3 178.2(8) . . ? F1 P1 F4 176.8(10) . . ? F2 P1 F4 93.5(9) . . ? F5 P1 F4 85.9(8) . . ? F6 P1 F4 93.5(8) . . ? F3 P1 F4 88.0(8) . . ? P2 F7 P2A 23.7(8) . . ? P2A F8 P2 23.8(8) . . ? F7 P2 F12 178.7(11) . . ? F7 P2 F11 89.3(9) . . ? F12 P2 F11 90.0(9) . . ? F7 P2 F9 91.7(9) . . ? F12 P2 F9 88.9(9) . . ? F11 P2 F9 178.9(12) . . ? F7 P2 F10 87.1(9) . . ? F12 P2 F10 91.8(9) . . ? F11 P2 F10 90.1(9) . . ? F9 P2 F10 89.9(9) . . ? F7 P2 F8 88.7(9) . . ? F12 P2 F8 92.4(9) . . ? F11 P2 F8 90.8(9) . . ? F9 P2 F8 89.3(9) . . ? F10 P2 F8 175.7(11) . . ? F8 P2A F10A 178.1(11) . . ? F8 P2A F12A 89.9(9) . . ? F10A P2A F12A 90.7(9) . . ? F8 P2A F11A 88.4(9) . . ? F10A P2A F11A 89.8(9) . . ? F12A P2A F11A 91.8(10) . . ? F8 P2A F9A 91.0(9) . . ? F10A P2A F9A 90.8(10) . . ? F12A P2A F9A 90.5(9) . . ? F11A P2A F9A 177.6(12) . . ? F8 P2A F7 88.6(9) . . ? F10A P2A F7 90.8(9) . . ? F12A P2A F7 176.8(11) . . ? F11A P2A F7 90.9(9) . . ? F9A P2A F7 86.8(9) . . ? C16 C11 C15 133.0 . . ? C16 C11 C12 125.9 . . ? C15 C11 C12 99.5 . . ? C16 C11 Mo2 131.5(5) . . ? C15 C11 Mo2 69.9(6) . . ? C12 C11 Mo2 71.1(6) . . ? C13 C12 C11 111.0 . . ? C13 C12 C17 124.0(14) . . ? C11 C12 C17 125.0(14) . . ? C13 C12 Mo2 70.5(5) . . ? C11 C12 Mo2 72.4(6) . . ? C17 C12 Mo2 125.3(12) . . ? C14 C13 C12 103.9 . . ? C14 C13 C18 129.3(15) . . ? C12 C13 C18 125.7(15) . . ? C14 C13 Mo2 76.4(7) . . ? C12 C13 Mo2 75.0(5) . . ? C18 C13 Mo2 122.5(13) . . ? C13 C14 C15 111.7 . . ? C13 C14 C19 127.2(14) . . ? C15 C14 C19 120.4(14) . . ? C13 C14 Mo2 70.5(7) . . ? C15 C14 Mo2 70.4(6) . . ? C19 C14 Mo2 119.4(14) . . ? C14 C15 C11 112.4 . . ? C14 C15 C20 131.9(15) . . ? C11 C15 C20 115.3(16) . . ? C14 C15 Mo2 76.5(6) . . ? C11 C15 Mo2 76.1(6) . . ? C20 C15 Mo2 120.7(15) . . ? C15A C11A C12A 103(6) . . ? C15A C11A C16A 143(7) . . ? C12A C11A C16A 114(6) . . ? C15A C11A Mo2 72(4) . . ? C12A C11A Mo2 74(4) . . ? C16A C11A Mo2 118(4) . . ? C11A C12A C17A 136(5) . . ? C11A C12A C13A 111(5) . . ? C17A C12A C13A 111(4) . . ? C11A C12A Mo2 75(4) . . ? C17A C12A Mo2 111(3) . . ? C13A C12A Mo2 71(3) . . ? C14A C13A C18A 130(6) . . ? C14A C13A C12A 98(5) . . ? C18A C13A C12A 132(5) . . ? C14A C13A Mo2 76(4) . . ? C18A C13A Mo2 120(4) . . ? C12A C13A Mo2 72(3) . . ? C15A C14A C13A 108(6) . . ? C15A C14A C19A 130(6) . . ? C13A C14A C19A 122(6) . . ? C15A C14A Mo2 71(4) . . ? C13A C14A Mo2 71(4) . . ? C19A C14A Mo2 123(4) . . ? C11A C15A C14A 120(6) . . ? C11A C15A C20A 117(5) . . ? C14A C15A C20A 122(5) . . ? C11A C15A Mo2 78(4) . . ? C14A C15A Mo2 78(4) . . ? C20A C15A Mo2 128(4) . . ? C11A C16A H16D 109.5 . . ? C11A C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? C11A C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? C12A C17A H17D 109.5 . . ? C12A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C12A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C13A C18A H18D 109.5 . . ? C13A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C13A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C14A C19A H19D 109.5 . . ? C14A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C14A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C15A C20A H20D 109.5 . . ? C15A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C15A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C32 C31 C32A 35(3) . . ? N3 C32 C31 175(6) . . ? N3A C32A C31 172(8) . . ? C30 N2 C28 119.4(12) . . ? C30 N2 Cu2 119.9(9) . 6_556 ? C28 N2 Cu2 120.7(9) . 6_556 ? C27 C28 N2 121.4(12) . . ? C27 C28 H28 119.3 . . ? N2 C28 H28 119.3 . . ? C28 C27 C26 121.2(12) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C29 C26 C27 114.4(12) . . ? C29 C26 C25 124.4(12) . . ? C27 C26 C25 120.8(12) . . ? C26 C29 C30 123.5(13) . . ? C26 C29 H29 118.3 . . ? C30 C29 H29 118.3 . . ? N2 C30 C29 120.1(13) . . ? N2 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.447 _refine_diff_density_min -1.578 _refine_diff_density_rms 0.236 #===END #============================================================================== data_5(aniline) _database_code_depnum_ccdc_archive 'CCDC 679378' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 Cu2 Mo2 N2 S4, 2(C6H5N),2(ClO4)' _chemical_formula_sum 'C44 H50 Cl2 Cu2 Mo2 N4 O8 S4' _chemical_formula_weight 1285.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 25.290(5) _cell_length_b 8.5496(17) _cell_length_c 30.769(11) _cell_angle_alpha 90.00 _cell_angle_beta 127.255(19) _cell_angle_gamma 90.00 _cell_volume 5295(2) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 16895 _cell_measurement_theta_min 3.0357 _cell_measurement_theta_max 25.3491 _exptl_crystal_description prism _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2599 _exptl_absorpt_coefficient_mu 1.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4486 _exptl_absorpt_correction_T_max 0.7246 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 49851 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.35 _reflns_number_total 9696 _reflns_number_gt 8766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+16.5000P] 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 9696 _refine_ls_number_parameters 591 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1759 _refine_ls_wR_factor_gt 0.1719 _refine_ls_goodness_of_fit_ref 1.362 _refine_ls_restrained_S_all 1.362 _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 0.42966(3) 0.45732(6) 0.22176(2) 0.02443(16) Uani 1 1 d . . . Cu1 Cu 0.51287(4) 0.24526(9) 0.30392(3) 0.0318(2) Uani 1 1 d . . . S1 S 0.41113(8) 0.19939(18) 0.21397(7) 0.0305(4) Uani 1 1 d . . . S2 S 0.51287(8) 0.50675(18) 0.31391(6) 0.0294(3) Uani 1 1 d . . . N1 N 0.5157(3) 0.1362(6) 0.3608(2) 0.0314(12) Uani 1 1 d . . . C1 C 0.3764(4) 0.6808(8) 0.2238(3) 0.0372(16) Uani 1 1 d . . . C2 C 0.3665(3) 0.6791(8) 0.1734(3) 0.0390(16) Uani 1 1 d . . . C3 C 0.3275(4) 0.5465(8) 0.1427(3) 0.0406(17) Uani 1 1 d . . . C4 C 0.3117(4) 0.4670(9) 0.1745(3) 0.0460(18) Uani 1 1 d . . . C5 C 0.3441(4) 0.5470(8) 0.2251(3) 0.0398(17) Uani 1 1 d . . . C6 C 0.4097(5) 0.8097(9) 0.2660(4) 0.055(2) Uani 1 1 d . . . H6A H 0.3771 0.8913 0.2566 0.083 Uiso 1 1 calc R . . H6B H 0.4459 0.8547 0.2668 0.083 Uiso 1 1 calc R . . H6C H 0.4276 0.7666 0.3020 0.083 Uiso 1 1 calc R . . C7 C 0.3882(5) 0.8062(9) 0.1532(4) 0.055(2) Uani 1 1 d . . . H7A H 0.4331 0.8411 0.1831 0.082 Uiso 1 1 calc R . . H7B H 0.3574 0.8947 0.1398 0.082 Uiso 1 1 calc R . . H7C H 0.3881 0.7653 0.1234 0.082 Uiso 1 1 calc R . . C8 C 0.3013(4) 0.5060(12) 0.0858(3) 0.062(2) Uani 1 1 d . . . H8A H 0.3366 0.5188 0.0817 0.093 Uiso 1 1 calc R . . H8B H 0.2641 0.5754 0.0601 0.093 Uiso 1 1 calc R . . H8C H 0.2860 0.3972 0.0781 0.093 Uiso 1 1 calc R . . C9 C 0.2653(4) 0.3341(11) 0.1552(4) 0.066(3) Uani 1 1 d . . . H9A H 0.2215 0.3725 0.1423 0.100 Uiso 1 1 calc R . . H9B H 0.2820 0.2603 0.1853 0.100 Uiso 1 1 calc R . . H9C H 0.2616 0.2812 0.1252 0.100 Uiso 1 1 calc R . . C10 C 0.3371(5) 0.5140(11) 0.2692(4) 0.060(2) Uani 1 1 d . . . H10A H 0.3263 0.4033 0.2681 0.090 Uiso 1 1 calc R . . H10B H 0.3015 0.5788 0.2636 0.090 Uiso 1 1 calc R . . H10C H 0.3790 0.5383 0.3049 0.090 Uiso 1 1 calc R . . C11 C 0.5723(4) 0.0859(9) 0.4069(3) 0.0378(16) Uani 1 1 d . . . H11 H 0.6114 0.0827 0.4090 0.045 Uiso 1 1 calc R . . C12 C 0.5758(4) 0.0382(9) 0.4515(3) 0.0398(17) Uani 1 1 d . . . H12 H 0.6167 0.0017 0.4834 0.048 Uiso 1 1 calc R . . C13 C 0.5202(3) 0.0434(8) 0.4501(3) 0.0360(16) Uani 1 1 d . . . C14 C 0.4614(4) 0.0945(11) 0.4014(3) 0.051(2) Uani 1 1 d . . . H14 H 0.4215 0.0997 0.3981 0.061 Uiso 1 1 calc R . . C15 C 0.4613(4) 0.1372(10) 0.3585(3) 0.0470(19) Uani 1 1 d . . . H15 H 0.4206 0.1691 0.3254 0.056 Uiso 1 1 calc R . . C16 C 0.5248(4) 0.0027(9) 0.4983(3) 0.0424(17) Uani 1 1 d . . . H16 H 0.5677 -0.0225 0.5305 0.051 Uiso 1 1 calc R . . Mo2 Mo 0.07024(3) 0.44276(6) 0.29228(2) 0.02607(16) Uani 1 1 d . . . Cu2 Cu 0.01329(5) 0.23142(9) 0.20941(3) 0.0355(2) Uani 1 1 d . . . S3 S 0.08817(9) 0.18416(19) 0.30276(7) 0.0340(4) Uani 1 1 d . . . S4 S 0.01399(9) 0.49233(19) 0.19966(7) 0.0311(4) Uani 1 1 d . . . N2 N 0.0176(3) 0.1268(7) 0.1558(2) 0.0364(13) Uani 1 1 d . . . C17 C 0.1233(4) 0.6653(8) 0.3475(3) 0.0388(16) Uani 1 1 d . . . C18 C 0.1551(4) 0.5292(9) 0.3814(3) 0.0417(17) Uani 1 1 d . . . C19 C 0.1878(4) 0.4512(9) 0.3638(3) 0.0455(18) Uani 1 1 d . . . C20 C 0.1734(4) 0.5326(9) 0.3167(3) 0.0432(18) Uani 1 1 d . . . C21 C 0.1347(4) 0.6655(9) 0.3080(3) 0.0418(17) Uani 1 1 d . . . C22 C 0.0897(4) 0.7923(9) 0.3561(3) 0.051(2) Uani 1 1 d . . . H22A H 0.0517 0.8320 0.3207 0.077 Uiso 1 1 calc R . . H22B H 0.1212 0.8776 0.3771 0.077 Uiso 1 1 calc R . . H22C H 0.0743 0.7504 0.3763 0.077 Uiso 1 1 calc R . . C23 C 0.1588(5) 0.4925(11) 0.4311(3) 0.060(2) Uani 1 1 d . . . H23A H 0.1929 0.5581 0.4617 0.090 Uiso 1 1 calc R . . H23B H 0.1703 0.3820 0.4408 0.090 Uiso 1 1 calc R . . H23C H 0.1157 0.5135 0.4232 0.090 Uiso 1 1 calc R . . C24 C 0.2342(4) 0.3140(12) 0.3916(4) 0.071(3) Uani 1 1 d . . . H24A H 0.2275 0.2648 0.4167 0.107 Uiso 1 1 calc R . . H24B H 0.2802 0.3502 0.4121 0.107 Uiso 1 1 calc R . . H24C H 0.2251 0.2377 0.3640 0.107 Uiso 1 1 calc R . . C25 C 0.2010(5) 0.4930(12) 0.2865(4) 0.065(2) Uani 1 1 d . . . H25A H 0.2496 0.4921 0.3120 0.097 Uiso 1 1 calc R . . H25B H 0.1863 0.5713 0.2580 0.097 Uiso 1 1 calc R . . H25C H 0.1850 0.3895 0.2697 0.097 Uiso 1 1 calc R . . C26 C 0.1152(5) 0.7903(9) 0.2671(4) 0.057(2) Uani 1 1 d . . . H26A H 0.1491 0.8725 0.2838 0.085 Uiso 1 1 calc R . . H26B H 0.0725 0.8351 0.2546 0.085 Uiso 1 1 calc R . . H26C H 0.1112 0.7456 0.2359 0.085 Uiso 1 1 calc R . . C27 C 0.0750(4) 0.0996(11) 0.1646(3) 0.051(2) Uani 1 1 d . . . H27 H 0.1150 0.1107 0.2006 0.061 Uiso 1 1 calc R . . C28 C 0.0789(4) 0.0559(12) 0.1234(3) 0.059(3) Uani 1 1 d . . . H28 H 0.1210 0.0372 0.1314 0.071 Uiso 1 1 calc R . . C29 C 0.0212(4) 0.0392(8) 0.0704(3) 0.0380(16) Uani 1 1 d . . . C30 C -0.0388(4) 0.0609(9) 0.0619(3) 0.0410(17) Uani 1 1 d . . . H30 H -0.0797 0.0464 0.0267 0.049 Uiso 1 1 calc R . . C31 C -0.0383(4) 0.1035(9) 0.1052(3) 0.0393(16) Uani 1 1 d . . . H31 H -0.0797 0.1172 0.0990 0.047 Uiso 1 1 calc R . . C32 C 0.0252(4) -0.0011(10) 0.0263(3) 0.0474(19) Uani 1 1 d . . . H32 H 0.0674 -0.0313 0.0362 0.057 Uiso 1 1 calc R . . N3 N 0.2139(7) 0.8484(16) 0.1296(6) 0.120(5) Uani 1 1 d . . . H3A H 0.2246 0.8908 0.1098 0.144 Uiso 1 1 calc R . . H3B H 0.2305 0.8865 0.1621 0.144 Uiso 1 1 calc R . . C33 C 0.1714(8) 0.723(2) 0.1097(7) 0.104(5) Uani 1 1 d . . . C34 C 0.1532(8) 0.6684(19) 0.1404(6) 0.098(4) Uani 1 1 d . . . H34 H 0.1708 0.7121 0.1751 0.118 Uiso 1 1 calc R . . C35 C 0.1084(8) 0.548(3) 0.1191(8) 0.141(8) Uani 1 1 d . . . H35 H 0.0937 0.5091 0.1392 0.169 Uiso 1 1 calc R . . C36 C 0.0830(7) 0.478(2) 0.0674(8) 0.136(6) Uani 1 1 d . . . H36 H 0.0548 0.3893 0.0536 0.163 Uiso 1 1 calc R . . C37 C 0.1032(11) 0.553(3) 0.0386(8) 0.156(11) Uani 1 1 d . . . H37 H 0.0845 0.5193 0.0025 0.187 Uiso 1 1 calc R . . C38 C 0.1466(10) 0.666(3) 0.0599(7) 0.120(7) Uani 1 1 d . . . H38 H 0.1609 0.7092 0.0401 0.144 Uiso 1 1 calc R . . N4 N 0.2893(6) 0.8206(15) 0.4128(4) 0.103(3) Uani 1 1 d . . . H4A H 0.2693 0.8570 0.4262 0.124 Uiso 1 1 calc R . . H4B H 0.2821 0.8643 0.3837 0.124 Uiso 1 1 calc R . . C39 C 0.3321(7) 0.6947(19) 0.4375(5) 0.097(4) Uani 1 1 d . . . C40 C 0.3655(7) 0.628(2) 0.4180(6) 0.105(5) Uani 1 1 d . . . H40 H 0.3572 0.6691 0.3857 0.126 Uiso 1 1 calc R . . C41 C 0.4080(8) 0.510(2) 0.4434(9) 0.128(6) Uani 1 1 d . . . H41 H 0.4307 0.4732 0.4297 0.154 Uiso 1 1 calc R . . C42 C 0.4201(8) 0.440(2) 0.4882(9) 0.123(6) Uani 1 1 d . . . H42 H 0.4500 0.3546 0.5053 0.147 Uiso 1 1 calc R . . C43 C 0.3868(8) 0.499(2) 0.5083(6) 0.118(5) Uani 1 1 d . . . H43 H 0.3938 0.4521 0.5394 0.141 Uiso 1 1 calc R . . C44 C 0.3448(6) 0.6223(17) 0.4837(5) 0.089(4) Uani 1 1 d . . . H44 H 0.3233 0.6606 0.4983 0.107 Uiso 1 1 calc R . . Cl1 Cl 0.26962(12) 0.0181(4) 0.28186(11) 0.0743(6) Uani 1 1 d . . . Cl2 Cl 0.2264(4) 0.0493(10) 0.0120(3) 0.0690(15) Uani 0.496(5) 1 d P A 1 O5 O 0.1720(6) 0.1543(17) -0.0027(5) 0.0690(15) Uani 0.496(5) 1 d P A 1 O6 O 0.1909(6) -0.0865(18) -0.0161(5) 0.0690(15) Uani 0.496(5) 1 d P A 1 O7 O 0.2538(6) 0.1350(18) -0.0093(5) 0.0690(15) Uani 0.496(5) 1 d P A 1 O8 O 0.2658(6) 0.0445(19) 0.0676(5) 0.0690(15) Uani 0.496(5) 1 d P A 1 O1 O 0.2356(6) 0.0471(19) 0.2261(6) 0.0743(6) Uani 0.496(5) 1 d P A 1 O2 O 0.3115(6) 0.1680(19) 0.3051(6) 0.0743(6) Uani 0.496(5) 1 d P A 1 O3 O 0.3157(7) -0.096(2) 0.3067(6) 0.0743(6) Uani 0.496(5) 1 d P A 1 O4 O 0.2313(7) 0.050(2) 0.3014(6) 0.0743(6) Uani 0.496(5) 1 d P A 1 O1A O 0.2258(6) -0.0989(19) 0.2353(5) 0.0743(6) Uani 0.504(5) 1 d P A 2 O2A O 0.3046(6) 0.0996(19) 0.2693(6) 0.0743(6) Uani 0.504(5) 1 d P A 2 O3A O 0.3103(6) -0.0872(19) 0.3285(6) 0.0743(6) Uani 0.504(5) 1 d P A 2 O4A O 0.2184(7) 0.084(2) 0.2808(6) 0.0743(6) Uani 0.504(5) 1 d P A 2 Cl2A Cl 0.2400(4) -0.0077(12) 0.0113(4) 0.093(2) Uani 0.504(5) 1 d P A 2 O5A O 0.2922(7) -0.103(2) 0.0178(5) 0.093(2) Uani 0.504(5) 1 d P A 2 O6A O 0.2815(7) 0.090(2) 0.0615(6) 0.093(2) Uani 0.504(5) 1 d P A 2 O7A O 0.2058(7) -0.117(2) 0.0194(6) 0.093(2) Uani 0.504(5) 1 d P A 2 O8A O 0.2044(7) 0.038(2) -0.0389(6) 0.093(2) Uani 0.504(5) 1 d P A 2 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 0.0335(3) 0.0197(3) 0.0258(3) 0.0000(2) 0.0209(2) 0.0016(2) Cu1 0.0518(5) 0.0242(4) 0.0316(4) 0.0030(3) 0.0315(4) -0.0012(4) S1 0.0413(9) 0.0232(8) 0.0329(8) -0.0027(6) 0.0256(8) -0.0050(7) S2 0.0424(9) 0.0254(8) 0.0285(8) -0.0050(6) 0.0257(7) -0.0027(7) N1 0.040(3) 0.030(3) 0.027(3) 0.006(2) 0.022(3) 0.000(2) C1 0.047(4) 0.025(3) 0.049(4) 0.000(3) 0.034(4) 0.015(3) C2 0.038(4) 0.031(4) 0.043(4) 0.011(3) 0.022(3) 0.012(3) C3 0.037(4) 0.037(4) 0.038(4) 0.004(3) 0.017(3) 0.010(3) C4 0.043(4) 0.042(4) 0.055(5) -0.002(4) 0.030(4) 0.006(3) C5 0.040(4) 0.039(4) 0.051(4) 0.005(3) 0.033(4) 0.011(3) C6 0.072(6) 0.038(4) 0.061(5) -0.010(4) 0.044(5) 0.006(4) C7 0.071(6) 0.038(4) 0.064(5) 0.030(4) 0.045(5) 0.022(4) C8 0.056(5) 0.072(6) 0.033(4) 0.009(4) 0.013(4) 0.024(5) C9 0.035(4) 0.062(6) 0.086(7) 0.002(5) 0.028(5) -0.004(4) C10 0.076(6) 0.057(5) 0.080(6) 0.011(5) 0.065(6) 0.017(5) C11 0.040(4) 0.049(4) 0.033(4) 0.009(3) 0.027(3) 0.009(3) C12 0.040(4) 0.055(5) 0.028(3) 0.016(3) 0.022(3) 0.014(3) C13 0.040(4) 0.043(4) 0.027(3) 0.006(3) 0.022(3) 0.000(3) C14 0.034(4) 0.087(6) 0.032(4) 0.019(4) 0.020(3) -0.001(4) C15 0.034(4) 0.074(6) 0.030(4) 0.018(4) 0.018(3) 0.004(4) C16 0.047(4) 0.055(4) 0.029(4) 0.010(3) 0.024(3) 0.000(4) Mo2 0.0344(3) 0.0228(3) 0.0261(3) -0.0015(2) 0.0209(3) -0.0003(2) Cu2 0.0576(5) 0.0285(4) 0.0334(4) -0.0037(3) 0.0343(4) 0.0016(4) S3 0.0495(10) 0.0255(8) 0.0332(9) 0.0039(7) 0.0283(8) 0.0073(7) S4 0.0417(9) 0.0293(8) 0.0314(8) 0.0048(7) 0.0269(8) 0.0000(7) N2 0.047(3) 0.036(3) 0.032(3) -0.005(3) 0.027(3) 0.008(3) C17 0.042(4) 0.035(4) 0.039(4) -0.010(3) 0.024(3) -0.009(3) C18 0.040(4) 0.050(4) 0.028(4) -0.010(3) 0.017(3) -0.012(3) C19 0.036(4) 0.047(5) 0.039(4) -0.006(3) 0.015(3) 0.000(3) C20 0.039(4) 0.046(4) 0.050(4) -0.012(4) 0.029(4) -0.012(3) C21 0.043(4) 0.036(4) 0.042(4) -0.009(3) 0.024(3) -0.015(3) C22 0.064(5) 0.033(4) 0.058(5) -0.015(4) 0.038(4) -0.007(4) C23 0.079(6) 0.061(5) 0.032(4) -0.007(4) 0.029(4) -0.015(5) C24 0.044(5) 0.073(7) 0.062(6) 0.008(5) 0.014(4) 0.011(5) C25 0.056(5) 0.080(6) 0.079(7) -0.010(5) 0.051(5) -0.007(5) C26 0.068(6) 0.037(4) 0.067(6) 0.001(4) 0.042(5) -0.017(4) C27 0.051(5) 0.070(5) 0.026(4) -0.005(4) 0.020(3) 0.016(4) C28 0.042(4) 0.101(7) 0.031(4) -0.008(4) 0.020(4) 0.024(5) C29 0.043(4) 0.044(4) 0.027(3) -0.006(3) 0.021(3) 0.005(3) C30 0.042(4) 0.051(4) 0.034(4) -0.011(3) 0.025(3) -0.002(3) C31 0.044(4) 0.044(4) 0.039(4) -0.011(3) 0.030(3) -0.005(3) C32 0.045(4) 0.066(5) 0.032(4) -0.009(4) 0.024(3) 0.010(4) N3 0.157(12) 0.120(10) 0.152(12) 0.041(9) 0.129(11) 0.055(9) C33 0.096(10) 0.132(13) 0.106(11) 0.058(10) 0.073(9) 0.071(9) C34 0.097(10) 0.129(12) 0.089(9) 0.034(9) 0.067(9) 0.042(9) C35 0.083(10) 0.24(2) 0.120(14) 0.066(15) 0.072(11) 0.067(13) C36 0.072(9) 0.158(17) 0.111(13) -0.003(12) 0.020(9) 0.019(9) C37 0.122(16) 0.25(3) 0.075(11) 0.049(15) 0.050(12) 0.101(17) C38 0.118(13) 0.173(18) 0.079(11) 0.060(11) 0.066(10) 0.090(13) N4 0.103(8) 0.130(10) 0.069(6) -0.014(7) 0.048(6) -0.018(8) C39 0.080(8) 0.125(12) 0.067(8) -0.029(8) 0.036(7) -0.043(8) C40 0.080(8) 0.163(15) 0.084(9) -0.024(10) 0.056(8) -0.037(10) C41 0.080(10) 0.149(16) 0.155(17) -0.054(14) 0.071(12) -0.033(11) C42 0.085(10) 0.115(13) 0.148(16) 0.001(11) 0.060(11) -0.018(9) C43 0.078(9) 0.145(14) 0.082(9) 0.011(10) 0.023(8) -0.039(10) C44 0.084(8) 0.109(10) 0.067(7) -0.018(7) 0.042(7) -0.036(8) Cl1 0.0507(11) 0.1062(18) 0.0698(14) 0.0116(13) 0.0385(11) 0.0009(11) Cl2 0.044(2) 0.102(4) 0.047(2) 0.004(3) 0.021(2) -0.024(2) O5 0.044(2) 0.102(4) 0.047(2) 0.004(3) 0.021(2) -0.024(2) O6 0.044(2) 0.102(4) 0.047(2) 0.004(3) 0.021(2) -0.024(2) O7 0.044(2) 0.102(4) 0.047(2) 0.004(3) 0.021(2) -0.024(2) O8 0.044(2) 0.102(4) 0.047(2) 0.004(3) 0.021(2) -0.024(2) O1 0.0507(11) 0.1062(18) 0.0698(14) 0.0116(13) 0.0385(11) 0.0009(11) O2 0.0507(11) 0.1062(18) 0.0698(14) 0.0116(13) 0.0385(11) 0.0009(11) O3 0.0507(11) 0.1062(18) 0.0698(14) 0.0116(13) 0.0385(11) 0.0009(11) O4 0.0507(11) 0.1062(18) 0.0698(14) 0.0116(13) 0.0385(11) 0.0009(11) O1A 0.0507(11) 0.1062(18) 0.0698(14) 0.0116(13) 0.0385(11) 0.0009(11) O2A 0.0507(11) 0.1062(18) 0.0698(14) 0.0116(13) 0.0385(11) 0.0009(11) O3A 0.0507(11) 0.1062(18) 0.0698(14) 0.0116(13) 0.0385(11) 0.0009(11) O4A 0.0507(11) 0.1062(18) 0.0698(14) 0.0116(13) 0.0385(11) 0.0009(11) Cl2A 0.058(3) 0.136(6) 0.054(3) 0.017(3) 0.017(2) -0.026(3) O5A 0.058(3) 0.136(6) 0.054(3) 0.017(3) 0.017(2) -0.026(3) O6A 0.058(3) 0.136(6) 0.054(3) 0.017(3) 0.017(2) -0.026(3) O7A 0.058(3) 0.136(6) 0.054(3) 0.017(3) 0.017(2) -0.026(3) O8A 0.058(3) 0.136(6) 0.054(3) 0.017(3) 0.017(2) -0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 S1 2.2370(17) . ? Mo1 S2 2.3286(19) . ? Mo1 S2 2.3295(17) 2_655 ? Mo1 C2 2.341(7) . ? Mo1 C5 2.357(7) . ? Mo1 C3 2.359(7) . ? Mo1 C1 2.361(6) . ? Mo1 C4 2.402(8) . ? Mo1 Cu1 2.7230(10) 2_655 ? Mo1 Cu1 2.7686(12) . ? Mo1 Mo1 2.8624(14) 2_655 ? Cu1 N1 1.947(5) . ? Cu1 S2 2.2567(18) . ? Cu1 S1 2.3308(18) 2_655 ? Cu1 S1 2.411(2) . ? Cu1 Mo1 2.7230(10) 2_655 ? Cu1 Cu1 2.9696(19) 2_655 ? S1 Cu1 2.3308(18) 2_655 ? S2 Mo1 2.3295(17) 2_655 ? N1 C15 1.332(9) . ? N1 C11 1.336(9) . ? C1 C2 1.413(10) . ? C1 C5 1.420(10) . ? C1 C6 1.512(10) . ? C2 C3 1.422(10) . ? C2 C7 1.511(10) . ? C3 C4 1.431(11) . ? C3 C8 1.491(11) . ? C4 C5 1.422(11) . ? C4 C9 1.476(11) . ? C5 C10 1.498(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.385(9) . ? C11 H11 0.9500 . ? C12 C13 1.380(10) . ? C12 H12 0.9500 . ? C13 C14 1.397(10) . ? C13 C16 1.458(9) . ? C14 C15 1.370(10) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C16 1.320(15) 3_656 ? C16 H16 0.9500 . ? Mo2 S3 2.2407(17) . ? Mo2 S4 2.3274(19) . ? Mo2 S4 2.3277(17) 2 ? Mo2 C17 2.355(7) . ? Mo2 C18 2.356(7) . ? Mo2 C21 2.359(7) . ? Mo2 C20 2.364(7) . ? Mo2 C19 2.401(7) . ? Mo2 Cu2 2.7194(12) . ? Mo2 Cu2 2.7563(11) 2 ? Mo2 Mo2 2.8634(15) 2 ? Cu2 N2 1.936(5) . ? Cu2 S4 2.2523(19) . ? Cu2 S3 2.327(2) . ? Cu2 S3 2.393(2) 2 ? Cu2 Mo2 2.7563(11) 2 ? Cu2 Cu2 2.9540(18) 2 ? S3 Cu2 2.393(2) 2 ? S4 Mo2 2.3277(17) 2 ? N2 C27 1.327(10) . ? N2 C31 1.341(9) . ? C17 C21 1.410(10) . ? C17 C18 1.440(11) . ? C17 C22 1.498(10) . ? C18 C19 1.402(11) . ? C18 C23 1.507(10) . ? C19 C20 1.442(11) . ? C19 C24 1.507(11) . ? C20 C21 1.415(11) . ? C20 C25 1.499(11) . ? C21 C26 1.488(11) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.380(10) . ? C27 H27 0.9500 . ? C28 C29 1.389(10) . ? C28 H28 0.9500 . ? C29 C30 1.389(10) . ? C29 C32 1.462(9) . ? C30 C31 1.373(9) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C32 1.321(15) 3 ? C32 H32 0.9500 . ? N3 C33 1.374(19) . ? N3 H3A 0.8800 . ? N3 H3B 0.8800 . ? C33 C38 1.35(2) . ? C33 C34 1.360(18) . ? C34 C35 1.37(2) . ? C34 H34 0.9500 . ? C35 C36 1.44(2) . ? C35 H35 0.9500 . ? C36 C37 1.41(3) . ? C36 H36 0.9500 . ? C37 C38 1.31(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? N4 C39 1.383(18) . ? N4 H4A 0.8800 . ? N4 H4B 0.8800 . ? C39 C44 1.398(17) . ? C39 C40 1.417(19) . ? C40 C41 1.33(2) . ? C40 H40 0.9500 . ? C41 C42 1.35(2) . ? C41 H41 0.9500 . ? C42 C43 1.41(2) . ? C42 H42 0.9500 . ? C43 C44 1.36(2) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? Cl1 O3 1.347(15) . ? Cl1 O2A 1.352(13) . ? Cl1 O4A 1.392(15) . ? Cl1 O1 1.399(14) . ? Cl1 O4 1.442(15) . ? Cl1 O3A 1.463(15) . ? Cl1 O2 1.536(15) . ? Cl1 O1A 1.536(16) . ? Cl2 O8 1.363(15) . ? Cl2 O6 1.401(16) . ? Cl2 O7 1.412(15) . ? Cl2 O5 1.467(16) . ? Cl2A O8A 1.293(16) . ? Cl2A O7A 1.395(18) . ? Cl2A O5A 1.46(2) . ? Cl2A O6A 1.49(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 S1 Mo1 S2 106.60(6) . . ? S1 Mo1 S2 106.16(6) . 2_655 ? S2 Mo1 S2 100.31(6) . 2_655 ? S1 Mo1 C2 135.42(19) . . ? S2 Mo1 C2 113.11(19) . . ? S2 Mo1 C2 86.22(19) 2_655 . ? S1 Mo1 C5 100.78(19) . . ? S2 Mo1 C5 93.7(2) . . ? S2 Mo1 C5 144.40(18) 2_655 . ? C2 Mo1 C5 58.2(3) . . ? S1 Mo1 C3 100.41(18) . . ? S2 Mo1 C3 144.59(18) . . ? S2 Mo1 C3 93.6(2) 2_655 . ? C2 Mo1 C3 35.2(2) . . ? C5 Mo1 C3 58.5(3) . . ? S1 Mo1 C1 135.63(19) . . ? S2 Mo1 C1 86.01(18) . . ? S2 Mo1 C1 113.25(18) 2_655 . ? C2 Mo1 C1 35.0(2) . . ? C5 Mo1 C1 35.0(2) . . ? C3 Mo1 C1 58.6(3) . . ? S1 Mo1 C4 82.32(19) . . ? S2 Mo1 C4 127.4(2) . . ? S2 Mo1 C4 127.5(2) 2_655 . ? C2 Mo1 C4 57.8(3) . . ? C5 Mo1 C4 34.8(3) . . ? C3 Mo1 C4 35.0(3) . . ? C1 Mo1 C4 57.9(3) . . ? S1 Mo1 Cu1 55.01(5) . 2_655 ? S2 Mo1 Cu1 103.09(5) . 2_655 ? S2 Mo1 Cu1 52.35(4) 2_655 2_655 ? C2 Mo1 Cu1 129.32(19) . 2_655 ? C5 Mo1 Cu1 153.53(19) . 2_655 ? C3 Mo1 Cu1 111.12(18) . 2_655 ? C1 Mo1 Cu1 163.78(18) . 2_655 ? C4 Mo1 Cu1 122.19(19) . 2_655 ? S1 Mo1 Cu1 56.39(5) . . ? S2 Mo1 Cu1 51.68(5) . . ? S2 Mo1 Cu1 101.70(5) 2_655 . ? C2 Mo1 Cu1 163.62(19) . . ? C5 Mo1 Cu1 112.55(18) . . ? C3 Mo1 Cu1 154.93(19) . . ? C1 Mo1 Cu1 129.52(18) . . ? C4 Mo1 Cu1 123.7(2) . . ? Cu1 Mo1 Cu1 65.46(4) 2_655 . ? S1 Mo1 Mo1 99.66(5) . 2_655 ? S2 Mo1 Mo1 52.10(5) . 2_655 ? S2 Mo1 Mo1 52.07(5) 2_655 2_655 ? C2 Mo1 Mo1 120.32(18) . 2_655 ? C5 Mo1 Mo1 144.13(19) . 2_655 ? C3 Mo1 Mo1 144.02(19) . 2_655 ? C1 Mo1 Mo1 120.24(18) . 2_655 ? C4 Mo1 Mo1 178.02(19) . 2_655 ? Cu1 Mo1 Mo1 59.37(3) 2_655 2_655 ? Cu1 Mo1 Mo1 57.81(3) . 2_655 ? N1 Cu1 S2 110.80(17) . . ? N1 Cu1 S1 123.06(17) . 2_655 ? S2 Cu1 S1 105.47(6) . 2_655 ? N1 Cu1 S1 112.78(17) . . ? S2 Cu1 S1 103.27(6) . . ? S1 Cu1 S1 99.27(7) 2_655 . ? N1 Cu1 Mo1 147.63(17) . 2_655 ? S2 Cu1 Mo1 54.82(5) . 2_655 ? S1 Cu1 Mo1 51.84(4) 2_655 2_655 ? S1 Cu1 Mo1 99.29(5) . 2_655 ? N1 Cu1 Mo1 136.78(17) . . ? S2 Cu1 Mo1 54.05(5) . . ? S1 Cu1 Mo1 100.03(5) 2_655 . ? S1 Cu1 Mo1 50.60(4) . . ? Mo1 Cu1 Mo1 62.82(3) 2_655 . ? N1 Cu1 Cu1 150.34(16) . 2_655 ? S2 Cu1 Cu1 97.71(4) . 2_655 ? S1 Cu1 Cu1 52.44(5) 2_655 2_655 ? S1 Cu1 Cu1 50.03(5) . 2_655 ? Mo1 Cu1 Cu1 58.01(3) 2_655 2_655 ? Mo1 Cu1 Cu1 56.53(3) . 2_655 ? Mo1 S1 Cu1 73.15(5) . 2_655 ? Mo1 S1 Cu1 73.01(5) . . ? Cu1 S1 Cu1 77.53(6) 2_655 . ? Cu1 S2 Mo1 74.27(5) . . ? Cu1 S2 Mo1 72.83(5) . 2_655 ? Mo1 S2 Mo1 75.83(6) . 2_655 ? C15 N1 C11 117.9(6) . . ? C15 N1 Cu1 118.3(5) . . ? C11 N1 Cu1 122.7(5) . . ? C2 C1 C5 107.5(6) . . ? C2 C1 C6 125.9(7) . . ? C5 C1 C6 126.3(7) . . ? C2 C1 Mo1 71.8(4) . . ? C5 C1 Mo1 72.3(4) . . ? C6 C1 Mo1 125.7(5) . . ? C1 C2 C3 109.1(6) . . ? C1 C2 C7 125.3(7) . . ? C3 C2 C7 125.3(7) . . ? C1 C2 Mo1 73.3(4) . . ? C3 C2 Mo1 73.1(4) . . ? C7 C2 Mo1 124.5(5) . . ? C2 C3 C4 107.1(7) . . ? C2 C3 C8 127.0(8) . . ? C4 C3 C8 125.6(8) . . ? C2 C3 Mo1 71.7(4) . . ? C4 C3 Mo1 74.2(4) . . ? C8 C3 Mo1 124.5(5) . . ? C5 C4 C3 107.8(7) . . ? C5 C4 C9 127.0(8) . . ? C3 C4 C9 125.0(8) . . ? C5 C4 Mo1 70.9(4) . . ? C3 C4 Mo1 70.9(4) . . ? C9 C4 Mo1 127.6(5) . . ? C1 C5 C4 108.4(7) . . ? C1 C5 C10 124.3(7) . . ? C4 C5 C10 126.7(7) . . ? C1 C5 Mo1 72.6(4) . . ? C4 C5 Mo1 74.4(4) . . ? C10 C5 Mo1 126.4(5) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 122.0(6) . . ? N1 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C13 C12 C11 120.5(6) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 116.5(6) . . ? C12 C13 C16 120.5(6) . . ? C14 C13 C16 122.9(7) . . ? C15 C14 C13 119.8(7) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? N1 C15 C14 123.2(7) . . ? N1 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? C16 C16 C13 126.3(9) 3_656 . ? C16 C16 H16 116.8 3_656 . ? C13 C16 H16 116.8 . . ? S3 Mo2 S4 106.04(6) . . ? S3 Mo2 S4 106.43(6) . 2 ? S4 Mo2 S4 100.19(6) . 2 ? S3 Mo2 C17 135.74(19) . . ? S4 Mo2 C17 113.28(19) . . ? S4 Mo2 C17 86.23(18) 2 . ? S3 Mo2 C18 100.4(2) . . ? S4 Mo2 C18 145.0(2) . . ? S4 Mo2 C18 93.8(2) 2 . ? C17 Mo2 C18 35.6(3) . . ? S3 Mo2 C21 135.4(2) . . ? S4 Mo2 C21 86.44(19) . . ? S4 Mo2 C21 113.3(2) 2 . ? C17 Mo2 C21 34.8(3) . . ? C18 Mo2 C21 58.6(3) . . ? S3 Mo2 C20 100.8(2) . . ? S4 Mo2 C20 93.9(2) . . ? S4 Mo2 C20 144.30(19) 2 . ? C17 Mo2 C20 58.1(3) . . ? C18 Mo2 C20 58.4(3) . . ? C21 Mo2 C20 34.9(3) . . ? S3 Mo2 C19 82.37(19) . . ? S4 Mo2 C19 128.1(2) . . ? S4 Mo2 C19 127.0(2) 2 . ? C17 Mo2 C19 57.7(3) . . ? C18 Mo2 C19 34.3(3) . . ? C21 Mo2 C19 58.0(3) . . ? C20 Mo2 C19 35.2(3) . . ? S3 Mo2 Cu2 54.93(5) . . ? S4 Mo2 Cu2 52.31(5) . . ? S4 Mo2 Cu2 102.80(5) 2 . ? C17 Mo2 Cu2 163.80(18) . . ? C18 Mo2 Cu2 153.2(2) . . ? C21 Mo2 Cu2 129.52(18) . . ? C20 Mo2 Cu2 111.72(18) . . ? C19 Mo2 Cu2 122.59(19) . . ? S3 Mo2 Cu2 56.08(5) . 2 ? S4 Mo2 Cu2 101.71(5) . 2 ? S4 Mo2 Cu2 51.76(5) 2 2 ? C17 Mo2 Cu2 129.68(18) . 2 ? C18 Mo2 Cu2 112.02(19) . 2 ? C21 Mo2 Cu2 163.72(19) . 2 ? C20 Mo2 Cu2 154.8(2) . 2 ? C19 Mo2 Cu2 123.1(2) . 2 ? Cu2 Mo2 Cu2 65.29(4) . 2 ? S3 Mo2 Mo2 99.35(5) . 2 ? S4 Mo2 Mo2 52.04(5) . 2 ? S4 Mo2 Mo2 52.03(5) 2 2 ? C17 Mo2 Mo2 120.46(18) . 2 ? C18 Mo2 Mo2 144.35(19) . 2 ? C21 Mo2 Mo2 120.62(19) . 2 ? C20 Mo2 Mo2 144.3(2) . 2 ? C19 Mo2 Mo2 178.19(19) . 2 ? Cu2 Mo2 Mo2 59.10(3) . 2 ? Cu2 Mo2 Mo2 57.84(3) 2 2 ? N2 Cu2 S4 109.60(18) . . ? N2 Cu2 S3 123.21(18) . . ? S4 Cu2 S3 105.68(7) . . ? N2 Cu2 S3 113.36(19) . 2 ? S4 Cu2 S3 103.92(7) . 2 ? S3 Cu2 S3 99.09(7) . 2 ? N2 Cu2 Mo2 146.60(19) . . ? S4 Cu2 Mo2 54.86(5) . . ? S3 Cu2 Mo2 52.02(5) . . ? S3 Cu2 Mo2 99.67(5) 2 . ? N2 Cu2 Mo2 136.43(17) . 2 ? S4 Cu2 Mo2 54.26(5) . 2 ? S3 Cu2 Mo2 100.30(5) . 2 ? S3 Cu2 Mo2 51.00(4) 2 2 ? Mo2 Cu2 Mo2 63.05(3) . 2 ? N2 Cu2 Cu2 151.53(18) . 2 ? S4 Cu2 Cu2 97.86(4) . 2 ? S3 Cu2 Cu2 52.25(5) . 2 ? S3 Cu2 Cu2 50.26(5) 2 2 ? Mo2 Cu2 Cu2 57.96(3) . 2 ? Mo2 Cu2 Cu2 56.75(3) 2 2 ? Mo2 S3 Cu2 73.05(5) . . ? Mo2 S3 Cu2 72.92(5) . 2 ? Cu2 S3 Cu2 77.48(7) . 2 ? Cu2 S4 Mo2 72.83(5) . . ? Cu2 S4 Mo2 73.98(5) . 2 ? Mo2 S4 Mo2 75.92(6) . 2 ? C27 N2 C31 117.7(6) . . ? C27 N2 Cu2 121.7(5) . . ? C31 N2 Cu2 119.7(5) . . ? C21 C17 C18 108.1(6) . . ? C21 C17 C22 125.9(7) . . ? C18 C17 C22 125.8(7) . . ? C21 C17 Mo2 72.7(4) . . ? C18 C17 Mo2 72.2(4) . . ? C22 C17 Mo2 125.3(5) . . ? C19 C18 C17 107.8(7) . . ? C19 C18 C23 127.2(8) . . ? C17 C18 C23 124.7(7) . . ? C19 C18 Mo2 74.6(4) . . ? C17 C18 Mo2 72.2(4) . . ? C23 C18 Mo2 124.7(5) . . ? C18 C19 C20 108.1(7) . . ? C18 C19 C24 126.2(8) . . ? C20 C19 C24 125.5(8) . . ? C18 C19 Mo2 71.1(4) . . ? C20 C19 Mo2 71.0(4) . . ? C24 C19 Mo2 127.1(6) . . ? C21 C20 C19 107.6(7) . . ? C21 C20 C25 126.3(8) . . ? C19 C20 C25 125.8(8) . . ? C21 C20 Mo2 72.3(4) . . ? C19 C20 Mo2 73.8(4) . . ? C25 C20 Mo2 124.5(6) . . ? C17 C21 C20 108.3(7) . . ? C17 C21 C26 126.4(7) . . ? C20 C21 C26 125.0(7) . . ? C17 C21 Mo2 72.5(4) . . ? C20 C21 Mo2 72.8(4) . . ? C26 C21 Mo2 124.9(5) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 C27 C28 122.5(7) . . ? N2 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C27 C28 C29 119.9(7) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 117.2(6) . . ? C30 C29 C32 122.6(7) . . ? C28 C29 C32 120.1(7) . . ? C31 C30 C29 119.1(7) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? N2 C31 C30 123.4(7) . . ? N2 C31 H31 118.3 . . ? C30 C31 H31 118.3 . . ? C32 C32 C29 125.1(9) 3 . ? C32 C32 H32 117.5 3 . ? C29 C32 H32 117.5 . . ? C33 N3 H3A 120.0 . . ? C33 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C38 C33 C34 123.2(19) . . ? C38 C33 N3 119.1(16) . . ? C34 C33 N3 117.5(16) . . ? C33 C34 C35 117.1(16) . . ? C33 C34 H34 121.4 . . ? C35 C34 H34 121.4 . . ? C34 C35 C36 121.7(17) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C37 C36 C35 115(2) . . ? C37 C36 H36 122.6 . . ? C35 C36 H36 122.6 . . ? C38 C37 C36 122(2) . . ? C38 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C37 C38 C33 121(2) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? C39 N4 H4A 120.0 . . ? C39 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? N4 C39 C44 121.6(14) . . ? N4 C39 C40 123.3(14) . . ? C44 C39 C40 115.1(16) . . ? C41 C40 C39 122.1(16) . . ? C41 C40 H40 118.9 . . ? C39 C40 H40 118.9 . . ? C40 C41 C42 122.6(18) . . ? C40 C41 H41 118.7 . . ? C42 C41 H41 118.7 . . ? C41 C42 C43 117.5(18) . . ? C41 C42 H42 121.2 . . ? C43 C42 H42 121.2 . . ? C44 C43 C42 120.5(15) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C39 122.1(15) . . ? C43 C44 H44 118.9 . . ? C39 C44 H44 118.9 . . ? O3 Cl1 O2A 92.5(9) . . ? O3 Cl1 O4A 141.0(9) . . ? O2A Cl1 O4A 123.0(10) . . ? O3 Cl1 O1 120.2(9) . . ? O2A Cl1 O1 65.3(8) . . ? O4A Cl1 O1 91.5(8) . . ? O3 Cl1 O4 117.9(9) . . ? O2A Cl1 O4 138.0(10) . . ? O4A Cl1 O4 23.8(7) . . ? O1 Cl1 O4 114.1(8) . . ? O3 Cl1 O3A 31.3(7) . . ? O2A Cl1 O3A 113.9(8) . . ? O4A Cl1 O3A 111.2(8) . . ? O1 Cl1 O3A 149.0(9) . . ? O4 Cl1 O3A 87.5(8) . . ? O3 Cl1 O2 102.9(8) . . ? O2A Cl1 O2 46.9(7) . . ? O4A Cl1 O2 92.6(9) . . ? O1 Cl1 O2 99.4(8) . . ? O4 Cl1 O2 95.7(9) . . ? O3A Cl1 O2 100.4(8) . . ? O3 Cl1 O1A 86.9(9) . . ? O2A Cl1 O1A 107.2(8) . . ? O4A Cl1 O1A 96.0(9) . . ? O1 Cl1 O1A 53.9(8) . . ? O4 Cl1 O1A 102.9(8) . . ? O3A Cl1 O1A 101.3(9) . . ? O2 Cl1 O1A 151.9(7) . . ? O8 Cl2 O6 117.2(11) . . ? O8 Cl2 O7 114.0(9) . . ? O6 Cl2 O7 117.1(10) . . ? O8 Cl2 O5 104.0(10) . . ? O6 Cl2 O5 100.7(9) . . ? O7 Cl2 O5 99.9(9) . . ? O8A Cl2A O7A 111.2(10) . . ? O8A Cl2A O5A 104.4(12) . . ? O7A Cl2A O5A 102.2(12) . . ? O8A Cl2A O6A 127.7(14) . . ? O7A Cl2A O6A 108.3(11) . . ? O5A Cl2A O6A 99.2(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.303 _refine_diff_density_min -1.773 _refine_diff_density_rms 0.117 #===END #============================================================================== data_62MeCN _database_code_depnum_ccdc_archive 'CCDC 679379' #============================================================================== # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H84 Cu4 Mo4 N4 S8, 4(PF6), 2(CH3CN)' _chemical_formula_sum 'C68 H90 Cu4 F24 Mo4 N6 P4 S8' _chemical_formula_weight 2465.74 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4 21 2' _symmetry_space_group_name_Hall 'P 4ab 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z' 'y+1/2, -x+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'y, x, -z' '-y, -x, -z' _cell_length_a 14.236(2) _cell_length_b 14.236(2) _cell_length_c 22.440(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4547.8(13) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 15990 _cell_measurement_theta_min 3.0043 _cell_measurement_theta_max 25.3491 _exptl_crystal_description flake _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 1.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5266 _exptl_absorpt_correction_T_max 0.9156 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45299 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.34 _reflns_number_total 4177 _reflns_number_gt 3865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+9.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.13(6) _refine_ls_number_reflns 4177 _refine_ls_number_parameters 299 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.1932 _refine_ls_wR_factor_gt 0.1894 _refine_ls_goodness_of_fit_ref 1.381 _refine_ls_restrained_S_all 1.386 _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 0.42832(6) 0.42925(6) 0.77804(3) 0.0289(2) Uani 1 1 d . . . Cu1 Cu 0.42935(10) 0.57256(10) 0.69543(4) 0.0382(3) Uani 1 1 d . . . S1 S 0.4086(2) 0.4067(2) 0.68011(10) 0.0382(5) Uani 1 1 d . . . S2 S 0.4114(2) 0.58957(19) 0.79499(9) 0.0353(4) Uani 1 1 d . . . C1 C 0.4102(8) 0.3152(10) 0.8542(6) 0.058(4) Uani 1 1 d . . . C2 C 0.3616(9) 0.3970(9) 0.8722(4) 0.058(4) Uani 1 1 d U . . C3 C 0.2871(7) 0.4095(9) 0.8306(5) 0.050(3) Uani 1 1 d . . . C4 C 0.2903(7) 0.3375(7) 0.7881(5) 0.037(2) Uani 1 1 d . . . C5 C 0.3697(8) 0.2784(8) 0.8019(6) 0.050(3) Uani 1 1 d U . . C6 C 0.4878(11) 0.2705(10) 0.8903(6) 0.079(4) Uani 1 1 d . . . H6A H 0.4604 0.2272 0.9195 0.118 Uiso 1 1 calc R . . H6B H 0.5233 0.3195 0.9112 0.118 Uiso 1 1 calc R . . H6C H 0.5300 0.2358 0.8637 0.118 Uiso 1 1 calc R . . C7 C 0.3755(12) 0.4561(12) 0.9254(5) 0.090(5) Uani 1 1 d . . . H7A H 0.4345 0.4386 0.9450 0.136 Uiso 1 1 calc R . . H7B H 0.3231 0.4468 0.9531 0.136 Uiso 1 1 calc R . . H7C H 0.3783 0.5223 0.9135 0.136 Uiso 1 1 calc R . . C8 C 0.2088(8) 0.4781(9) 0.8374(7) 0.073(4) Uani 1 1 d . . . H8A H 0.1588 0.4501 0.8616 0.110 Uiso 1 1 calc R . . H8B H 0.1839 0.4944 0.7980 0.110 Uiso 1 1 calc R . . H8C H 0.2322 0.5350 0.8570 0.110 Uiso 1 1 calc R . . C9 C 0.2189(8) 0.3177(9) 0.7412(7) 0.068(4) Uani 1 1 d . . . H9A H 0.1825 0.3747 0.7332 0.102 Uiso 1 1 calc R . . H9B H 0.1767 0.2678 0.7549 0.102 Uiso 1 1 calc R . . H9C H 0.2507 0.2975 0.7046 0.102 Uiso 1 1 calc R . . C10 C 0.3953(10) 0.1897(8) 0.7702(7) 0.074(4) Uani 1 1 d . . . H10A H 0.4638 0.1824 0.7701 0.111 Uiso 1 1 calc R . . H10B H 0.3724 0.1924 0.7291 0.111 Uiso 1 1 calc R . . H10C H 0.3667 0.1360 0.7907 0.111 Uiso 1 1 calc R . . C11 C 0.3662(8) 0.7278(9) 0.6221(6) 0.049(3) Uani 1 1 d . . . H11 H 0.4227 0.7568 0.6351 0.058 Uiso 1 1 calc R . . C12 C 0.2709(7) 0.6016(7) 0.6187(5) 0.040(3) Uani 1 1 d . . . H12 H 0.2561 0.5393 0.6306 0.048 Uiso 1 1 calc R . . C13 C 0.2080(8) 0.6471(8) 0.5803(5) 0.048(3) Uani 1 1 d . . . H13 H 0.1546 0.6151 0.5650 0.058 Uiso 1 1 calc R . . C14 C 0.3077(8) 0.7787(7) 0.5868(5) 0.046(3) Uani 1 1 d . . . H14 H 0.3234 0.8416 0.5769 0.055 Uiso 1 1 calc R . . C15 C 0.2251(7) 0.7394(7) 0.5652(4) 0.038(3) Uani 1 1 d . . . C16 C 0.1581(9) 0.7947(9) 0.5265(4) 0.066(5) Uani 1 1 d . . . H16A H 0.1273 0.8435 0.5512 0.079 Uiso 1 1 calc R . . H16B H 0.1085 0.7519 0.5116 0.079 Uiso 1 1 calc R . . P2 P 0.0000 0.5000 0.6741(4) 0.0588(17) Uani 1 4 d S . . F7 F -0.1101(5) 0.5051(6) 0.6750(6) 0.107(4) Uani 1 1 d . . . F6 F 0.0000 0.5000 0.7439(8) 0.091(5) Uani 1 4 d S . . F5 F 0.0000 0.5000 0.6069(12) 0.148(10) Uani 1 4 d S . . P1 P 0.2772(2) 0.7228(2) 1.0000 0.139(4) Uani 1 2 d SD . . F1 F 0.2769(12) 0.7193(13) 0.9292(4) 0.231(9) Uani 1 1 d D . . F2 F 0.2027(6) 0.7973(6) 1.0000 0.39(3) Uani 1 2 d SD . . F3 F 0.3386(18) 0.6394(12) 1.0059(11) 0.141(11) Uani 0.50 1 d PD . . F4 F 0.3590(12) 0.7934(11) 0.9969(10) 0.39(2) Uani 1 1 d D . . P3 P 0.0000 0.5000 0.4138(5) 0.092(3) Uani 1 4 d SD . . C17 C 0.5000 0.0000 0.9894(15) 0.18(2) Uani 1 4 d SD . . C18 C 0.5000 0.0000 0.9251(15) 0.105(12) Uani 1 4 d SD . . N1 N 0.3496(6) 0.6392(6) 0.6396(3) 0.0395(17) Uani 1 1 d . . . N2 N 0.5000 0.0000 0.8736(18) 0.110(11) Uani 1 4 d S . . F8 F -0.009(3) 0.4212(14) 0.3644(8) 0.149(12) Uani 0.50 1 d PD . . F9 F -0.0055(19) 0.4170(15) 0.4614(10) 0.143(12) Uani 0.50 1 d PD . . F10 F 0.1095(10) 0.4901(14) 0.4134(18) 0.174(18) Uani 0.50 1 d PD . . C20 C 0.5000 0.5000 0.5000 0.067(6) Uani 1 4 d SD . . C19 C 0.5725(10) 0.4275(10) 0.5000 0.129(11) Uani 0.50 2 d SPD . . N3 N 0.554(2) 0.446(2) 0.5000 0.129(11) Uani 0.50 2 d SP . . 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 0.0254(5) 0.0316(5) 0.0297(4) 0.0037(4) 0.0006(4) -0.0033(2) Cu1 0.0429(8) 0.0406(8) 0.0312(6) 0.0052(6) -0.0061(6) 0.0050(4) S1 0.0385(16) 0.0393(17) 0.0367(10) -0.0050(13) -0.0071(13) -0.0062(8) S2 0.0406(17) 0.0305(15) 0.0349(10) -0.0034(12) 0.0032(13) 0.0012(7) C1 0.043(7) 0.083(10) 0.046(7) 0.033(7) 0.007(6) -0.020(7) C2 0.091(10) 0.070(8) 0.015(5) 0.015(5) 0.013(5) -0.015(8) C3 0.033(6) 0.075(8) 0.041(6) 0.016(6) 0.023(5) 0.008(6) C4 0.028(5) 0.034(5) 0.048(6) -0.002(4) 0.005(4) -0.008(4) C5 0.046(7) 0.041(6) 0.062(7) 0.041(6) -0.008(6) 0.003(5) C6 0.076(9) 0.079(9) 0.081(9) 0.043(8) -0.010(8) -0.018(8) C7 0.106(12) 0.140(14) 0.026(6) 0.015(7) 0.020(7) -0.013(11) C8 0.048(7) 0.057(8) 0.114(12) 0.001(7) 0.034(8) -0.017(6) C9 0.033(6) 0.056(7) 0.116(11) 0.004(7) 0.000(7) -0.017(5) C10 0.075(9) 0.027(6) 0.120(12) 0.005(7) -0.004(8) -0.008(6) C11 0.026(5) 0.059(7) 0.061(7) -0.010(6) -0.002(5) -0.011(5) C12 0.034(5) 0.037(6) 0.049(6) 0.020(5) -0.017(5) -0.005(4) C13 0.041(6) 0.057(7) 0.046(6) -0.004(5) 0.004(5) -0.007(5) C14 0.052(7) 0.034(5) 0.051(6) 0.032(5) 0.007(6) 0.014(5) C15 0.036(5) 0.048(6) 0.029(4) 0.012(4) -0.004(4) 0.012(5) C16 0.082(9) 0.087(10) 0.029(5) -0.003(5) 0.002(5) 0.058(8) P2 0.0317(18) 0.0317(18) 0.113(6) 0.000 0.000 0.000 F7 0.034(4) 0.079(6) 0.209(11) -0.050(7) -0.009(6) -0.002(4) F6 0.085(7) 0.085(7) 0.101(12) 0.000 0.000 0.000 F5 0.166(16) 0.166(16) 0.112(18) 0.000 0.000 0.000 P1 0.142(5) 0.142(5) 0.132(6) 0.088(5) 0.088(5) 0.099(6) F1 0.208(16) 0.35(2) 0.131(10) 0.147(15) 0.040(12) 0.148(15) F2 0.48(5) 0.48(5) 0.21(3) 0.13(4) 0.13(4) 0.40(5) F3 0.28(3) 0.067(10) 0.076(12) -0.028(13) 0.018(18) 0.087(15) F4 0.75(6) 0.200(19) 0.23(2) -0.05(2) 0.17(4) -0.26(3) P3 0.050(3) 0.050(3) 0.177(10) 0.000 0.000 0.000 C17 0.24(4) 0.24(4) 0.07(3) 0.000 0.000 0.000 C18 0.099(18) 0.099(18) 0.12(3) 0.000 0.000 0.000 N1 0.028(5) 0.042(5) 0.049(4) 0.000(4) -0.004(4) -0.006(3) N2 0.076(12) 0.076(12) 0.18(4) 0.000 0.000 0.000 F8 0.25(3) 0.066(15) 0.130(18) -0.018(12) 0.01(3) -0.04(2) F9 0.15(2) 0.10(2) 0.18(2) 0.068(16) -0.01(2) -0.03(2) F10 0.062(14) 0.056(13) 0.40(6) 0.05(3) 0.03(3) -0.021(10) C20 0.076(10) 0.076(10) 0.048(11) 0.000 0.000 -0.037(13) C19 0.129(16) 0.129(16) 0.13(2) -0.010(19) -0.010(19) 0.070(19) N3 0.129(16) 0.129(16) 0.13(2) -0.010(19) -0.010(19) 0.070(19) _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 S1 2.238(2) . ? Mo1 S2 2.326(3) . ? Mo1 S2 2.329(3) 2_665 ? Mo1 C3 2.348(9) . ? Mo1 C2 2.362(9) . ? Mo1 C5 2.365(11) . ? Mo1 C4 2.371(10) . ? Mo1 C1 2.371(11) . ? Mo1 Cu1 2.7464(15) 2_665 ? Mo1 Cu1 2.7567(15) . ? Mo1 Mo1 2.8677(13) 2_665 ? Cu1 N1 1.938(7) . ? Cu1 S2 2.262(2) . ? Cu1 S1 2.351(3) 2_665 ? Cu1 S1 2.405(3) . ? Cu1 Mo1 2.7464(15) 2_665 ? Cu1 Cu1 2.883(2) 2_665 ? S1 Cu1 2.351(3) 2_665 ? S2 Mo1 2.329(3) 2_665 ? C1 C5 1.408(18) . ? C1 C2 1.414(19) . ? C1 C6 1.510(18) . ? C2 C3 1.425(16) . ? C2 C7 1.474(18) . ? C3 C4 1.400(16) . ? C3 C8 1.490(16) . ? C4 C5 1.443(15) . ? C4 C9 1.490(16) . ? C5 C10 1.495(18) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N1 1.341(15) . ? C11 C14 1.358(16) . ? C11 H11 0.9500 . ? C12 N1 1.328(14) . ? C12 C13 1.401(15) . ? C12 H12 0.9500 . ? C13 C15 1.379(14) . ? C13 H13 0.9500 . ? C14 C15 1.389(14) . ? C14 H14 0.9500 . ? C15 C16 1.512(13) . ? C16 C16 1.52(2) 8_666 ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? P2 F5 1.51(3) . ? P2 F6 1.57(2) . ? P2 F7 1.569(7) 2_565 ? P2 F7 1.569(7) 4_455 ? P2 F7 1.569(7) 3 ? P2 F7 1.569(7) . ? P1 F3 1.481(11) 8_667 ? P1 F3 1.481(11) . ? P1 F2 1.500(13) . ? P1 F4 1.541(12) . ? P1 F4 1.541(12) 8_667 ? P1 F1 1.590(10) 8_667 ? P1 F1 1.590(10) . ? F3 F3 0.51(6) 8_667 ? P3 F10 1.566(15) 4_455 ? P3 F10 1.566(15) . ? P3 F10 1.566(15) 3 ? P3 F10 1.566(15) 2_565 ? P3 F8 1.582(15) 3 ? P3 F8 1.582(15) 2_565 ? P3 F8 1.582(15) . ? P3 F8 1.582(15) 4_455 ? P3 F9 1.595(15) 3 ? P3 F9 1.595(15) 2_565 ? P3 F9 1.595(15) . ? P3 F9 1.595(15) 4_455 ? C17 C18 1.44(5) . ? C18 N2 1.16(4) . ? F8 F10 1.18(3) 4_455 ? F8 F8 1.60(3) 3 ? F8 F8 1.60(3) 4_455 ? F9 F10 1.14(3) 4_455 ? F9 F9 1.67(3) 3 ? F9 F9 1.67(3) 4_455 ? F10 F9 1.14(3) 3 ? F10 F8 1.18(3) 3 ? C20 N3 1.08(4) . ? C20 N3 1.08(4) 2_665 ? C20 C19 1.46(2) . ? C20 C19 1.46(2) 2_665 ? 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 S1 Mo1 S2 106.76(10) . . ? S1 Mo1 S2 105.47(10) . 2_665 ? S2 Mo1 S2 100.82(7) . 2_665 ? S1 Mo1 C3 111.6(3) . . ? S2 Mo1 C3 86.9(3) . . ? S2 Mo1 C3 138.0(3) 2_665 . ? S1 Mo1 C2 143.1(3) . . ? S2 Mo1 C2 90.2(3) . . ? S2 Mo1 C2 103.0(3) 2_665 . ? C3 Mo1 C2 35.2(4) . . ? S1 Mo1 C5 92.7(3) . . ? S2 Mo1 C5 144.8(3) . . ? S2 Mo1 C5 101.8(3) 2_665 . ? C3 Mo1 C5 58.4(4) . . ? C2 Mo1 C5 58.6(5) . . ? S1 Mo1 C4 84.9(3) . . ? S2 Mo1 C4 116.0(3) . . ? S2 Mo1 C4 137.2(3) 2_665 . ? C3 Mo1 C4 34.5(4) . . ? C2 Mo1 C4 58.3(4) . . ? C5 Mo1 C4 35.5(4) . . ? S1 Mo1 C1 126.5(4) . . ? S2 Mo1 C1 122.9(4) . . ? S2 Mo1 C1 84.8(3) 2_665 . ? C3 Mo1 C1 57.5(4) . . ? C2 Mo1 C1 34.8(5) . . ? C5 Mo1 C1 34.6(4) . . ? C4 Mo1 C1 57.6(4) . . ? S1 Mo1 Cu1 55.15(7) . 2_665 ? S2 Mo1 Cu1 101.31(8) . 2_665 ? S2 Mo1 Cu1 52.14(6) 2_665 2_665 ? C3 Mo1 Cu1 165.9(3) . 2_665 ? C2 Mo1 Cu1 154.0(3) . 2_665 ? C5 Mo1 Cu1 113.9(3) . 2_665 ? C4 Mo1 Cu1 132.1(3) . 2_665 ? C1 Mo1 Cu1 124.1(3) . 2_665 ? S1 Mo1 Cu1 56.41(7) . . ? S2 Mo1 Cu1 52.01(6) . . ? S2 Mo1 Cu1 100.94(8) 2_665 . ? C3 Mo1 Cu1 115.5(3) . . ? C2 Mo1 Cu1 138.4(3) . . ? C5 Mo1 Cu1 145.7(3) . . ? C4 Mo1 Cu1 118.5(3) . . ? C1 Mo1 Cu1 172.7(3) . . ? Cu1 Mo1 Cu1 63.20(4) 2_665 . ? S1 Mo1 Mo1 100.96(5) . 2_665 ? S2 Mo1 Mo1 52.03(8) . 2_665 ? S2 Mo1 Mo1 51.93(8) 2_665 2_665 ? C3 Mo1 Mo1 133.9(3) . 2_665 ? C2 Mo1 Mo1 115.0(3) . 2_665 ? C5 Mo1 Mo1 152.7(3) . 2_665 ? C4 Mo1 Mo1 167.7(3) . 2_665 ? C1 Mo1 Mo1 123.9(3) . 2_665 ? Cu1 Mo1 Mo1 58.77(4) 2_665 2_665 ? Cu1 Mo1 Mo1 58.42(4) . 2_665 ? N1 Cu1 S2 121.3(2) . . ? N1 Cu1 S1 114.7(3) . 2_665 ? S2 Cu1 S1 104.01(11) . 2_665 ? N1 Cu1 S1 108.5(3) . . ? S2 Cu1 S1 103.44(11) . . ? S1 Cu1 S1 102.90(8) 2_665 . ? N1 Cu1 Mo1 150.8(3) . 2_665 ? S2 Cu1 Mo1 54.40(8) . 2_665 ? S1 Cu1 Mo1 51.38(6) 2_665 2_665 ? S1 Cu1 Mo1 100.25(7) . 2_665 ? N1 Cu1 Mo1 142.5(3) . . ? S2 Cu1 Mo1 54.15(7) . . ? S1 Cu1 Mo1 101.34(8) 2_665 . ? S1 Cu1 Mo1 50.85(6) . . ? Mo1 Cu1 Mo1 62.81(3) 2_665 . ? N1 Cu1 Cu1 139.4(2) . 2_665 ? S2 Cu1 Cu1 98.96(6) . 2_665 ? S1 Cu1 Cu1 53.53(8) 2_665 2_665 ? S1 Cu1 Cu1 51.84(8) . 2_665 ? Mo1 Cu1 Cu1 58.58(4) 2_665 2_665 ? Mo1 Cu1 Cu1 58.23(4) . 2_665 ? Mo1 S1 Cu1 73.46(7) . 2_665 ? Mo1 S1 Cu1 72.74(7) . . ? Cu1 S1 Cu1 74.63(7) 2_665 . ? Cu1 S2 Mo1 73.84(8) . . ? Cu1 S2 Mo1 73.46(8) . 2_665 ? Mo1 S2 Mo1 76.04(6) . 2_665 ? C5 C1 C2 110.1(11) . . ? C5 C1 C6 126.2(14) . . ? C2 C1 C6 123.4(12) . . ? C5 C1 Mo1 72.5(6) . . ? C2 C1 Mo1 72.3(7) . . ? C6 C1 Mo1 126.6(8) . . ? C1 C2 C3 106.3(11) . . ? C1 C2 C7 129.5(12) . . ? C3 C2 C7 124.0(13) . . ? C1 C2 Mo1 73.0(6) . . ? C3 C2 Mo1 71.9(5) . . ? C7 C2 Mo1 124.0(8) . . ? C4 C3 C2 109.3(10) . . ? C4 C3 C8 125.0(11) . . ? C2 C3 C8 124.9(12) . . ? C4 C3 Mo1 73.6(6) . . ? C2 C3 Mo1 72.9(6) . . ? C8 C3 Mo1 127.8(8) . . ? C3 C4 C5 107.9(10) . . ? C3 C4 C9 126.7(10) . . ? C5 C4 C9 125.1(10) . . ? C3 C4 Mo1 71.8(6) . . ? C5 C4 Mo1 72.1(6) . . ? C9 C4 Mo1 127.0(8) . . ? C1 C5 C4 106.4(12) . . ? C1 C5 C10 127.6(11) . . ? C4 C5 C10 125.6(11) . . ? C1 C5 Mo1 72.9(7) . . ? C4 C5 Mo1 72.5(6) . . ? C10 C5 Mo1 125.0(8) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C14 124.3(11) . . ? N1 C11 H11 117.8 . . ? C14 C11 H11 117.8 . . ? N1 C12 C13 124.8(10) . . ? N1 C12 H12 117.6 . . ? C13 C12 H12 117.6 . . ? C15 C13 C12 118.5(10) . . ? C15 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C11 C14 C15 120.5(10) . . ? C11 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C13 C15 C14 116.6(9) . . ? C13 C15 C16 121.7(10) . . ? C14 C15 C16 121.7(9) . . ? C15 C16 C16 113.6(9) . 8_666 ? C15 C16 H16A 108.8 . . ? C16 C16 H16A 108.8 8_666 . ? C15 C16 H16B 108.8 . . ? C16 C16 H16B 108.8 8_666 . ? H16A C16 H16B 107.7 . . ? F5 P2 F6 180.000(7) . . ? F5 P2 F7 90.7(6) . 2_565 ? F6 P2 F7 89.3(6) . 2_565 ? F5 P2 F7 90.7(6) . 4_455 ? F6 P2 F7 89.3(6) . 4_455 ? F7 P2 F7 89.991(18) 2_565 4_455 ? F5 P2 F7 90.7(6) . 3 ? F6 P2 F7 89.3(6) . 3 ? F7 P2 F7 89.991(16) 2_565 3 ? F7 P2 F7 178.6(11) 4_455 3 ? F5 P2 F7 90.7(6) . . ? F6 P2 F7 89.3(6) . . ? F7 P2 F7 178.6(11) 2_565 . ? F7 P2 F7 89.991(17) 4_455 . ? F7 P2 F7 89.991(19) 3 . ? F3 P1 F3 20(2) 8_667 . ? F3 P1 F2 170.0(11) 8_667 . ? F3 P1 F2 170.0(11) . . ? F3 P1 F4 77.0(16) 8_667 . ? F3 P1 F4 94.6(11) . . ? F2 P1 F4 94.2(8) . . ? F3 P1 F4 94.6(11) 8_667 8_667 ? F3 P1 F4 77.0(16) . 8_667 ? F2 P1 F4 94.2(8) . 8_667 ? F4 P1 F4 171.5(15) . 8_667 ? F3 P1 F1 93.7(10) 8_667 8_667 ? F3 P1 F1 84.0(11) . 8_667 ? F2 P1 F1 91.2(4) . 8_667 ? F4 P1 F1 91.1(8) . 8_667 ? F4 P1 F1 88.7(8) 8_667 8_667 ? F3 P1 F1 84.0(11) 8_667 . ? F3 P1 F1 93.7(10) . . ? F2 P1 F1 91.2(4) . . ? F4 P1 F1 88.7(8) . . ? F4 P1 F1 91.1(8) 8_667 . ? F1 P1 F1 177.6(8) 8_667 . ? F3 F3 P1 80.0(11) 8_667 . ? F10 P3 F10 90.00(2) 4_455 . ? F10 P3 F10 179(3) 4_455 3 ? F10 P3 F10 90.00(3) . 3 ? F10 P3 F10 90.00(3) 4_455 2_565 ? F10 P3 F10 179(3) . 2_565 ? F10 P3 F10 90.00(2) 3 2_565 ? F10 P3 F8 89(2) 4_455 3 ? F10 P3 F8 44.1(13) . 3 ? F10 P3 F8 90.7(12) 3 3 ? F10 P3 F8 135(2) 2_565 3 ? F10 P3 F8 135(2) 4_455 2_565 ? F10 P3 F8 89(2) . 2_565 ? F10 P3 F8 44.1(13) 3 2_565 ? F10 P3 F8 90.7(12) 2_565 2_565 ? F8 P3 F8 60.6(10) 3 2_565 ? F10 P3 F8 44.1(13) 4_455 . ? F10 P3 F8 90.7(12) . . ? F10 P3 F8 135(2) 3 . ? F10 P3 F8 89(2) 2_565 . ? F8 P3 F8 60.6(10) 3 . ? F8 P3 F8 91.1(17) 2_565 . ? F10 P3 F8 90.7(12) 4_455 4_455 ? F10 P3 F8 135(2) . 4_455 ? F10 P3 F8 89(2) 3 4_455 ? F10 P3 F8 44.1(13) 2_565 4_455 ? F8 P3 F8 91.1(17) 3 4_455 ? F8 P3 F8 60.6(10) 2_565 4_455 ? F8 P3 F8 60.6(10) . 4_455 ? F10 P3 F9 91(2) 4_455 3 ? F10 P3 F9 42.4(14) . 3 ? F10 P3 F9 89.2(11) 3 3 ? F10 P3 F9 138(2) 2_565 3 ? F8 P3 F9 86.5(9) 3 3 ? F8 P3 F9 116.4(17) 2_565 3 ? F8 P3 F9 119.6(16) . 3 ? F8 P3 F9 177(2) 4_455 3 ? F10 P3 F9 138(2) 4_455 2_565 ? F10 P3 F9 91(2) . 2_565 ? F10 P3 F9 42.4(14) 3 2_565 ? F10 P3 F9 89.2(11) 2_565 2_565 ? F8 P3 F9 119.6(17) 3 2_565 ? F8 P3 F9 86.5(9) 2_565 2_565 ? F8 P3 F9 177(2) . 2_565 ? F8 P3 F9 116.4(17) 4_455 2_565 ? F9 P3 F9 63.3(11) 3 2_565 ? F10 P3 F9 42.4(14) 4_455 . ? F10 P3 F9 89.2(11) . . ? F10 P3 F9 138(2) 3 . ? F10 P3 F9 91(2) 2_565 . ? F8 P3 F9 116.4(17) 3 . ? F8 P3 F9 177(2) 2_565 . ? F8 P3 F9 86.5(9) . . ? F8 P3 F9 119.6(17) 4_455 . ? F9 P3 F9 63.3(11) 3 . ? F9 P3 F9 96(2) 2_565 . ? F10 P3 F9 89.2(11) 4_455 4_455 ? F10 P3 F9 138(2) . 4_455 ? F10 P3 F9 91(2) 3 4_455 ? F10 P3 F9 42.4(14) 2_565 4_455 ? F8 P3 F9 177(2) 3 4_455 ? F8 P3 F9 119.6(16) 2_565 4_455 ? F8 P3 F9 116.4(17) . 4_455 ? F8 P3 F9 86.5(9) 4_455 4_455 ? F9 P3 F9 96(2) 3 4_455 ? F9 P3 F9 63.3(11) 2_565 4_455 ? F9 P3 F9 63.3(11) . 4_455 ? N2 C18 C17 180.000(17) . . ? C12 N1 C11 115.1(9) . . ? C12 N1 Cu1 121.7(7) . . ? C11 N1 Cu1 123.1(8) . . ? F10 F8 P3 67.2(11) 4_455 . ? F10 F8 F8 103.8(18) 4_455 3 ? P3 F8 F8 59.7(5) . 3 ? F10 F8 F8 106(2) 4_455 4_455 ? P3 F8 F8 59.7(5) . 4_455 ? F8 F8 F8 90.000(5) 3 4_455 ? F10 F9 P3 67.4(12) 4_455 . ? F10 F9 F9 105.0(16) 4_455 3 ? P3 F9 F9 58.3(5) . 3 ? F10 F9 F9 102(2) 4_455 4_455 ? P3 F9 F9 58.3(5) . 4_455 ? F9 F9 F9 90.000(6) 3 4_455 ? F9 F10 F8 139(2) 3 3 ? F9 F10 P3 70.2(14) 3 . ? F8 F10 P3 68.6(13) 3 . ? N3 C20 N3 180.000(11) . 2_665 ? N3 C20 C19 0.000(5) . . ? N3 C20 C19 180.000(5) 2_665 . ? N3 C20 C19 180.000(5) . 2_665 ? N3 C20 C19 0.000(5) 2_665 2_665 ? C19 C20 C19 180.000(3) . 2_665 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.644 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.120 #===END #============================================================================== data_7 _database_code_depnum_ccdc_archive 'CCDC 679380' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H108 Cu4 Mo4 P4 S8, 4(Cl O4)' _chemical_formula_sum 'C92 H108 Cl4 Cu4 Mo4 O16 P4 S8' _chemical_formula_weight 2629.86 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.234(4) _cell_length_b 17.989(4) _cell_length_c 30.820(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.11(3) _cell_angle_gamma 90.00 _cell_volume 10498(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 16895 _cell_measurement_theta_min 3.0357 _cell_measurement_theta_max 25.3491 _exptl_crystal_description prism _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5312 _exptl_absorpt_coefficient_mu 1.637 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4554 _exptl_absorpt_correction_T_max 0.8404 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 49808 _diffrn_reflns_av_R_equivalents 0.0869 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 9570 _reflns_number_gt 7933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+9.8000P] 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 9570 _refine_ls_number_parameters 581 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1145 _refine_ls_R_factor_gt 0.0960 _refine_ls_wR_factor_ref 0.3116 _refine_ls_wR_factor_gt 0.2952 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.59584(4) 0.69620(5) 0.10793(3) 0.0287(3) Uani 1 1 d . . . Mo2 Mo 0.54893(4) 0.84741(5) 0.10335(3) 0.0272(3) Uani 1 1 d . . . Cu1 Cu 0.62261(6) 0.78771(7) 0.18103(4) 0.0317(3) Uani 1 1 d . . . Cu2 Cu 0.47474(6) 0.73747(7) 0.13913(4) 0.0329(3) Uani 1 1 d . . . S1 S 0.57441(14) 0.66636(15) 0.17507(8) 0.0338(6) Uani 1 1 d . . . S2 S 0.51335(13) 0.85433(14) 0.16862(8) 0.0312(6) Uani 1 1 d . . . S3 S 0.66466(13) 0.80378(14) 0.11789(8) 0.0314(6) Uani 1 1 d . . . S4 S 0.49105(13) 0.74389(14) 0.06842(8) 0.0322(6) Uani 1 1 d . . . P1 P 0.68336(14) 0.83194(14) 0.24352(8) 0.0285(6) Uani 1 1 d . . . C1 C 0.6920(6) 0.6208(6) 0.1008(4) 0.043(3) Uani 1 1 d . . . C2 C 0.6417(8) 0.5726(7) 0.1103(4) 0.053(3) Uani 1 1 d . . . C3 C 0.5812(7) 0.5788(6) 0.0748(5) 0.052(3) Uani 1 1 d . . . C4 C 0.5991(7) 0.6266(7) 0.0434(4) 0.050(3) Uani 1 1 d . . . C5 C 0.6690(7) 0.6550(6) 0.0595(4) 0.043(3) Uani 1 1 d . . . C6 C 0.7666(8) 0.6305(11) 0.1280(5) 0.078(5) Uani 1 1 d . . . H6A H 0.7829 0.6815 0.1247 0.118 Uiso 1 1 calc R . . H6B H 0.7990 0.5955 0.1175 0.118 Uiso 1 1 calc R . . H6C H 0.7655 0.6208 0.1591 0.118 Uiso 1 1 calc R . . C7 C 0.6518(12) 0.5187(8) 0.1466(6) 0.092(6) Uani 1 1 d . . . H7A H 0.6092 0.4883 0.1451 0.138 Uiso 1 1 calc R . . H7B H 0.6610 0.5453 0.1748 0.138 Uiso 1 1 calc R . . H7C H 0.6921 0.4865 0.1443 0.138 Uiso 1 1 calc R . . C8 C 0.5154(11) 0.5339(12) 0.0714(8) 0.109(8) Uani 1 1 d . . . H8A H 0.4743 0.5667 0.0647 0.164 Uiso 1 1 calc R . . H8B H 0.5149 0.5083 0.0994 0.164 Uiso 1 1 calc R . . H8C H 0.5139 0.4971 0.0477 0.164 Uiso 1 1 calc R . . C9 C 0.5535(8) 0.6428(10) -0.0006(4) 0.076(5) Uani 1 1 d . . . H9A H 0.5771 0.6795 -0.0166 0.114 Uiso 1 1 calc R . . H9B H 0.5079 0.6625 0.0039 0.114 Uiso 1 1 calc R . . H9C H 0.5460 0.5968 -0.0179 0.114 Uiso 1 1 calc R . . C10 C 0.7101(9) 0.7016(9) 0.0351(5) 0.068(4) Uani 1 1 d . . . H10A H 0.6782 0.7317 0.0138 0.102 Uiso 1 1 calc R . . H10B H 0.7392 0.6702 0.0194 0.102 Uiso 1 1 calc R . . H10C H 0.7407 0.7343 0.0555 0.102 Uiso 1 1 calc R . . C11 C 0.5959(6) 0.9573(6) 0.0813(4) 0.041(3) Uani 1 1 d . . . C12 C 0.5670(7) 0.9195(6) 0.0438(4) 0.043(3) Uani 1 1 d . . . C13 C 0.4946(7) 0.9154(6) 0.0422(4) 0.050(3) Uani 1 1 d . . . C14 C 0.4782(6) 0.9542(7) 0.0803(4) 0.047(3) Uani 1 1 d . . . C15 C 0.5435(6) 0.9807(6) 0.1034(3) 0.039(2) Uani 1 1 d . . . C16 C 0.6745(7) 0.9821(7) 0.0939(5) 0.056(3) Uani 1 1 d . . . H16A H 0.6866 0.9888 0.1259 0.083 Uiso 1 1 calc R . . H16B H 0.6813 1.0292 0.0792 0.083 Uiso 1 1 calc R . . H16C H 0.7052 0.9440 0.0846 0.083 Uiso 1 1 calc R . . C17 C 0.6073(9) 0.8918(9) 0.0099(4) 0.070(4) Uani 1 1 d . . . H17A H 0.5743 0.8794 -0.0171 0.105 Uiso 1 1 calc R . . H17B H 0.6341 0.8473 0.0210 0.105 Uiso 1 1 calc R . . H17C H 0.6399 0.9305 0.0035 0.105 Uiso 1 1 calc R . . C18 C 0.4405(9) 0.8871(9) 0.0044(5) 0.087(6) Uani 1 1 d . . . H18A H 0.3978 0.8721 0.0153 0.130 Uiso 1 1 calc R . . H18B H 0.4598 0.8442 -0.0092 0.130 Uiso 1 1 calc R . . H18C H 0.4288 0.9265 -0.0176 0.130 Uiso 1 1 calc R . . C19 C 0.4049(8) 0.9677(10) 0.0909(6) 0.076(5) Uani 1 1 d . . . H19A H 0.3696 0.9426 0.0690 0.114 Uiso 1 1 calc R . . H19B H 0.3952 1.0212 0.0903 0.114 Uiso 1 1 calc R . . H19C H 0.4027 0.9480 0.1203 0.114 Uiso 1 1 calc R . . C20 C 0.5486(9) 1.0280(7) 0.1441(4) 0.062(4) Uani 1 1 d . . . H20A H 0.5983 1.0347 0.1574 0.093 Uiso 1 1 calc R . . H20B H 0.5237 1.0035 0.1653 0.093 Uiso 1 1 calc R . . H20C H 0.5270 1.0766 0.1361 0.093 Uiso 1 1 calc R . . C21 C 0.6474(5) 0.8020(5) 0.2917(4) 0.033(2) Uani 1 1 d . . . H21A H 0.6775 0.8211 0.3188 0.040 Uiso 1 1 calc R . . H21B H 0.5994 0.8230 0.2902 0.040 Uiso 1 1 calc R . . C23 C 0.7749(6) 0.8092(6) 0.2565(4) 0.036(2) Uani 1 1 d . . . C24 C 0.8143(7) 0.8175(11) 0.2987(5) 0.070(4) Uani 1 1 d . . . H24 H 0.7909 0.8323 0.3220 0.084 Uiso 1 1 calc R . . C25 C 0.8835(9) 0.8054(13) 0.3073(6) 0.095(6) Uani 1 1 d . . . H25 H 0.9099 0.8160 0.3357 0.114 Uiso 1 1 calc R . . C26 C 0.9183(8) 0.7757(11) 0.2728(6) 0.084(6) Uani 1 1 d . . . H26 H 0.9668 0.7622 0.2790 0.101 Uiso 1 1 calc R . . C27 C 0.8813(7) 0.7677(9) 0.2327(6) 0.066(4) Uani 1 1 d . . . H27 H 0.9044 0.7504 0.2098 0.080 Uiso 1 1 calc R . . C28 C 0.8101(6) 0.7839(6) 0.2231(4) 0.039(2) Uani 1 1 d . . . H28 H 0.7849 0.7778 0.1939 0.046 Uiso 1 1 calc R . . C29 C 0.6811(6) 0.9330(6) 0.2472(4) 0.041(3) Uani 1 1 d . . . C30 C 0.6311(8) 0.9704(7) 0.2628(4) 0.052(3) Uani 1 1 d . . . H30 H 0.5967 0.9443 0.2755 0.062 Uiso 1 1 calc R . . C31 C 0.6289(10) 1.0497(9) 0.2606(5) 0.072(4) Uani 1 1 d . . . H31 H 0.5912 1.0765 0.2693 0.087 Uiso 1 1 calc R . . C32 C 0.6825(13) 1.0863(8) 0.2455(5) 0.091(7) Uani 1 1 d . . . H32 H 0.6839 1.1391 0.2463 0.109 Uiso 1 1 calc R . . C33 C 0.7348(9) 1.0476(8) 0.2291(5) 0.068(4) Uani 1 1 d . . . H33 H 0.7708 1.0733 0.2177 0.082 Uiso 1 1 calc R . . C34 C 0.7333(8) 0.9720(8) 0.2297(5) 0.058(3) Uani 1 1 d . . . H34 H 0.7682 0.9450 0.2180 0.069 Uiso 1 1 calc R . . Cl1 Cl 0.28998(19) 0.5255(2) -0.00657(12) 0.0618(9) Uani 1 1 d . . . O1 O 0.2943(10) 0.4547(8) 0.0160(5) 0.129(6) Uani 1 1 d . . . O2 O 0.3562(8) 0.5547(12) -0.0025(7) 0.166(8) Uani 1 1 d . . . O3 O 0.2646(10) 0.5175(11) -0.0518(5) 0.156(8) Uani 1 1 d . . . O4 O 0.2448(8) 0.5733(7) 0.0112(4) 0.098(4) Uani 1 1 d . . . Cl2 Cl 0.9432(2) 0.7253(3) 0.10637(15) 0.1086(15) Uani 1 1 d D . . O5 O 0.9763(6) 0.7936(6) 0.1166(4) 0.1086(15) Uani 1 1 d D . . O6 O 0.8778(5) 0.7373(7) 0.0825(3) 0.1086(15) Uani 1 1 d D . . O7 O 0.9412(6) 0.6889(6) 0.1447(3) 0.1086(15) Uani 1 1 d D . . O8 O 0.9840(5) 0.6864(7) 0.0817(3) 0.1086(15) Uani 1 1 d D . . P2 P 0.62390(14) 0.68691(14) 0.34687(9) 0.0300(6) Uani 1 1 d . . . C22 C 0.6437(6) 0.7163(5) 0.2939(3) 0.030(2) Uani 1 1 d . . . H22A H 0.6894 0.6948 0.2897 0.036 Uiso 1 1 calc R . . H22B H 0.6066 0.6978 0.2699 0.036 Uiso 1 1 calc R . . C35 C 0.7045(6) 0.7092(6) 0.3841(3) 0.034(2) Uani 1 1 d . . . C36 C 0.7022(8) 0.7574(9) 0.4188(5) 0.068(4) Uani 1 1 d . . . H36 H 0.6585 0.7752 0.4250 0.081 Uiso 1 1 calc R . . C37 C 0.7681(10) 0.7794(11) 0.4451(7) 0.099(7) Uani 1 1 d . . . H37 H 0.7670 0.8130 0.4687 0.118 Uiso 1 1 calc R . . C38 C 0.8280(10) 0.7565(11) 0.4385(7) 0.091(6) Uani 1 1 d . . . H38 H 0.8701 0.7741 0.4564 0.109 Uiso 1 1 calc R . . C39 C 0.8316(7) 0.7044(9) 0.4041(5) 0.067(4) Uani 1 1 d . . . H39 H 0.8757 0.6850 0.3997 0.080 Uiso 1 1 calc R . . C40 C 0.7693(7) 0.6824(7) 0.3772(5) 0.051(3) Uani 1 1 d . . . H40 H 0.7712 0.6486 0.3538 0.061 Uiso 1 1 calc R . . C41 C 0.6197(5) 0.5872(6) 0.3431(4) 0.036(2) Uani 1 1 d . . . C42 C 0.6422(7) 0.5426(6) 0.3796(4) 0.046(3) Uani 1 1 d . . . H42 H 0.6646 0.5643 0.4066 0.055 Uiso 1 1 calc R . . C43 C 0.6320(8) 0.4663(8) 0.3765(6) 0.069(4) Uani 1 1 d . . . H43 H 0.6463 0.4361 0.4018 0.083 Uiso 1 1 calc R . . C44 C 0.6016(8) 0.4338(8) 0.3377(6) 0.064(4) Uani 1 1 d . . . H44 H 0.5952 0.3814 0.3359 0.077 Uiso 1 1 calc R . . C45 C 0.5814(9) 0.4755(9) 0.3032(6) 0.075(5) Uani 1 1 d . . . H45 H 0.5621 0.4524 0.2760 0.090 Uiso 1 1 calc R . . C46 C 0.5870(8) 0.5516(7) 0.3046(5) 0.062(4) Uani 1 1 d . . . H46 H 0.5685 0.5802 0.2793 0.074 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 0.0271(5) 0.0284(5) 0.0314(5) -0.0024(3) 0.0075(4) -0.0014(3) Mo2 0.0269(5) 0.0264(5) 0.0285(5) 0.0020(3) 0.0059(4) -0.0025(3) Cu1 0.0319(7) 0.0333(7) 0.0294(7) 0.0000(5) 0.0036(5) -0.0057(5) Cu2 0.0297(7) 0.0346(7) 0.0364(7) -0.0026(5) 0.0114(5) -0.0079(5) S1 0.0370(14) 0.0317(13) 0.0335(13) 0.0014(10) 0.0083(11) -0.0055(11) S2 0.0294(13) 0.0320(13) 0.0339(13) -0.0032(10) 0.0104(10) -0.0040(10) S3 0.0255(12) 0.0347(14) 0.0343(13) 0.0017(10) 0.0061(10) -0.0043(10) S4 0.0301(13) 0.0333(13) 0.0330(13) -0.0030(10) 0.0047(10) -0.0021(10) P1 0.0275(13) 0.0290(13) 0.0288(12) -0.0026(10) 0.0043(10) -0.0038(10) C1 0.035(6) 0.035(6) 0.058(7) -0.012(5) 0.007(5) 0.012(5) C2 0.071(9) 0.040(7) 0.051(7) -0.012(6) 0.017(7) 0.016(6) C3 0.055(8) 0.031(6) 0.075(9) -0.019(6) 0.027(7) -0.004(5) C4 0.061(8) 0.044(7) 0.046(6) -0.019(5) 0.014(6) 0.007(6) C5 0.049(7) 0.038(6) 0.045(6) -0.010(5) 0.021(6) 0.000(5) C6 0.056(9) 0.112(14) 0.065(9) -0.021(9) 0.003(7) 0.034(9) C7 0.143(18) 0.032(7) 0.112(14) 0.026(8) 0.055(13) 0.032(9) C8 0.093(13) 0.095(14) 0.151(18) -0.070(13) 0.054(13) -0.061(12) C9 0.069(10) 0.113(14) 0.046(7) -0.040(8) 0.011(7) 0.019(9) C10 0.077(10) 0.076(10) 0.064(9) -0.001(8) 0.048(8) 0.005(8) C11 0.036(6) 0.038(6) 0.046(6) 0.018(5) 0.001(5) -0.009(5) C12 0.051(7) 0.037(6) 0.039(6) 0.008(5) 0.002(5) -0.002(5) C13 0.063(8) 0.035(6) 0.042(6) 0.020(5) -0.015(6) -0.013(6) C14 0.035(6) 0.043(7) 0.064(8) 0.019(6) 0.011(5) 0.013(5) C15 0.052(7) 0.029(5) 0.033(5) 0.001(4) 0.003(5) 0.001(5) C16 0.051(7) 0.035(6) 0.080(9) 0.002(6) 0.011(7) -0.017(6) C17 0.097(12) 0.073(10) 0.049(7) 0.016(7) 0.037(8) 0.014(9) C18 0.089(12) 0.074(10) 0.075(10) 0.033(8) -0.049(9) -0.027(9) C19 0.043(8) 0.080(11) 0.105(12) 0.030(10) 0.010(8) 0.004(7) C20 0.102(12) 0.035(6) 0.048(7) 0.000(5) 0.010(7) -0.014(7) C21 0.026(5) 0.025(5) 0.050(6) -0.001(4) 0.009(5) 0.004(4) C23 0.039(6) 0.029(5) 0.041(6) 0.005(4) 0.007(5) -0.005(4) C24 0.042(8) 0.117(14) 0.050(8) -0.011(8) 0.008(6) -0.014(8) C25 0.049(9) 0.16(2) 0.066(10) -0.004(11) -0.002(8) -0.005(11) C26 0.029(7) 0.122(15) 0.104(14) 0.045(12) 0.017(8) 0.013(8) C27 0.033(7) 0.085(11) 0.083(11) 0.012(8) 0.017(7) 0.004(7) C28 0.028(5) 0.042(6) 0.048(6) 0.002(5) 0.012(5) 0.005(5) C29 0.043(6) 0.034(6) 0.042(6) -0.001(5) -0.004(5) -0.006(5) C30 0.068(8) 0.044(7) 0.046(7) -0.013(5) 0.017(6) -0.001(6) C31 0.090(12) 0.057(9) 0.070(10) -0.014(8) 0.014(9) 0.025(9) C32 0.17(2) 0.035(8) 0.061(9) -0.007(7) -0.008(11) -0.024(11) C33 0.081(11) 0.035(7) 0.091(11) 0.003(7) 0.022(9) -0.017(7) C34 0.058(8) 0.045(7) 0.072(9) 0.013(6) 0.015(7) -0.010(6) Cl1 0.056(2) 0.064(2) 0.065(2) -0.0053(17) 0.0103(16) 0.0145(16) O1 0.195(18) 0.079(9) 0.132(12) 0.021(8) 0.081(12) 0.038(10) O2 0.073(10) 0.173(18) 0.24(2) 0.029(16) 0.003(12) -0.042(11) O3 0.157(15) 0.201(18) 0.090(10) -0.079(11) -0.033(10) 0.078(14) O4 0.128(11) 0.074(7) 0.111(9) 0.004(7) 0.069(9) 0.047(7) Cl2 0.076(3) 0.162(5) 0.079(3) -0.028(3) -0.009(2) 0.020(3) O5 0.076(3) 0.162(5) 0.079(3) -0.028(3) -0.009(2) 0.020(3) O6 0.076(3) 0.162(5) 0.079(3) -0.028(3) -0.009(2) 0.020(3) O7 0.076(3) 0.162(5) 0.079(3) -0.028(3) -0.009(2) 0.020(3) O8 0.076(3) 0.162(5) 0.079(3) -0.028(3) -0.009(2) 0.020(3) P2 0.0272(13) 0.0298(13) 0.0338(13) 0.0022(10) 0.0078(11) 0.0050(10) C22 0.037(5) 0.023(5) 0.031(5) -0.001(4) 0.004(4) 0.006(4) C35 0.038(6) 0.028(5) 0.035(5) 0.002(4) 0.002(5) 0.001(4) C36 0.058(9) 0.071(10) 0.071(10) -0.027(8) 0.003(7) 0.006(7) C37 0.067(12) 0.104(14) 0.106(15) -0.051(12) -0.037(10) -0.006(11) C38 0.060(11) 0.083(12) 0.110(15) 0.009(11) -0.037(10) -0.017(9) C39 0.029(7) 0.082(11) 0.084(11) 0.004(9) -0.007(7) 0.010(7) C40 0.038(7) 0.044(7) 0.066(8) 0.004(6) -0.002(6) 0.015(5) C41 0.028(5) 0.034(6) 0.049(6) 0.005(5) 0.017(5) 0.006(4) C42 0.053(7) 0.034(6) 0.053(7) 0.013(5) 0.018(6) 0.005(5) C43 0.073(10) 0.039(7) 0.097(11) 0.026(8) 0.016(9) 0.030(7) C44 0.072(10) 0.039(7) 0.085(11) -0.005(7) 0.025(8) 0.002(7) C45 0.091(12) 0.054(9) 0.074(10) -0.023(8) 0.001(9) -0.026(8) C46 0.071(9) 0.043(7) 0.068(9) 0.008(6) 0.001(7) -0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 S1 2.245(3) . ? Mo1 S4 2.328(3) . ? Mo1 S3 2.334(3) . ? Mo1 C1 2.335(10) . ? Mo1 C3 2.341(11) . ? Mo1 C5 2.344(11) . ? Mo1 C4 2.360(11) . ? Mo1 C2 2.389(12) . ? Mo1 Cu1 2.7646(15) . ? Mo1 Cu2 2.7726(16) . ? Mo1 Mo2 2.8614(13) . ? Mo2 S2 2.239(3) . ? Mo2 C12 2.322(11) . ? Mo2 C11 2.324(10) . ? Mo2 S3 2.328(3) . ? Mo2 S4 2.334(3) . ? Mo2 C13 2.335(10) . ? Mo2 C14 2.389(11) . ? Mo2 C15 2.400(11) . ? Mo2 Cu1 2.7752(16) . ? Mo2 Cu2 2.7779(15) . ? Cu1 P1 2.218(3) . ? Cu1 S3 2.253(3) . ? Cu1 S1 2.366(3) . ? Cu1 S2 2.391(3) . ? Cu1 Cu2 3.0469(19) . ? Cu2 P2 2.214(3) 2_655 ? Cu2 S4 2.259(3) . ? Cu2 S2 2.358(3) . ? Cu2 S1 2.407(3) . ? P1 C23 1.784(12) . ? P1 C29 1.823(11) . ? P1 C21 1.826(11) . ? C1 C2 1.368(19) . ? C1 C5 1.413(17) . ? C1 C6 1.539(19) . ? C2 C3 1.46(2) . ? C2 C7 1.468(19) . ? C3 C4 1.383(19) . ? C3 C8 1.49(2) . ? C4 C5 1.443(18) . ? C4 C9 1.509(19) . ? C5 C10 1.450(18) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.371(16) . ? C11 C15 1.378(17) . ? C11 C16 1.560(16) . ? C12 C13 1.387(18) . ? C12 C17 1.492(18) . ? C13 C14 1.449(19) . ? C13 C18 1.507(18) . ? C14 C15 1.414(17) . ? C14 C19 1.521(18) . ? C15 C20 1.503(16) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.546(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C23 C24 1.392(18) . ? C23 C28 1.403(16) . ? C24 C25 1.33(2) . ? C24 H24 0.9500 . ? C25 C26 1.45(3) . ? C25 H25 0.9500 . ? C26 C27 1.32(2) . ? C26 H26 0.9500 . ? C27 C28 1.380(17) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.331(17) . ? C29 C34 1.408(17) . ? C30 C31 1.43(2) . ? C30 H30 0.9500 . ? C31 C32 1.37(3) . ? C31 H31 0.9500 . ? C32 C33 1.39(3) . ? C32 H32 0.9500 . ? C33 C34 1.360(19) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? Cl1 O2 1.362(15) . ? Cl1 O3 1.400(14) . ? Cl1 O4 1.402(10) . ? Cl1 O1 1.448(14) . ? Cl2 O6 1.358(9) . ? Cl2 O7 1.359(9) . ? Cl2 O8 1.377(9) . ? Cl2 O5 1.393(9) . ? P2 C41 1.798(11) . ? P2 C35 1.804(11) . ? P2 C22 1.819(10) . ? P2 Cu2 2.214(3) 2_655 ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C35 C36 1.384(17) . ? C35 C40 1.387(17) . ? C36 C37 1.44(2) . ? C36 H36 0.9500 . ? C37 C38 1.27(3) . ? C37 H37 0.9500 . ? C38 C39 1.43(3) . ? C38 H38 0.9500 . ? C39 C40 1.388(19) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.388(16) . ? C41 C46 1.395(18) . ? C42 C43 1.389(18) . ? C42 H42 0.9500 . ? C43 C44 1.37(2) . ? C43 H43 0.9500 . ? C44 C45 1.30(2) . ? C44 H44 0.9500 . ? C45 C46 1.37(2) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? 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 S1 Mo1 S4 106.74(10) . . ? S1 Mo1 S3 105.59(10) . . ? S4 Mo1 S3 100.50(10) . . ? S1 Mo1 C1 103.0(3) . . ? S4 Mo1 C1 142.4(3) . . ? S3 Mo1 C1 93.1(3) . . ? S1 Mo1 C3 99.1(4) . . ? S4 Mo1 C3 94.4(4) . . ? S3 Mo1 C3 145.8(3) . . ? C1 Mo1 C3 58.1(4) . . ? S1 Mo1 C5 137.7(3) . . ? S4 Mo1 C5 110.2(3) . . ? S3 Mo1 C5 87.4(3) . . ? C1 Mo1 C5 35.2(4) . . ? C3 Mo1 C5 58.5(4) . . ? S1 Mo1 C4 133.3(3) . . ? S4 Mo1 C4 84.4(3) . . ? S3 Mo1 C4 116.9(3) . . ? C1 Mo1 C4 58.3(4) . . ? C3 Mo1 C4 34.2(5) . . ? C5 Mo1 C4 35.7(4) . . ? S1 Mo1 C2 82.9(3) . . ? S4 Mo1 C2 129.8(4) . . ? S3 Mo1 C2 124.7(4) . . ? C1 Mo1 C2 33.7(4) . . ? C3 Mo1 C2 35.8(5) . . ? C5 Mo1 C2 57.7(4) . . ? C4 Mo1 C2 57.8(4) . . ? S1 Mo1 Cu1 55.20(7) . . ? S4 Mo1 Cu1 103.13(8) . . ? S3 Mo1 Cu1 51.62(7) . . ? C1 Mo1 Cu1 112.7(3) . . ? C3 Mo1 Cu1 152.1(4) . . ? C5 Mo1 Cu1 131.3(3) . . ? C4 Mo1 Cu1 166.9(3) . . ? C2 Mo1 Cu1 121.0(3) . . ? S1 Mo1 Cu2 56.15(8) . . ? S4 Mo1 Cu2 51.68(7) . . ? S3 Mo1 Cu2 102.94(7) . . ? C1 Mo1 Cu2 156.3(3) . . ? C3 Mo1 Cu2 110.4(3) . . ? C5 Mo1 Cu2 160.1(3) . . ? C4 Mo1 Cu2 125.6(3) . . ? C2 Mo1 Cu2 124.5(3) . . ? Cu1 Mo1 Cu2 66.77(5) . . ? S1 Mo1 Mo2 99.53(8) . . ? S4 Mo1 Mo2 52.22(7) . . ? S3 Mo1 Mo2 52.05(7) . . ? C1 Mo1 Mo2 142.7(3) . . ? C3 Mo1 Mo2 145.4(4) . . ? C5 Mo1 Mo2 119.2(3) . . ? C4 Mo1 Mo2 121.2(3) . . ? C2 Mo1 Mo2 176.4(4) . . ? Cu1 Mo1 Mo2 59.08(4) . . ? Cu2 Mo1 Mo2 59.06(3) . . ? S2 Mo2 C12 142.2(3) . . ? S2 Mo2 C11 114.3(3) . . ? C12 Mo2 C11 34.3(4) . . ? S2 Mo2 S3 106.17(10) . . ? C12 Mo2 S3 94.0(3) . . ? C11 Mo2 S3 86.3(3) . . ? S2 Mo2 S4 105.22(9) . . ? C12 Mo2 S4 102.0(3) . . ? C11 Mo2 S4 136.3(3) . . ? S3 Mo2 S4 100.50(10) . . ? S2 Mo2 C13 122.2(4) . . ? C12 Mo2 C13 34.7(4) . . ? C11 Mo2 C13 57.4(4) . . ? S3 Mo2 C13 127.5(4) . . ? S4 Mo2 C13 86.3(3) . . ? S2 Mo2 C14 88.5(3) . . ? C12 Mo2 C14 58.2(4) . . ? C11 Mo2 C14 57.3(4) . . ? S3 Mo2 C14 143.5(3) . . ? S4 Mo2 C14 107.7(3) . . ? C13 Mo2 C14 35.7(5) . . ? S2 Mo2 C15 85.6(3) . . ? C12 Mo2 C15 57.0(4) . . ? C11 Mo2 C15 33.9(4) . . ? S3 Mo2 C15 112.1(3) . . ? S4 Mo2 C15 141.3(3) . . ? C13 Mo2 C15 57.6(4) . . ? C14 Mo2 C15 34.4(4) . . ? S2 Mo2 Cu1 55.73(7) . . ? C12 Mo2 Cu1 140.6(3) . . ? C11 Mo2 Cu1 114.5(3) . . ? S3 Mo2 Cu1 51.50(7) . . ? S4 Mo2 Cu1 102.66(8) . . ? C13 Mo2 Cu1 171.0(3) . . ? C14 Mo2 Cu1 138.2(3) . . ? C15 Mo2 Cu1 113.7(3) . . ? S2 Mo2 Cu2 54.80(7) . . ? C12 Mo2 Cu2 150.5(3) . . ? C11 Mo2 Cu2 167.1(3) . . ? S3 Mo2 Cu2 102.94(7) . . ? S4 Mo2 Cu2 51.56(7) . . ? C13 Mo2 Cu2 120.3(3) . . ? C14 Mo2 Cu2 112.6(3) . . ? C15 Mo2 Cu2 133.3(3) . . ? Cu1 Mo2 Cu2 66.55(4) . . ? S2 Mo2 Mo1 98.74(7) . . ? C12 Mo2 Mo1 118.7(3) . . ? C11 Mo2 Mo1 133.5(3) . . ? S3 Mo2 Mo1 52.24(7) . . ? S4 Mo2 Mo1 52.04(7) . . ? C13 Mo2 Mo1 129.1(3) . . ? C14 Mo2 Mo1 159.6(3) . . ? C15 Mo2 Mo1 164.4(3) . . ? Cu1 Mo2 Mo1 58.72(4) . . ? Cu2 Mo2 Mo1 58.88(4) . . ? P1 Cu1 S3 119.33(11) . . ? P1 Cu1 S1 122.54(10) . . ? S3 Cu1 S1 104.26(10) . . ? P1 Cu1 S2 105.87(11) . . ? S3 Cu1 S2 103.66(10) . . ? S1 Cu1 S2 97.39(10) . . ? P1 Cu1 Mo1 156.31(9) . . ? S3 Cu1 Mo1 54.29(7) . . ? S1 Cu1 Mo1 51.17(7) . . ? S2 Cu1 Mo1 97.78(8) . . ? P1 Cu1 Mo2 136.20(9) . . ? S3 Cu1 Mo2 53.96(7) . . ? S1 Cu1 Mo2 98.99(8) . . ? S2 Cu1 Mo2 50.71(7) . . ? Mo1 Cu1 Mo2 62.20(4) . . ? P1 Cu1 Cu2 141.70(9) . . ? S3 Cu1 Cu2 97.00(8) . . ? S1 Cu1 Cu2 50.92(7) . . ? S2 Cu1 Cu2 49.61(7) . . ? Mo1 Cu1 Cu2 56.74(4) . . ? Mo2 Cu1 Cu2 56.76(4) . . ? P2 Cu2 S4 118.56(11) 2_655 . ? P2 Cu2 S2 120.92(10) 2_655 . ? S4 Cu2 S2 103.81(10) . . ? P2 Cu2 S1 109.43(11) 2_655 . ? S4 Cu2 S1 103.70(10) . . ? S2 Cu2 S1 97.18(10) . . ? P2 Cu2 Mo1 139.33(9) 2_655 . ? S4 Cu2 Mo1 53.96(8) . . ? S2 Cu2 Mo1 98.37(7) . . ? S1 Cu2 Mo1 50.77(7) . . ? P2 Cu2 Mo2 152.56(9) 2_655 . ? S4 Cu2 Mo2 54.02(7) . . ? S2 Cu2 Mo2 50.90(7) . . ? S1 Cu2 Mo2 97.93(8) . . ? Mo1 Cu2 Mo2 62.07(4) . . ? P2 Cu2 Cu1 143.85(9) 2_655 . ? S4 Cu2 Cu1 96.68(8) . . ? S2 Cu2 Cu1 50.57(7) . . ? S1 Cu2 Cu1 49.74(7) . . ? Mo1 Cu2 Cu1 56.49(4) . . ? Mo2 Cu2 Cu1 56.68(4) . . ? Mo1 S1 Cu1 73.63(8) . . ? Mo1 S1 Cu2 73.08(9) . . ? Cu1 S1 Cu2 79.34(9) . . ? Mo2 S2 Cu2 74.30(8) . . ? Mo2 S2 Cu1 73.57(8) . . ? Cu2 S2 Cu1 79.82(9) . . ? Cu1 S3 Mo2 74.54(9) . . ? Cu1 S3 Mo1 74.09(8) . . ? Mo2 S3 Mo1 75.72(8) . . ? Cu2 S4 Mo1 74.37(9) . . ? Cu2 S4 Mo2 74.42(8) . . ? Mo1 S4 Mo2 75.74(8) . . ? C23 P1 C29 104.3(5) . . ? C23 P1 C21 104.5(5) . . ? C29 P1 C21 103.1(5) . . ? C23 P1 Cu1 117.5(4) . . ? C29 P1 Cu1 113.4(4) . . ? C21 P1 Cu1 112.5(4) . . ? C2 C1 C5 110.4(11) . . ? C2 C1 C6 125.6(13) . . ? C5 C1 C6 123.7(12) . . ? C2 C1 Mo1 75.4(7) . . ? C5 C1 Mo1 72.8(6) . . ? C6 C1 Mo1 124.1(8) . . ? C1 C2 C3 107.0(11) . . ? C1 C2 C7 125.3(14) . . ? C3 C2 C7 127.3(15) . . ? C1 C2 Mo1 71.0(7) . . ? C3 C2 Mo1 70.3(6) . . ? C7 C2 Mo1 129.5(9) . . ? C4 C3 C2 108.1(12) . . ? C4 C3 C8 126.9(16) . . ? C2 C3 C8 124.7(15) . . ? C4 C3 Mo1 73.6(7) . . ? C2 C3 Mo1 73.9(7) . . ? C8 C3 Mo1 123.8(10) . . ? C3 C4 C5 108.1(12) . . ? C3 C4 C9 124.9(14) . . ? C5 C4 C9 126.9(13) . . ? C3 C4 Mo1 72.2(7) . . ? C5 C4 Mo1 71.5(6) . . ? C9 C4 Mo1 124.0(9) . . ? C1 C5 C4 106.3(11) . . ? C1 C5 C10 127.4(13) . . ? C4 C5 C10 125.8(13) . . ? C1 C5 Mo1 72.1(6) . . ? C4 C5 Mo1 72.7(6) . . ? C10 C5 Mo1 126.3(9) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 110.2(10) . . ? C12 C11 C16 125.7(11) . . ? C15 C11 C16 123.4(11) . . ? C12 C11 Mo2 72.8(6) . . ? C15 C11 Mo2 76.1(6) . . ? C16 C11 Mo2 125.5(8) . . ? C11 C12 C13 108.3(11) . . ? C11 C12 C17 125.0(13) . . ? C13 C12 C17 126.7(13) . . ? C11 C12 Mo2 72.9(6) . . ? C13 C12 Mo2 73.2(6) . . ? C17 C12 Mo2 122.3(9) . . ? C12 C13 C14 107.7(10) . . ? C12 C13 C18 126.8(14) . . ? C14 C13 C18 124.8(14) . . ? C12 C13 Mo2 72.2(7) . . ? C14 C13 Mo2 74.2(6) . . ? C18 C13 Mo2 126.7(8) . . ? C15 C14 C13 105.7(10) . . ? C15 C14 C19 127.8(13) . . ? C13 C14 C19 126.4(13) . . ? C15 C14 Mo2 73.3(6) . . ? C13 C14 Mo2 70.1(6) . . ? C19 C14 Mo2 124.4(9) . . ? C11 C15 C14 108.0(10) . . ? C11 C15 C20 129.7(12) . . ? C14 C15 C20 122.2(12) . . ? C11 C15 Mo2 70.0(6) . . ? C14 C15 Mo2 72.4(6) . . ? C20 C15 Mo2 124.8(8) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P1 110.9(7) . . ? C22 C21 H21A 109.5 . . ? P1 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? P1 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C24 C23 C28 117.8(12) . . ? C24 C23 P1 122.5(10) . . ? C28 C23 P1 119.6(9) . . ? C25 C24 C23 122.0(15) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C24 C25 C26 119.2(16) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 118.8(14) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 121.9(15) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C27 C28 C23 120.0(12) . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? C30 C29 C34 119.7(12) . . ? C30 C29 P1 123.6(10) . . ? C34 C29 P1 116.5(10) . . ? C29 C30 C31 120.2(14) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 118.6(15) . . ? C32 C31 H31 120.7 . . ? C30 C31 H31 120.7 . . ? C31 C32 C33 121.2(13) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C34 C33 C32 118.5(14) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C33 C34 C29 121.4(14) . . ? C33 C34 H34 119.3 . . ? C29 C34 H34 119.3 . . ? O2 Cl1 O3 106.7(14) . . ? O2 Cl1 O4 111.2(12) . . ? O3 Cl1 O4 108.7(9) . . ? O2 Cl1 O1 108.7(12) . . ? O3 Cl1 O1 111.6(12) . . ? O4 Cl1 O1 109.8(8) . . ? O6 Cl2 O7 112.5(5) . . ? O6 Cl2 O8 110.1(5) . . ? O7 Cl2 O8 110.0(5) . . ? O6 Cl2 O5 109.0(5) . . ? O7 Cl2 O5 108.1(5) . . ? O8 Cl2 O5 106.9(5) . . ? C41 P2 C35 106.7(5) . . ? C41 P2 C22 104.2(5) . . ? C35 P2 C22 102.4(5) . . ? C41 P2 Cu2 113.1(3) . 2_655 ? C35 P2 Cu2 117.1(4) . 2_655 ? C22 P2 Cu2 112.1(3) . 2_655 ? C21 C22 P2 110.4(7) . . ? C21 C22 H22A 109.6 . . ? P2 C22 H22A 109.6 . . ? C21 C22 H22B 109.6 . . ? P2 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C36 C35 C40 119.2(11) . . ? C36 C35 P2 119.3(9) . . ? C40 C35 P2 121.4(9) . . ? C35 C36 C37 117.6(15) . . ? C35 C36 H36 121.2 . . ? C37 C36 H36 121.2 . . ? C38 C37 C36 123.7(18) . . ? C38 C37 H37 118.1 . . ? C36 C37 H37 118.1 . . ? C37 C38 C39 119.6(15) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C40 C39 C38 118.8(14) . . ? C40 C39 H39 120.6 . . ? C38 C39 H39 120.6 . . ? C35 C40 C39 120.9(13) . . ? C35 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C42 C41 C46 116.9(11) . . ? C42 C41 P2 121.3(9) . . ? C46 C41 P2 121.5(9) . . ? C41 C42 C43 119.7(13) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C44 C43 C42 121.1(13) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C45 C44 C43 119.2(14) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C44 C45 C46 122.5(15) . . ? C44 C45 H45 118.8 . . ? C46 C45 H45 118.8 . . ? C45 C46 C41 120.5(13) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.807 _refine_diff_density_min -2.880 _refine_diff_density_rms 0.178 #===END #============================================================================== data_82MeCN _database_code_depnum_ccdc_archive 'CCDC 679381' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H116 Cu4 Mo4 P4 S8, 2(C2 H3 N), 4(Cl O4)' _chemical_formula_sum 'C100 H122 Cl4 Cu4 Mo4 N2 O16 P4 S8' _chemical_formula_weight 2768.20 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.667(3) _cell_length_b 25.855(5) _cell_length_c 26.805(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.64(3) _cell_angle_gamma 90.00 _cell_volume 11473(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 44957 _cell_measurement_theta_min 2.9999 _cell_measurement_theta_max 27.4835 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5616 _exptl_absorpt_coefficient_mu 1.503 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4658 _exptl_absorpt_correction_T_max 0.7237 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 128327 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 26273 _reflns_number_gt 20692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+9.5000P] 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 26273 _refine_ls_number_parameters 1032 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0870 _refine_ls_wR_factor_ref 0.2584 _refine_ls_wR_factor_gt 0.2394 _refine_ls_goodness_of_fit_ref 1.278 _refine_ls_restrained_S_all 1.279 _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 1.04051(4) 0.99926(2) 0.32264(2) 0.03514(16) Uani 1 1 d . . . Mo2 Mo 1.05503(3) 0.96170(2) 0.22345(2) 0.03165(15) Uani 1 1 d . . . Mo3 Mo 0.55827(3) 0.76027(2) 0.50153(2) 0.03019(15) Uani 1 1 d . . . Mo4 Mo 0.49029(3) 0.68305(2) 0.43231(2) 0.02958(15) Uani 1 1 d . . . Cu1 Cu 1.02339(5) 0.89516(3) 0.29907(3) 0.0353(2) Uani 1 1 d . . . Cu2 Cu 0.90523(5) 0.97028(4) 0.25773(4) 0.0408(2) Uani 1 1 d . . . Cu3 Cu 0.65572(5) 0.69750(3) 0.45041(3) 0.03215(19) Uani 1 1 d . . . Cu4 Cu 0.54579(5) 0.77765(3) 0.39959(3) 0.0352(2) Uani 1 1 d . . . S1 S 0.94073(12) 0.94973(7) 0.34392(7) 0.0393(4) Uani 1 1 d . . . S2 S 0.96032(11) 0.90022(7) 0.21630(7) 0.0370(4) Uani 1 1 d . . . S3 S 1.13642(10) 0.94215(7) 0.29740(6) 0.0358(4) Uani 1 1 d . . . S4 S 0.99002(12) 1.03693(7) 0.24592(7) 0.0393(4) Uani 1 1 d . . . S5 S 0.65789(10) 0.78899(6) 0.45971(7) 0.0336(4) Uani 1 1 d . . . S6 S 0.57283(11) 0.69124(7) 0.37293(6) 0.0353(4) Uani 1 1 d . . . S7 S 0.57421(10) 0.67073(7) 0.50682(6) 0.0317(3) Uani 1 1 d . . . S8 S 0.44116(10) 0.76619(7) 0.44504(7) 0.0345(4) Uani 1 1 d . . . P1 P 1.02899(11) 0.82101(7) 0.34046(7) 0.0318(4) Uani 1 1 d . . . P2 P 0.77764(10) 0.66218(6) 0.46317(7) 0.0300(4) Uani 1 1 d . . . P3 P 0.77236(11) 0.96987(8) 0.23631(7) 0.0384(4) Uani 1 1 d . . . P4 P 0.52278(11) 0.82727(7) 0.33224(7) 0.0349(4) Uani 1 1 d . . . N1 N 1.1857(11) 0.7972(5) 0.6181(4) 0.140(6) Uani 1 1 d . . . N2 N 1.3506(15) 0.9741(8) 0.5055(7) 0.195(10) Uani 1 1 d . . . C1 C 1.1482(3) 1.03173(19) 0.37894(16) 0.059(2) Uani 1 1 d G . . C2 C 1.0901(3) 1.01435(16) 0.40905(15) 0.0413(16) Uani 1 1 d G . . C3 C 1.0209(3) 1.04530(16) 0.39868(15) 0.054(2) Uani 1 1 d G . . C4 C 1.0362(3) 1.08180(17) 0.36214(17) 0.079(4) Uani 1 1 d G . . C5 C 1.1149(3) 1.0734(2) 0.34995(18) 0.086(4) Uani 1 1 d G . . C6 C 1.2308(4) 1.0097(3) 0.3779(3) 0.0879(16) Uani 1 1 d G . . H6A H 1.2397 0.9820 0.4028 0.132 Uiso 1 1 calc R . . H6B H 1.2712 1.0370 0.3858 0.132 Uiso 1 1 calc R . . H6C H 1.2359 0.9958 0.3444 0.132 Uiso 1 1 calc R . . C7 C 1.1001(4) 0.9707(3) 0.4457(2) 0.0879(16) Uani 1 1 d G . . H7A H 1.1332 0.9435 0.4327 0.132 Uiso 1 1 calc R . . H7B H 1.0469 0.9565 0.4504 0.132 Uiso 1 1 calc R . . H7C H 1.1267 0.9832 0.4779 0.132 Uiso 1 1 calc R . . C8 C 0.9444(4) 1.0403(3) 0.4223(3) 0.0879(16) Uani 1 1 d G . . H8A H 0.9353 1.0038 0.4301 0.132 Uiso 1 1 calc R . . H8B H 0.8991 1.0531 0.3990 0.132 Uiso 1 1 calc R . . H8C H 0.9486 1.0606 0.4534 0.132 Uiso 1 1 calc R . . C9 C 0.9790(5) 1.1224(3) 0.3401(3) 0.0879(16) Uani 1 1 d G . . H9A H 1.0021 1.1400 0.3127 0.132 Uiso 1 1 calc R . . H9B H 0.9697 1.1476 0.3661 0.132 Uiso 1 1 calc R . . H9C H 0.9276 1.1063 0.3271 0.132 Uiso 1 1 calc R . . C10 C 1.1558(6) 1.1066(4) 0.3132(3) 0.0879(16) Uani 1 1 d GU . . H10A H 1.1223 1.1070 0.2806 0.132 Uiso 1 1 calc R . . H10B H 1.2089 1.0920 0.3091 0.132 Uiso 1 1 calc R . . H10C H 1.1623 1.1419 0.3262 0.132 Uiso 1 1 calc R . . C11 C 1.1596(3) 0.93572(17) 0.17857(15) 0.064(3) Uani 1 1 d G . . C12 C 1.1674(2) 0.98993(17) 0.18665(14) 0.065(3) Uani 1 1 d G . . C13 C 1.1007(3) 1.01216(15) 0.15931(13) 0.061(3) Uani 1 1 d G . . C14 C 1.0513(3) 0.97232(17) 0.13568(15) 0.052(2) Uani 1 1 d G . . C15 C 1.0909(3) 0.92577(18) 0.14673(15) 0.060(2) Uani 1 1 d G . . C16 C 1.2235(4) 0.8969(2) 0.1969(2) 0.104(2) Uani 1 1 d G . . H16A H 1.2422 0.9037 0.2324 0.157 Uiso 1 1 calc R . . H16B H 1.2691 0.9000 0.1771 0.157 Uiso 1 1 calc R . . H16C H 1.2009 0.8620 0.1934 0.157 Uiso 1 1 calc R . . C17 C 1.2383(3) 1.0176(2) 0.2140(2) 0.104(2) Uani 1 1 d G . . H17A H 1.2697 1.0341 0.1896 0.157 Uiso 1 1 calc R . . H17B H 1.2725 0.9927 0.2342 0.157 Uiso 1 1 calc R . . H17C H 1.2192 1.0440 0.2359 0.157 Uiso 1 1 calc R . . C18 C 1.0840(4) 1.0680(2) 0.1510(2) 0.104(2) Uani 1 1 d G . . H18A H 1.0994 1.0870 0.1823 0.157 Uiso 1 1 calc R . . H18B H 1.0262 1.0730 0.1404 0.157 Uiso 1 1 calc R . . H18C H 1.1153 1.0810 0.1249 0.157 Uiso 1 1 calc R . . C19 C 0.9765(4) 0.9783(2) 0.1002(2) 0.104(2) Uani 1 1 d G . . H19A H 0.9904 0.9783 0.0656 0.157 Uiso 1 1 calc R . . H19B H 0.9502 1.0111 0.1069 0.157 Uiso 1 1 calc R . . H19C H 0.9397 0.9496 0.1046 0.157 Uiso 1 1 calc R . . C20 C 1.0628(4) 0.8761(2) 0.1229(2) 0.104(2) Uani 1 1 d G . . H20A H 1.0946 0.8476 0.1391 0.157 Uiso 1 1 calc R . . H20B H 1.0696 0.8770 0.0871 0.157 Uiso 1 1 calc R . . H20C H 1.0056 0.8710 0.1268 0.157 Uiso 1 1 calc R . . C21 C 0.4996(2) 0.82388(15) 0.55156(15) 0.054(2) Uani 1 1 d G . . C22 C 0.4957(2) 0.77493(17) 0.57526(15) 0.057(2) Uani 1 1 d G . . C23 C 0.5760(3) 0.75839(15) 0.59078(14) 0.053(2) Uani 1 1 d G . . C24 C 0.6295(2) 0.79714(14) 0.57667(13) 0.0462(19) Uani 1 1 d G . . C25 C 0.5823(2) 0.83762(13) 0.55243(14) 0.0434(17) Uani 1 1 d G . . C26 C 0.4282(3) 0.8557(2) 0.5293(2) 0.084(4) Uani 1 1 d G . . H26A H 0.3830 0.8328 0.5181 0.126 Uiso 1 1 calc R . . H26B H 0.4433 0.8755 0.5007 0.126 Uiso 1 1 calc R . . H26C H 0.4122 0.8796 0.5548 0.126 Uiso 1 1 calc R . . C27 C 0.4196(4) 0.7456(3) 0.5827(2) 0.109(5) Uani 1 1 d G . . H27A H 0.3907 0.7637 0.6073 0.163 Uiso 1 1 calc R . . H27B H 0.4337 0.7107 0.5949 0.163 Uiso 1 1 calc R . . H27C H 0.3849 0.7434 0.5506 0.163 Uiso 1 1 calc R . . C28 C 0.6003(4) 0.7084(2) 0.6176(2) 0.097(4) Uani 1 1 d G . . H28A H 0.5633 0.6808 0.6047 0.146 Uiso 1 1 calc R . . H28B H 0.5979 0.7127 0.6537 0.146 Uiso 1 1 calc R . . H28C H 0.6555 0.6993 0.6117 0.146 Uiso 1 1 calc R . . C29 C 0.7207(3) 0.7956(2) 0.5858(2) 0.061(2) Uani 1 1 d G . . H29A H 0.7433 0.8166 0.5604 0.091 Uiso 1 1 calc R . . H29B H 0.7392 0.7598 0.5836 0.091 Uiso 1 1 calc R . . H29C H 0.7386 0.8094 0.6193 0.091 Uiso 1 1 calc R . . C30 C 0.6143(3) 0.88663(19) 0.5313(2) 0.066(3) Uani 1 1 d G . . H30A H 0.6190 0.9136 0.5572 0.099 Uiso 1 1 calc R . . H30B H 0.5771 0.8982 0.5024 0.099 Uiso 1 1 calc R . . H30C H 0.6676 0.8799 0.5205 0.099 Uiso 1 1 calc R . . C31 C 0.3866(2) 0.62961(13) 0.45742(13) 0.0462(19) Uani 1 1 d G . . C32 C 0.4449(2) 0.59592(12) 0.44093(13) 0.0416(18) Uani 1 1 d G . . C33 C 0.4459(2) 0.60362(12) 0.38878(13) 0.0436(18) Uani 1 1 d G . . C34 C 0.3882(2) 0.64210(13) 0.37304(12) 0.0402(17) Uani 1 1 d G . . C35 C 0.35149(19) 0.65816(13) 0.41546(13) 0.0454(19) Uani 1 1 d G . . C36 C 0.3655(3) 0.6343(2) 0.51028(18) 0.059(2) Uani 1 1 d G . . H36A H 0.4131 0.6262 0.5340 0.089 Uiso 1 1 calc R . . H36B H 0.3219 0.6100 0.5152 0.089 Uiso 1 1 calc R . . H36C H 0.3477 0.6697 0.5161 0.089 Uiso 1 1 calc R . . C37 C 0.4968(3) 0.55846(18) 0.47318(19) 0.060(3) Uani 1 1 d G . . H37A H 0.4829 0.5230 0.4625 0.090 Uiso 1 1 calc R . . H37B H 0.4875 0.5629 0.5084 0.090 Uiso 1 1 calc R . . H37C H 0.5538 0.5650 0.4697 0.090 Uiso 1 1 calc R . . C38 C 0.4990(3) 0.5758(2) 0.35586(18) 0.068(3) Uani 1 1 d G . . H38A H 0.5392 0.5552 0.3768 0.102 Uiso 1 1 calc R . . H38B H 0.5266 0.6012 0.3366 0.102 Uiso 1 1 calc R . . H38C H 0.4659 0.5530 0.3327 0.102 Uiso 1 1 calc R . . C39 C 0.3691(3) 0.6624(2) 0.32044(17) 0.059(2) Uani 1 1 d G . . H39A H 0.3296 0.6396 0.3015 0.089 Uiso 1 1 calc R . . H39B H 0.4186 0.6634 0.3040 0.089 Uiso 1 1 calc R . . H39C H 0.3467 0.6973 0.3215 0.089 Uiso 1 1 calc R . . C40 C 0.2866(3) 0.6985(2) 0.41588(19) 0.065(3) Uani 1 1 d G . . H40A H 0.2855 0.7200 0.3857 0.097 Uiso 1 1 calc R . . H40B H 0.2979 0.7202 0.4458 0.097 Uiso 1 1 calc R . . H40C H 0.2341 0.6815 0.4164 0.097 Uiso 1 1 calc R . . C41 C 0.9312(4) 0.8015(3) 0.3581(3) 0.0359(15) Uani 1 1 d . . . H41A H 0.9150 0.8266 0.3830 0.043 Uiso 1 1 calc R . . H41B H 0.8909 0.8038 0.3280 0.043 Uiso 1 1 calc R . . C42 C 0.9274(4) 0.7478(3) 0.3800(3) 0.0420(17) Uani 1 1 d . . . H42A H 0.9750 0.7425 0.4052 0.050 Uiso 1 1 calc R . . H42B H 0.9306 0.7221 0.3528 0.050 Uiso 1 1 calc R . . C43 C 0.8499(4) 0.7378(3) 0.4049(3) 0.0364(15) Uani 1 1 d . . . H43A H 0.8492 0.7602 0.4348 0.044 Uiso 1 1 calc R . . H43B H 0.8017 0.7458 0.3811 0.044 Uiso 1 1 calc R . . C44 C 0.8492(4) 0.6811(3) 0.4203(3) 0.0368(15) Uani 1 1 d . . . H44A H 0.9041 0.6719 0.4360 0.044 Uiso 1 1 calc R . . H44B H 0.8382 0.6600 0.3894 0.044 Uiso 1 1 calc R . . C45 C 1.0960(3) 0.8272(2) 0.39900(14) 0.0384(16) Uani 1 1 d G . . C46 C 1.1777(3) 0.8349(2) 0.39572(16) 0.0476(19) Uani 1 1 d G . . H46 H 1.1978 0.8335 0.3640 0.057 Uiso 1 1 calc R . . C47 C 1.2302(2) 0.8446(2) 0.4389(2) 0.061(2) Uani 1 1 d G . . H47 H 1.2860 0.8499 0.4366 0.073 Uiso 1 1 calc R . . C48 C 1.2008(3) 0.8466(2) 0.48533(17) 0.063(3) Uani 1 1 d G . . H48 H 1.2367 0.8533 0.5148 0.076 Uiso 1 1 calc R . . C49 C 1.1191(3) 0.8389(2) 0.48861(14) 0.060(2) Uani 1 1 d G . . H49 H 1.0990 0.8403 0.5203 0.072 Uiso 1 1 calc R . . C50 C 1.0666(2) 0.8292(2) 0.44544(18) 0.0478(19) Uani 1 1 d G . . H50 H 1.0108 0.8239 0.4477 0.057 Uiso 1 1 calc R . . C51 C 1.0684(3) 0.76712(16) 0.30736(18) 0.0360(15) Uani 1 1 d G . . C52 C 1.0672(4) 0.77011(18) 0.25550(18) 0.054(2) Uani 1 1 d G . . H52 H 1.0457 0.7999 0.2380 0.065 Uiso 1 1 calc R . . C53 C 1.0976(4) 0.7296(2) 0.22928(15) 0.074(3) Uani 1 1 d G . . H53 H 1.0968 0.7316 0.1938 0.088 Uiso 1 1 calc R . . C54 C 1.1292(4) 0.6860(2) 0.2549(2) 0.075(3) Uani 1 1 d G . . H54 H 1.1500 0.6583 0.2370 0.089 Uiso 1 1 calc R . . C55 C 1.1304(4) 0.68304(17) 0.3068(2) 0.054(2) Uani 1 1 d G . . H55 H 1.1519 0.6533 0.3243 0.065 Uiso 1 1 calc R . . C56 C 1.1000(3) 0.72358(18) 0.33299(15) 0.0454(18) Uani 1 1 d G . . H56 H 1.1008 0.7215 0.3684 0.055 Uiso 1 1 calc R . . C57 C 0.8251(3) 0.67688(19) 0.52640(14) 0.0344(14) Uani 1 1 d G . . C58 C 0.7952(3) 0.6529(2) 0.56687(19) 0.052(2) Uani 1 1 d G . . H58 H 0.7541 0.6275 0.5612 0.062 Uiso 1 1 calc R . . C59 C 0.8256(3) 0.6662(2) 0.61567(16) 0.063(3) Uani 1 1 d G . . H59 H 0.8052 0.6498 0.6433 0.076 Uiso 1 1 calc R . . C60 C 0.8859(4) 0.7034(2) 0.62400(15) 0.059(2) Uani 1 1 d G . . H60 H 0.9067 0.7125 0.6573 0.071 Uiso 1 1 calc R . . C61 C 0.9157(3) 0.7274(2) 0.5835(2) 0.068(3) Uani 1 1 d G . . H61 H 0.9569 0.7528 0.5892 0.082 Uiso 1 1 calc R . . C62 C 0.8853(3) 0.7141(2) 0.53473(18) 0.053(2) Uani 1 1 d G . . H62 H 0.9057 0.7305 0.5071 0.063 Uiso 1 1 calc R . . C63 C 0.7771(3) 0.59180(12) 0.45808(18) 0.0311(14) Uani 1 1 d G . . C64 C 0.8416(2) 0.56205(16) 0.47943(18) 0.0421(17) Uani 1 1 d G . . H64 H 0.8853 0.5780 0.4996 0.050 Uiso 1 1 calc R . . C65 C 0.8420(3) 0.50896(15) 0.47127(19) 0.0422(17) Uani 1 1 d G . . H65 H 0.8861 0.4886 0.4859 0.051 Uiso 1 1 calc R . . C66 C 0.7781(3) 0.48563(12) 0.44176(19) 0.0441(18) Uani 1 1 d G . . H66 H 0.7784 0.4494 0.4362 0.053 Uiso 1 1 calc R . . C67 C 0.7136(3) 0.51539(16) 0.42041(19) 0.051(2) Uani 1 1 d G . . H67 H 0.6698 0.4994 0.4002 0.061 Uiso 1 1 calc R . . C68 C 0.7131(2) 0.56848(16) 0.42856(18) 0.0437(17) Uani 1 1 d G . . H68 H 0.6690 0.5888 0.4140 0.052 Uiso 1 1 calc R . . C69 C 0.7213(5) 0.9106(3) 0.2497(3) 0.0476(19) Uani 1 1 d . . . H69A H 0.6628 0.9148 0.2388 0.057 Uiso 1 1 calc R . . H69B H 0.7413 0.8824 0.2294 0.057 Uiso 1 1 calc R . . C70 C 0.7323(8) 0.8946(6) 0.3044(4) 0.095(3) Uani 1 1 d . . . H70A H 0.7746 0.8675 0.3083 0.114 Uiso 1 1 calc R . . H70B H 0.7541 0.9249 0.3242 0.114 Uiso 1 1 calc R . . C71 C 0.6697(8) 0.8771(6) 0.3257(4) 0.095(3) Uani 1 1 d . . . H71A H 0.6372 0.9074 0.3335 0.114 Uiso 1 1 calc R . . H71B H 0.6911 0.8613 0.3582 0.114 Uiso 1 1 calc R . . C72 C 0.6091(5) 0.8362(4) 0.2970(4) 0.058(2) Uani 1 1 d . . . H72A H 0.6371 0.8028 0.2939 0.069 Uiso 1 1 calc R . . H72B H 0.5904 0.8490 0.2628 0.069 Uiso 1 1 calc R . . C73 C 0.7206(3) 1.0187(2) 0.2688(2) 0.0476(19) Uani 1 1 d G . . C74 C 0.7670(3) 1.0537(2) 0.2992(3) 0.063(2) Uani 1 1 d G . . H74 H 0.8243 1.0514 0.3025 0.075 Uiso 1 1 calc R . . C75 C 0.7297(5) 1.0920(2) 0.3246(3) 0.086(3) Uani 1 1 d G . . H75 H 0.7614 1.1159 0.3453 0.103 Uiso 1 1 calc R . . C76 C 0.6459(5) 1.0954(2) 0.3197(3) 0.079(3) Uani 1 1 d G . . H76 H 0.6204 1.1215 0.3371 0.095 Uiso 1 1 calc R . . C77 C 0.5995(3) 1.0604(3) 0.2894(3) 0.075(3) Uani 1 1 d G . . H77 H 0.5422 1.0627 0.2861 0.090 Uiso 1 1 calc R . . C78 C 0.6368(3) 1.0221(2) 0.2640(2) 0.063(2) Uani 1 1 d G . . H78 H 0.6050 0.9982 0.2432 0.076 Uiso 1 1 calc R . . C79 C 0.7439(3) 0.9833(2) 0.16978(14) 0.0386(16) Uani 1 1 d G . . C80 C 0.6867(3) 0.95391(19) 0.14038(18) 0.0494(19) Uani 1 1 d G . . H80 H 0.6600 0.9263 0.1550 0.059 Uiso 1 1 calc R . . C81 C 0.6686(3) 0.9649(2) 0.08957(17) 0.061(2) Uani 1 1 d G . . H81 H 0.6296 0.9449 0.0695 0.073 Uiso 1 1 calc R . . C82 C 0.7077(4) 1.0054(3) 0.06816(14) 0.066(3) Uani 1 1 d G . . H82 H 0.6954 1.0129 0.0334 0.079 Uiso 1 1 calc R . . C83 C 0.7649(4) 1.0348(2) 0.0976(2) 0.074(3) Uani 1 1 d G . . H83 H 0.7916 1.0624 0.0829 0.089 Uiso 1 1 calc R . . C84 C 0.7829(3) 1.0237(2) 0.1484(2) 0.060(2) Uani 1 1 d G . . H84 H 0.8220 1.0438 0.1685 0.072 Uiso 1 1 calc R . . C85 C 0.4861(4) 0.89151(16) 0.3433(2) 0.052(2) Uani 1 1 d G . . C86 C 0.4612(4) 0.9243(2) 0.30340(17) 0.056(2) Uani 1 1 d G . . H86 H 0.4599 0.9122 0.2698 0.067 Uiso 1 1 calc R . . C87 C 0.4380(4) 0.9747(2) 0.3126(2) 0.069(3) Uani 1 1 d G . . H87 H 0.4210 0.9971 0.2853 0.082 Uiso 1 1 calc R . . C88 C 0.4399(5) 0.99238(18) 0.3617(3) 0.084(4) Uani 1 1 d G . . H88 H 0.4240 1.0268 0.3680 0.101 Uiso 1 1 calc R . . C89 C 0.4648(5) 0.9596(2) 0.4016(2) 0.094(4) Uani 1 1 d G . . H89 H 0.4661 0.9717 0.4351 0.113 Uiso 1 1 calc R . . C90 C 0.4880(5) 0.9092(2) 0.39239(18) 0.073(3) Uani 1 1 d G . . H90 H 0.5050 0.8868 0.4197 0.088 Uiso 1 1 calc R . . C91 C 0.4442(3) 0.7987(2) 0.2886(2) 0.0447(18) Uani 1 1 d G . . C92 C 0.4635(4) 0.7660(3) 0.2506(2) 0.079(3) Uani 1 1 d G . . H92 H 0.5184 0.7599 0.2462 0.095 Uiso 1 1 calc R . . C93 C 0.4024(7) 0.7423(3) 0.2190(2) 0.111(6) Uani 1 1 d G . . H93 H 0.4156 0.7200 0.1930 0.133 Uiso 1 1 calc R . . C94 C 0.3220(6) 0.7512(3) 0.2255(3) 0.127(8) Uani 1 1 d G . . H94 H 0.2802 0.7350 0.2039 0.152 Uiso 1 1 calc R . . C95 C 0.3027(3) 0.7839(3) 0.2635(4) 0.110(6) Uani 1 1 d G . . H95 H 0.2478 0.7900 0.2679 0.132 Uiso 1 1 calc R . . C96 C 0.3638(4) 0.8076(2) 0.2951(3) 0.071(3) Uani 1 1 d G . . H96 H 0.3506 0.8300 0.3211 0.085 Uiso 1 1 calc R . . C97 C 1.1941(13) 0.7196(7) 0.5627(8) 0.162(9) Uani 1 1 d . . . H97A H 1.2490 0.7177 0.5530 0.243 Uiso 1 1 calc R . . H97B H 1.1553 0.7222 0.5324 0.243 Uiso 1 1 calc R . . H97C H 1.1828 0.6885 0.5814 0.243 Uiso 1 1 calc R . . C98 C 1.1873(8) 0.7642(5) 0.5934(5) 0.086(4) Uani 1 1 d . . . C99 C 1.2872(12) 1.0216(8) 0.5770(7) 0.135(6) Uani 1 1 d . . . H99A H 1.3279 1.0242 0.6063 0.203 Uiso 1 1 calc R . . H99B H 1.2394 1.0036 0.5864 0.203 Uiso 1 1 calc R . . H99C H 1.2718 1.0564 0.5648 0.203 Uiso 1 1 calc R . . C100 C 1.3195(11) 0.9936(7) 0.5384(7) 0.111(5) Uani 1 1 d . . . Cl1 Cl 1.08343(12) 0.63241(9) 0.46718(10) 0.0561(5) Uani 1 1 d . . . O1 O 1.0614(6) 0.6843(3) 0.4730(5) 0.132(4) Uani 1 1 d . . . O2 O 1.0248(5) 0.5969(4) 0.4801(4) 0.112(3) Uani 1 1 d . . . O3 O 1.0893(5) 0.6269(4) 0.4153(3) 0.099(3) Uani 1 1 d . . . O4 O 1.1593(4) 0.6218(3) 0.4945(3) 0.0687(19) Uani 1 1 d . . . Cl2 Cl 1.45644(14) 0.58398(9) 0.65223(8) 0.0553(5) Uani 1 1 d . . . O5 O 1.3966(6) 0.6227(5) 0.6412(4) 0.126(4) Uani 1 1 d . . . O6 O 1.5220(5) 0.6050(4) 0.6840(3) 0.092(3) Uani 1 1 d . . . O7 O 1.4811(5) 0.5653(4) 0.6062(3) 0.091(3) Uani 1 1 d . . . O8 O 1.4225(8) 0.5439(4) 0.6766(3) 0.115(4) Uani 1 1 d . . . Cl3 Cl 1.1338(2) 1.11690(12) 0.50858(16) 0.1021(10) Uani 1 1 d . . . O9 O 1.0870(5) 1.1531(3) 0.4779(4) 0.1021(10) Uani 1 1 d . . . O10 O 1.1712(5) 1.1404(3) 0.5524(4) 0.1021(10) Uani 1 1 d . . . O11 O 1.1897(5) 1.0957(3) 0.4797(4) 0.1021(10) Uani 1 1 d . . . O12 O 1.0783(5) 1.0796(3) 0.5198(4) 0.1021(10) Uani 1 1 d . . . Cl4 Cl 0.5907(3) 0.85968(19) 0.69681(18) 0.0907(11) Uani 0.70 1 d PD . . O13 O 0.6596(5) 0.8844(4) 0.6800(4) 0.0907(11) Uani 0.70 1 d PD . . O14 O 0.5756(6) 0.8797(4) 0.7418(3) 0.0907(11) Uani 0.70 1 d PD . . O15 O 0.6093(6) 0.8060(3) 0.7015(4) 0.0907(11) Uani 0.70 1 d PD . . O16 O 0.5260(5) 0.8659(4) 0.6591(4) 0.0907(11) Uani 0.70 1 d PD . . Cl4A Cl 0.7847(6) 0.7673(4) 0.7505(3) 0.089(3) Uani 0.30 1 d PD . . O14A O 0.8127(12) 0.7222(7) 0.7402(6) 0.089(3) Uani 0.30 1 d PD . . O13A O 0.7383(11) 0.7882(8) 0.7072(6) 0.089(3) Uani 0.30 1 d PD . . O15A O 0.8469(11) 0.8034(7) 0.7617(6) 0.089(3) Uani 0.30 1 d PD . . O16A O 0.7379(10) 0.7681(8) 0.7883(6) 0.089(3) Uani 0.30 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 Mo1 0.0441(4) 0.0318(3) 0.0292(3) 0.0036(2) 0.0028(2) -0.0056(3) Mo2 0.0300(3) 0.0370(3) 0.0279(3) 0.0065(2) 0.0036(2) -0.0062(2) Mo3 0.0272(3) 0.0340(3) 0.0295(3) -0.0007(2) 0.0036(2) -0.0022(2) Mo4 0.0276(3) 0.0290(3) 0.0307(3) 0.0062(2) -0.0026(2) -0.0058(2) Cu1 0.0368(5) 0.0329(4) 0.0355(5) 0.0085(3) 0.0020(3) -0.0064(3) Cu2 0.0326(5) 0.0475(5) 0.0423(5) 0.0118(4) 0.0042(4) -0.0031(4) Cu3 0.0273(4) 0.0345(4) 0.0345(4) 0.0028(3) 0.0028(3) 0.0006(3) Cu4 0.0347(4) 0.0352(4) 0.0355(5) 0.0090(3) 0.0031(3) -0.0039(4) S1 0.0448(10) 0.0420(10) 0.0324(9) 0.0076(7) 0.0100(7) -0.0034(8) S2 0.0362(9) 0.0419(9) 0.0323(9) 0.0032(7) 0.0012(7) -0.0091(7) S3 0.0333(9) 0.0401(9) 0.0332(9) 0.0048(7) -0.0002(7) -0.0054(7) S4 0.0468(10) 0.0351(9) 0.0359(9) 0.0087(7) 0.0046(8) -0.0018(8) S5 0.0304(8) 0.0319(8) 0.0386(9) -0.0008(7) 0.0048(7) -0.0061(7) S6 0.0396(9) 0.0349(9) 0.0310(8) 0.0011(7) 0.0022(7) -0.0031(7) S7 0.0303(8) 0.0362(8) 0.0278(8) 0.0055(6) -0.0003(6) -0.0031(7) S8 0.0282(8) 0.0354(9) 0.0395(9) 0.0048(7) 0.0017(7) -0.0014(7) P1 0.0315(9) 0.0308(8) 0.0331(9) 0.0058(7) 0.0041(7) -0.0014(7) P2 0.0278(8) 0.0286(8) 0.0340(9) 0.0022(7) 0.0047(7) -0.0016(7) P3 0.0331(9) 0.0463(11) 0.0364(10) 0.0105(8) 0.0068(7) -0.0022(8) P4 0.0364(9) 0.0348(9) 0.0332(9) 0.0075(7) 0.0032(7) -0.0049(7) N1 0.247(19) 0.106(9) 0.061(7) -0.012(7) -0.001(9) 0.034(11) N2 0.29(3) 0.159(17) 0.133(15) 0.011(12) 0.029(16) 0.090(17) C1 0.050(5) 0.076(6) 0.050(5) -0.025(5) -0.001(4) -0.011(5) C2 0.045(4) 0.040(4) 0.037(4) -0.007(3) -0.002(3) -0.007(3) C3 0.066(6) 0.052(5) 0.039(4) -0.001(4) -0.009(4) 0.008(4) C4 0.133(11) 0.044(5) 0.052(6) -0.006(4) -0.020(6) 0.002(6) C5 0.142(11) 0.073(7) 0.040(5) -0.001(5) 0.004(6) -0.071(8) C6 0.097(4) 0.098(4) 0.065(3) -0.014(3) -0.004(3) -0.008(3) C7 0.097(4) 0.098(4) 0.065(3) -0.014(3) -0.004(3) -0.008(3) C8 0.097(4) 0.098(4) 0.065(3) -0.014(3) -0.004(3) -0.008(3) C9 0.097(4) 0.098(4) 0.065(3) -0.014(3) -0.004(3) -0.008(3) C10 0.097(4) 0.098(4) 0.065(3) -0.014(3) -0.004(3) -0.008(3) C11 0.046(5) 0.087(7) 0.066(6) 0.021(5) 0.033(5) 0.016(5) C12 0.049(5) 0.110(8) 0.036(4) 0.000(5) 0.013(4) -0.038(5) C13 0.096(7) 0.046(5) 0.047(5) 0.017(4) 0.033(5) -0.018(5) C14 0.048(5) 0.078(6) 0.031(4) 0.014(4) 0.008(3) -0.007(4) C15 0.076(7) 0.058(5) 0.054(5) -0.014(4) 0.038(5) -0.010(5) C16 0.116(5) 0.133(5) 0.073(4) 0.017(4) 0.045(3) -0.001(4) C17 0.116(5) 0.133(5) 0.073(4) 0.017(4) 0.045(3) -0.001(4) C18 0.116(5) 0.133(5) 0.073(4) 0.017(4) 0.045(3) -0.001(4) C19 0.116(5) 0.133(5) 0.073(4) 0.017(4) 0.045(3) -0.001(4) C20 0.116(5) 0.133(5) 0.073(4) 0.017(4) 0.045(3) -0.001(4) C21 0.061(5) 0.067(6) 0.037(4) -0.014(4) 0.009(4) 0.006(4) C22 0.050(5) 0.085(7) 0.038(4) -0.020(4) 0.015(4) -0.008(5) C23 0.079(6) 0.060(5) 0.023(3) -0.005(3) 0.012(4) -0.004(5) C24 0.059(5) 0.044(4) 0.033(4) -0.014(3) -0.005(3) -0.002(4) C25 0.047(4) 0.038(4) 0.045(4) -0.012(3) 0.002(3) 0.002(3) C26 0.061(6) 0.097(9) 0.095(9) -0.031(7) 0.012(6) 0.029(6) C27 0.096(9) 0.164(14) 0.076(8) -0.051(8) 0.057(7) -0.064(9) C28 0.153(13) 0.087(8) 0.047(6) 0.017(6) -0.007(7) 0.005(8) C29 0.049(5) 0.081(6) 0.049(5) -0.020(5) -0.007(4) 0.006(5) C30 0.085(7) 0.037(4) 0.073(6) -0.022(4) -0.003(5) -0.003(5) C31 0.038(4) 0.048(4) 0.048(4) 0.014(3) -0.010(3) -0.025(3) C32 0.038(4) 0.029(3) 0.054(5) 0.011(3) -0.011(3) -0.012(3) C33 0.043(4) 0.039(4) 0.045(4) 0.004(3) -0.011(3) -0.014(3) C34 0.038(4) 0.037(4) 0.042(4) 0.007(3) -0.010(3) -0.016(3) C35 0.028(3) 0.045(4) 0.060(5) 0.015(4) -0.011(3) -0.014(3) C36 0.051(5) 0.071(6) 0.055(5) 0.017(4) 0.002(4) -0.016(4) C37 0.066(6) 0.034(4) 0.074(6) 0.024(4) -0.020(5) -0.012(4) C38 0.091(8) 0.048(5) 0.060(6) -0.008(4) -0.011(5) 0.002(5) C39 0.059(5) 0.058(5) 0.055(5) 0.011(4) -0.017(4) -0.015(4) C40 0.038(4) 0.062(6) 0.091(7) 0.019(5) -0.008(4) -0.006(4) C41 0.030(3) 0.037(4) 0.041(4) 0.000(3) 0.008(3) 0.000(3) C42 0.033(4) 0.037(4) 0.056(5) 0.010(3) 0.010(3) -0.004(3) C43 0.036(4) 0.033(4) 0.042(4) 0.005(3) 0.011(3) -0.004(3) C44 0.040(4) 0.028(3) 0.045(4) 0.006(3) 0.016(3) 0.003(3) C45 0.046(4) 0.034(3) 0.033(4) 0.003(3) -0.005(3) 0.003(3) C46 0.044(4) 0.045(4) 0.053(5) 0.008(4) -0.001(4) 0.002(3) C47 0.042(5) 0.066(6) 0.070(6) -0.008(5) -0.011(4) 0.005(4) C48 0.064(6) 0.062(6) 0.057(6) -0.006(4) -0.024(5) 0.019(5) C49 0.060(6) 0.080(6) 0.039(4) -0.005(4) -0.005(4) 0.005(5) C50 0.062(5) 0.049(4) 0.031(4) 0.002(3) 0.000(3) -0.002(4) C51 0.032(3) 0.031(3) 0.045(4) -0.001(3) 0.004(3) -0.007(3) C52 0.064(5) 0.046(4) 0.049(5) -0.006(4) -0.002(4) -0.007(4) C53 0.088(8) 0.084(7) 0.049(5) -0.031(5) 0.009(5) 0.001(6) C54 0.069(7) 0.066(6) 0.084(8) -0.031(6) -0.012(6) 0.013(5) C55 0.055(5) 0.051(5) 0.056(5) -0.014(4) 0.000(4) 0.011(4) C56 0.038(4) 0.045(4) 0.053(5) -0.005(4) 0.002(3) 0.000(3) C57 0.033(3) 0.031(3) 0.039(4) 0.000(3) 0.003(3) 0.006(3) C58 0.051(5) 0.060(5) 0.043(4) 0.002(4) -0.002(4) -0.001(4) C59 0.049(5) 0.096(7) 0.042(5) 0.006(5) -0.003(4) 0.018(5) C60 0.067(6) 0.064(6) 0.042(5) -0.008(4) -0.010(4) 0.015(5) C61 0.069(6) 0.055(5) 0.070(7) -0.003(5) -0.029(5) -0.005(5) C62 0.062(5) 0.047(5) 0.046(5) 0.001(4) -0.008(4) 0.002(4) C63 0.035(3) 0.026(3) 0.035(3) -0.001(3) 0.013(3) -0.004(3) C64 0.040(4) 0.035(4) 0.052(5) 0.006(3) 0.010(3) -0.002(3) C65 0.041(4) 0.031(4) 0.057(5) 0.004(3) 0.018(3) 0.008(3) C66 0.058(5) 0.035(4) 0.043(4) -0.003(3) 0.019(4) 0.001(4) C67 0.062(5) 0.038(4) 0.048(5) -0.005(3) -0.005(4) -0.011(4) C68 0.052(5) 0.037(4) 0.042(4) -0.004(3) 0.003(3) -0.001(3) C69 0.046(4) 0.046(4) 0.051(5) 0.011(4) 0.006(4) -0.013(4) C70 0.094(6) 0.132(8) 0.054(4) 0.033(5) -0.012(4) -0.063(6) C71 0.094(6) 0.132(8) 0.054(4) 0.033(5) -0.012(4) -0.063(6) C72 0.037(4) 0.081(6) 0.058(5) 0.027(5) 0.015(4) -0.006(4) C73 0.049(5) 0.054(5) 0.043(4) 0.013(4) 0.016(4) 0.001(4) C74 0.060(6) 0.060(6) 0.067(6) -0.004(5) 0.004(5) 0.000(5) C75 0.103(10) 0.076(7) 0.081(8) -0.015(6) 0.016(7) 0.018(7) C76 0.108(10) 0.060(6) 0.073(7) -0.001(5) 0.027(7) 0.027(6) C77 0.069(7) 0.081(7) 0.080(7) 0.006(6) 0.031(6) 0.025(6) C78 0.061(6) 0.068(6) 0.064(6) 0.006(5) 0.020(5) 0.019(5) C79 0.036(4) 0.046(4) 0.035(4) 0.010(3) 0.008(3) 0.004(3) C80 0.052(5) 0.058(5) 0.037(4) 0.003(4) 0.001(3) 0.002(4) C81 0.061(6) 0.079(6) 0.043(5) 0.007(4) 0.005(4) 0.012(5) C82 0.049(5) 0.114(9) 0.037(4) 0.018(5) 0.015(4) 0.030(5) C83 0.052(5) 0.104(8) 0.068(6) 0.054(6) 0.014(5) 0.008(5) C84 0.049(5) 0.074(6) 0.056(5) 0.036(5) 0.001(4) -0.009(4) C85 0.071(6) 0.034(4) 0.054(5) 0.006(3) 0.019(4) 0.000(4) C86 0.065(6) 0.041(4) 0.060(5) 0.008(4) -0.004(4) 0.012(4) C87 0.075(7) 0.044(5) 0.084(7) 0.012(5) 0.000(6) 0.010(5) C88 0.105(9) 0.043(5) 0.110(10) -0.010(6) 0.032(8) 0.012(6) C89 0.154(13) 0.055(6) 0.080(8) -0.022(6) 0.042(8) 0.012(7) C90 0.116(9) 0.053(5) 0.053(6) 0.000(4) 0.016(6) 0.002(6) C91 0.052(5) 0.040(4) 0.040(4) 0.013(3) -0.004(3) -0.014(3) C92 0.130(10) 0.072(7) 0.038(5) -0.007(4) 0.020(6) -0.033(7) C93 0.198(17) 0.087(9) 0.045(6) -0.007(6) 0.010(8) -0.078(10) C94 0.157(15) 0.135(13) 0.071(9) 0.057(9) -0.060(10) -0.091(12) C95 0.072(8) 0.086(9) 0.158(14) 0.057(9) -0.054(9) -0.026(7) C96 0.043(5) 0.051(5) 0.113(9) 0.012(5) -0.016(5) -0.009(4) C97 0.175(18) 0.126(15) 0.20(2) -0.065(14) 0.097(17) -0.073(14) C98 0.096(9) 0.100(9) 0.064(7) -0.026(7) 0.019(6) 0.004(7) C99 0.147(16) 0.153(16) 0.110(13) -0.015(12) 0.033(12) -0.016(13) C100 0.131(14) 0.101(11) 0.099(12) -0.015(9) 0.007(10) -0.009(10) Cl1 0.0329(9) 0.0554(12) 0.0788(16) 0.0081(11) 0.0009(9) 0.0057(9) O1 0.088(7) 0.069(5) 0.229(13) -0.005(7) -0.030(7) 0.033(5) O2 0.064(5) 0.153(9) 0.120(8) 0.033(7) 0.019(5) -0.035(5) O3 0.088(6) 0.134(8) 0.073(5) 0.024(5) -0.001(4) -0.028(5) O4 0.037(3) 0.068(4) 0.097(5) 0.009(4) -0.012(3) 0.003(3) Cl2 0.0545(12) 0.0686(14) 0.0436(11) -0.0057(9) 0.0088(9) -0.0107(10) O5 0.097(7) 0.170(10) 0.115(8) 0.024(7) 0.027(6) 0.055(7) O6 0.074(5) 0.123(7) 0.077(5) -0.024(5) 0.006(4) -0.041(5) O7 0.088(6) 0.142(8) 0.043(4) -0.016(4) 0.008(4) 0.021(5) O8 0.189(11) 0.094(6) 0.064(5) -0.002(4) 0.021(6) -0.060(7) Cl3 0.0975(19) 0.0642(14) 0.158(3) -0.0372(15) 0.0736(19) -0.0261(12) O9 0.0975(19) 0.0642(14) 0.158(3) -0.0372(15) 0.0736(19) -0.0261(12) O10 0.0975(19) 0.0642(14) 0.158(3) -0.0372(15) 0.0736(19) -0.0261(12) O11 0.0975(19) 0.0642(14) 0.158(3) -0.0372(15) 0.0736(19) -0.0261(12) O12 0.0975(19) 0.0642(14) 0.158(3) -0.0372(15) 0.0736(19) -0.0261(12) Cl4 0.080(2) 0.102(3) 0.094(3) -0.022(2) 0.0229(18) 0.020(2) O13 0.080(2) 0.102(3) 0.094(3) -0.022(2) 0.0229(18) 0.020(2) O14 0.080(2) 0.102(3) 0.094(3) -0.022(2) 0.0229(18) 0.020(2) O15 0.080(2) 0.102(3) 0.094(3) -0.022(2) 0.0229(18) 0.020(2) O16 0.080(2) 0.102(3) 0.094(3) -0.022(2) 0.0229(18) 0.020(2) Cl4A 0.094(6) 0.123(6) 0.043(4) 0.046(4) -0.026(4) -0.035(5) O14A 0.094(6) 0.123(6) 0.043(4) 0.046(4) -0.026(4) -0.035(5) O13A 0.094(6) 0.123(6) 0.043(4) 0.046(4) -0.026(4) -0.035(5) O15A 0.094(6) 0.123(6) 0.043(4) 0.046(4) -0.026(4) -0.035(5) O16A 0.094(6) 0.123(6) 0.043(4) 0.046(4) -0.026(4) -0.035(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 S1 2.2249(19) . ? Mo1 S3 2.333(2) . ? Mo1 S4 2.3421(19) . ? Mo1 C5 2.354(5) . ? Mo1 C1 2.362(4) . ? Mo1 C4 2.387(5) . ? Mo1 C2 2.399(4) . ? Mo1 C3 2.415(4) . ? Mo1 Cu1 2.7718(12) . ? Mo1 Cu2 2.7868(14) . ? Mo1 Mo2 2.8670(10) . ? Mo2 S2 2.2327(18) . ? Mo2 S3 2.3246(19) . ? Mo2 C11 2.328(4) . ? Mo2 C12 2.333(4) . ? Mo2 S4 2.339(2) . ? Mo2 C13 2.354(4) . ? Mo2 C14 2.362(4) . ? Mo2 C15 2.394(4) . ? Mo2 Cu1 2.7554(11) . ? Mo2 Cu2 2.7671(13) . ? Mo3 S5 2.2349(18) . ? Mo3 S7 2.3327(19) . ? Mo3 S8 2.3331(19) . ? Mo3 C22 2.369(4) . ? Mo3 C23 2.377(4) . ? Mo3 C21 2.401(4) . ? Mo3 C24 2.413(3) . ? Mo3 C25 2.428(3) . ? Mo3 Cu4 2.7534(12) . ? Mo3 Cu3 2.7684(11) . ? Mo3 Mo4 2.8682(10) . ? Mo4 S6 2.231(2) . ? Mo4 S7 2.3240(18) . ? Mo4 S8 2.3391(19) . ? Mo4 C31 2.371(3) . ? Mo4 C35 2.393(3) . ? Mo4 C32 2.396(3) . ? Mo4 C34 2.432(3) . ? Mo4 C33 2.434(3) . ? Mo4 Cu3 2.7693(11) . ? Mo4 Cu4 2.7919(11) . ? Cu1 P1 2.2116(19) . ? Cu1 S3 2.2463(19) . ? Cu1 S2 2.346(2) . ? Cu1 S1 2.391(2) . ? Cu1 Cu2 2.8938(14) . ? Cu2 P3 2.223(2) . ? Cu2 S4 2.274(2) . ? Cu2 S2 2.365(2) . ? Cu2 S1 2.378(2) . ? Cu3 P2 2.2179(19) . ? Cu3 S7 2.2553(19) . ? Cu3 S6 2.363(2) . ? Cu3 S5 2.3784(19) . ? Cu3 Cu4 2.9883(13) . ? Cu4 P4 2.2117(19) . ? Cu4 S8 2.259(2) . ? Cu4 S5 2.341(2) . ? Cu4 S6 2.404(2) . ? P1 C51 1.815(4) . ? P1 C41 1.821(7) . ? P1 C45 1.824(4) . ? P2 C44 1.817(7) . ? P2 C63 1.825(3) . ? P2 C57 1.826(4) . ? P3 C69 1.809(8) . ? P3 C73 1.809(5) . ? P3 C79 1.825(4) . ? P4 C85 1.806(4) . ? P4 C91 1.809(5) . ? P4 C72 1.825(8) . ? N1 C98 1.082(15) . ? N2 C100 1.19(2) . ? C1 C2 1.404(3) . ? C1 C5 1.405(3) . ? C1 C6 1.493(3) . ? C2 C3 1.405(3) . ? C2 C7 1.493(3) . ? C3 C4 1.405(3) . ? C3 C8 1.493(3) . ? C4 C5 1.405(3) . ? C4 C9 1.493(3) . ? C5 C10 1.525(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C15 1.371(2) . ? C11 C12 1.422(2) . ? C11 C16 1.504(2) . ? C12 C13 1.385(2) . ? C12 C17 1.497(2) . ? C13 C14 1.421(2) . ? C13 C18 1.483(2) . ? C14 C15 1.388(2) . ? C14 C19 1.486(2) . ? C15 C20 1.485(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.421(2) . ? C21 C25 1.421(2) . ? C21 C26 1.511(2) . ? C22 C23 1.421(2) . ? C22 C27 1.511(2) . ? C23 C24 1.421(2) . ? C23 C28 1.511(2) . ? C24 C25 1.421(2) . ? C24 C29 1.511(2) . ? C25 C30 1.511(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C35 1.4140(19) . ? C31 C32 1.4141(19) . ? C31 C36 1.503(2) . ? C32 C33 1.4139(19) . ? C32 C37 1.503(2) . ? C33 C34 1.4142(19) . ? C33 C38 1.503(2) . ? C34 C35 1.4141(19) . ? C34 C39 1.503(2) . ? C35 C40 1.503(2) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.512(10) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.544(10) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.524(9) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C46 C47 1.3900 . ? C46 H46 0.9500 . ? C47 C48 1.3900 . ? C47 H47 0.9500 . ? C48 C49 1.3900 . ? C48 H48 0.9500 . ? C49 C50 1.3900 . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.3900 . ? C57 C62 1.3900 . ? C58 C59 1.3900 . ? C58 H58 0.9500 . ? C59 C60 1.3900 . ? C59 H59 0.9500 . ? C60 C61 1.3900 . ? C60 H60 0.9500 . ? C61 C62 1.3900 . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.3900 . ? C63 C68 1.3900 . ? C64 C65 1.3900 . ? C64 H64 0.9500 . ? C65 C66 1.3900 . ? C65 H65 0.9500 . ? C66 C67 1.3900 . ? C66 H66 0.9500 . ? C67 C68 1.3900 . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.516(13) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.326(15) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.595(14) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.3900 . ? C73 C78 1.3900 . ? C74 C75 1.3900 . ? C74 H74 0.9500 . ? C75 C76 1.3900 . ? C75 H75 0.9500 . ? C76 C77 1.3900 . ? C76 H76 0.9500 . ? C77 C78 1.3900 . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C80 1.3900 . ? C79 C84 1.3900 . ? C80 C81 1.3900 . ? C80 H80 0.9500 . ? C81 C82 1.3900 . ? C81 H81 0.9500 . ? C82 C83 1.3900 . ? C82 H82 0.9500 . ? C83 C84 1.3900 . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 C86 1.3900 . ? C85 C90 1.3900 . ? C86 C87 1.3900 . ? C86 H86 0.9500 . ? C87 C88 1.3900 . ? C87 H87 0.9500 . ? C88 C89 1.3900 . ? C88 H88 0.9500 . ? C89 C90 1.3900 . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C92 C93 1.3900 . ? C92 H92 0.9500 . ? C93 C94 1.3900 . ? C93 H93 0.9500 . ? C94 C95 1.3900 . ? C94 H94 0.9500 . ? C95 C96 1.3900 . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C97 C98 1.429(19) . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C99 C100 1.42(2) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? Cl1 O1 1.406(9) . ? Cl1 O3 1.412(9) . ? Cl1 O4 1.412(6) . ? Cl1 O2 1.412(8) . ? Cl2 O8 1.380(9) . ? Cl2 O6 1.413(8) . ? Cl2 O5 1.420(10) . ? Cl2 O7 1.429(7) . ? Cl3 O11 1.391(8) . ? Cl3 O12 1.392(8) . ? Cl3 O10 1.404(11) . ? Cl3 O9 1.419(11) . ? Cl4 O14 1.363(9) . ? Cl4 O16 1.399(9) . ? Cl4 O15 1.424(9) . ? Cl4 O13 1.431(9) . ? Cl4A O14A 1.298(15) . ? Cl4A O16A 1.348(15) . ? Cl4A O15A 1.401(14) . ? Cl4A O13A 1.426(13) . ? 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 S1 Mo1 S3 105.52(7) . . ? S1 Mo1 S4 105.13(7) . . ? S3 Mo1 S4 101.38(7) . . ? S1 Mo1 Cu1 55.89(6) . . ? S3 Mo1 Cu1 51.34(5) . . ? S4 Mo1 Cu1 100.75(5) . . ? S1 Mo1 Cu2 55.28(5) . . ? S3 Mo1 Cu2 100.42(5) . . ? S4 Mo1 Cu2 51.75(5) . . ? Cu1 Mo1 Cu2 62.74(3) . . ? S1 Mo1 Mo2 100.86(6) . . ? S3 Mo1 Mo2 51.87(5) . . ? S4 Mo1 Mo2 52.18(5) . . ? Cu1 Mo1 Mo2 58.47(2) . . ? Cu2 Mo1 Mo2 58.59(3) . . ? S2 Mo2 S3 104.81(7) . . ? S2 Mo2 S4 105.68(7) . . ? S3 Mo2 S4 101.73(7) . . ? C11 Mo2 S4 140.33(12) . . ? C12 Mo2 S4 105.50(12) . . ? S2 Mo2 Cu1 54.92(5) . . ? S3 Mo2 Cu1 51.64(5) . . ? C11 Mo2 Cu1 114.72(11) . . ? C12 Mo2 Cu1 137.53(11) . . ? S4 Mo2 Cu1 101.31(5) . . ? C13 Mo2 Cu1 171.46(11) . . ? C14 Mo2 Cu1 145.08(11) . . ? C15 Mo2 Cu1 118.52(11) . . ? S2 Mo2 Cu2 55.22(6) . . ? S3 Mo2 Cu2 101.21(6) . . ? S4 Mo2 Cu2 52.07(5) . . ? Cu1 Mo2 Cu2 63.20(3) . . ? S2 Mo2 Mo1 100.73(6) . . ? S3 Mo2 Mo1 52.15(5) . . ? S4 Mo2 Mo1 52.28(5) . . ? Cu1 Mo2 Mo1 59.04(3) . . ? Cu2 Mo2 Mo1 59.26(4) . . ? S5 Mo3 S7 105.92(6) . . ? S5 Mo3 S8 105.48(7) . . ? S7 Mo3 S8 100.68(6) . . ? S5 Mo3 Cu4 54.78(5) . . ? S7 Mo3 Cu4 102.55(5) . . ? S8 Mo3 Cu4 51.94(5) . . ? S5 Mo3 Cu3 55.54(5) . . ? S7 Mo3 Cu3 51.62(5) . . ? S8 Mo3 Cu3 102.23(5) . . ? Cu4 Mo3 Cu3 65.53(3) . . ? S5 Mo3 Mo4 99.66(5) . . ? S7 Mo3 Mo4 51.85(4) . . ? S8 Mo3 Mo4 52.22(5) . . ? Cu4 Mo3 Mo4 59.51(3) . . ? Cu3 Mo3 Mo4 58.82(3) . . ? S6 Mo4 S7 105.46(7) . . ? S6 Mo4 S8 105.78(7) . . ? S7 Mo4 S8 100.76(6) . . ? S6 Mo4 Cu3 55.15(5) . . ? S7 Mo4 Cu3 51.67(5) . . ? S8 Mo4 Cu3 102.05(5) . . ? C31 Mo4 Cu3 140.62(8) . . ? C35 Mo4 Cu3 172.08(9) . . ? C32 Mo4 Cu3 115.40(9) . . ? C34 Mo4 Cu3 141.31(9) . . ? C33 Mo4 Cu3 116.04(9) . . ? S6 Mo4 Cu4 55.85(5) . . ? S7 Mo4 Cu4 101.64(5) . . ? S8 Mo4 Cu4 51.33(5) . . ? Cu3 Mo4 Cu4 65.00(3) . . ? S6 Mo4 Mo3 99.52(5) . . ? S7 Mo4 Mo3 52.12(5) . . ? S8 Mo4 Mo3 52.03(5) . . ? Cu3 Mo4 Mo3 58.79(3) . . ? Cu4 Mo4 Mo3 58.20(3) . . ? P1 Cu1 S3 119.46(8) . . ? P1 Cu1 S2 120.73(7) . . ? S3 Cu1 S2 103.66(7) . . ? P1 Cu1 S1 104.63(7) . . ? S3 Cu1 S1 102.96(8) . . ? S2 Cu1 S1 102.79(7) . . ? P1 Cu1 Mo2 155.46(6) . . ? S3 Cu1 Mo2 54.24(5) . . ? S2 Cu1 Mo2 51.14(5) . . ? S1 Cu1 Mo2 99.89(6) . . ? P1 Cu1 Mo1 136.89(6) . . ? S3 Cu1 Mo1 54.20(5) . . ? S2 Cu1 Mo1 100.63(5) . . ? S1 Cu1 Mo1 50.40(5) . . ? Mo2 Cu1 Mo1 62.49(3) . . ? P1 Cu1 Cu2 139.57(6) . . ? S3 Cu1 Cu2 99.48(6) . . ? S2 Cu1 Cu2 52.40(6) . . ? S1 Cu1 Cu2 52.43(5) . . ? Mo2 Cu1 Cu2 58.60(3) . . ? Mo1 Cu1 Cu2 58.88(3) . . ? P3 Cu2 S4 125.75(8) . . ? P3 Cu2 S2 107.72(8) . . ? S4 Cu2 S2 103.52(8) . . ? P3 Cu2 S1 112.25(8) . . ? S4 Cu2 S1 102.46(8) . . ? S2 Cu2 S1 102.63(7) . . ? P3 Cu2 Mo2 145.50(7) . . ? S4 Cu2 Mo2 54.23(5) . . ? S2 Cu2 Mo2 50.84(5) . . ? S1 Cu2 Mo2 99.90(6) . . ? P3 Cu2 Mo1 150.77(7) . . ? S4 Cu2 Mo1 53.99(5) . . ? S2 Cu2 Mo1 99.74(5) . . ? S1 Cu2 Mo1 50.28(5) . . ? Mo2 Cu2 Mo1 62.16(3) . . ? P3 Cu2 Cu1 135.19(7) . . ? S4 Cu2 Cu1 98.94(6) . . ? S2 Cu2 Cu1 51.81(5) . . ? S1 Cu2 Cu1 52.85(6) . . ? Mo2 Cu2 Cu1 58.20(3) . . ? Mo1 Cu2 Cu1 58.38(3) . . ? P2 Cu3 S7 112.48(7) . . ? P2 Cu3 S6 122.64(8) . . ? S7 Cu3 S6 103.41(7) . . ? P2 Cu3 S5 113.01(7) . . ? S7 Cu3 S5 103.77(7) . . ? S6 Cu3 S5 99.24(7) . . ? P2 Cu3 Mo3 138.12(6) . . ? S7 Cu3 Mo3 54.18(5) . . ? S6 Cu3 Mo3 99.11(6) . . ? S5 Cu3 Mo3 50.78(5) . . ? P2 Cu3 Mo4 147.93(6) . . ? S7 Cu3 Mo4 53.93(5) . . ? S6 Cu3 Mo4 50.78(5) . . ? S5 Cu3 Mo4 98.93(5) . . ? Mo3 Cu3 Mo4 62.39(3) . . ? P2 Cu3 Cu4 149.13(6) . . ? S7 Cu3 Cu4 97.66(5) . . ? S6 Cu3 Cu4 51.79(5) . . ? S5 Cu3 Cu4 50.15(5) . . ? Mo3 Cu3 Cu4 56.99(3) . . ? Mo4 Cu3 Cu4 57.86(3) . . ? P4 Cu4 S8 116.38(8) . . ? P4 Cu4 S5 122.59(7) . . ? S8 Cu4 S5 104.45(7) . . ? P4 Cu4 S6 108.50(8) . . ? S8 Cu4 S6 102.79(7) . . ? S5 Cu4 S6 99.15(7) . . ? P4 Cu4 Mo3 152.97(7) . . ? S8 Cu4 Mo3 54.40(5) . . ? S5 Cu4 Mo3 51.27(5) . . ? S6 Cu4 Mo3 98.52(5) . . ? P4 Cu4 Mo4 137.06(6) . . ? S8 Cu4 Mo4 53.93(5) . . ? S5 Cu4 Mo4 99.24(5) . . ? S6 Cu4 Mo4 50.18(5) . . ? Mo3 Cu4 Mo4 62.29(3) . . ? P4 Cu4 Cu3 144.46(7) . . ? S8 Cu4 Cu3 97.70(5) . . ? S5 Cu4 Cu3 51.27(5) . . ? S6 Cu4 Cu3 50.58(5) . . ? Mo3 Cu4 Cu3 57.48(3) . . ? Mo4 Cu4 Cu3 57.13(3) . . ? Mo1 S1 Cu2 74.44(6) . . ? Mo1 S1 Cu1 73.71(6) . . ? Cu2 S1 Cu1 74.72(6) . . ? Mo2 S2 Cu1 73.94(6) . . ? Mo2 S2 Cu2 73.94(6) . . ? Cu1 S2 Cu2 75.79(6) . . ? Cu1 S3 Mo2 74.12(6) . . ? Cu1 S3 Mo1 74.47(6) . . ? Mo2 S3 Mo1 75.98(6) . . ? Cu2 S4 Mo2 73.71(6) . . ? Cu2 S4 Mo1 74.26(6) . . ? Mo2 S4 Mo1 75.53(6) . . ? Mo3 S5 Cu4 73.95(6) . . ? Mo3 S5 Cu3 73.68(6) . . ? Cu4 S5 Cu3 78.57(6) . . ? Mo4 S6 Cu3 74.07(6) . . ? Mo4 S6 Cu4 73.97(6) . . ? Cu3 S6 Cu4 77.63(6) . . ? Cu3 S7 Mo4 74.40(6) . . ? Cu3 S7 Mo3 74.20(6) . . ? Mo4 S7 Mo3 76.04(5) . . ? Cu4 S8 Mo3 73.66(6) . . ? Cu4 S8 Mo4 74.75(6) . . ? Mo3 S8 Mo4 75.74(5) . . ? C51 P1 C41 107.5(3) . . ? C51 P1 C45 105.5(2) . . ? C41 P1 C45 106.1(3) . . ? C51 P1 Cu1 114.64(18) . . ? C41 P1 Cu1 112.5(2) . . ? C45 P1 Cu1 109.99(18) . . ? C44 P2 C63 102.6(3) . . ? C44 P2 C57 106.6(3) . . ? C63 P2 C57 106.0(2) . . ? C44 P2 Cu3 116.7(2) . . ? C63 P2 Cu3 113.74(16) . . ? C57 P2 Cu3 110.38(19) . . ? C69 P3 C73 103.6(4) . . ? C69 P3 C79 106.2(3) . . ? C73 P3 C79 104.7(3) . . ? C69 P3 Cu2 115.5(3) . . ? C73 P3 Cu2 112.9(2) . . ? C79 P3 Cu2 112.99(19) . . ? C85 P4 C91 104.4(3) . . ? C85 P4 C72 105.6(4) . . ? C91 P4 C72 105.8(4) . . ? C85 P4 Cu4 115.5(2) . . ? C91 P4 Cu4 109.6(2) . . ? C72 P4 Cu4 115.1(3) . . ? C2 C1 C5 108.0 . . ? C2 C1 C6 126.0 . . ? C5 C1 C6 126.0 . . ? C3 C2 C1 108.0 . . ? C3 C2 C7 126.0 . . ? C1 C2 C7 126.0 . . ? C2 C3 C4 108.0 . . ? C2 C3 C8 126.0 . . ? C4 C3 C8 126.0 . . ? C5 C4 C3 108.0 . . ? C5 C4 C9 126.0 . . ? C3 C4 C9 126.0 . . ? C4 C5 C1 108.0 . . ? C4 C5 C10 124.2(5) . . ? C1 C5 C10 127.7(5) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C11 C12 109.6 . . ? C15 C11 C16 126.0 . . ? C12 C11 C16 123.9 . . ? C13 C12 C11 105.9 . . ? C13 C12 C17 126.9 . . ? C11 C12 C17 126.8 . . ? C12 C13 C14 108.9 . . ? C12 C13 C18 127.5 . . ? C14 C13 C18 123.4 . . ? C15 C14 C13 107.3 . . ? C15 C14 C19 124.7 . . ? C13 C14 C19 127.5 . . ? C11 C15 C14 108.2 . . ? C11 C15 C20 129.0 . . ? C14 C15 C20 122.7 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C25 108.0 . . ? C22 C21 C26 126.0 . . ? C25 C21 C26 126.0 . . ? C21 C22 C23 108.0 . . ? C21 C22 C27 126.0 . . ? C23 C22 C27 126.0 . . ? C24 C23 C22 108.0 . . ? C24 C23 C28 126.0 . . ? C22 C23 C28 126.0 . . ? C25 C24 C23 108.0 . . ? C25 C24 C29 126.0 . . ? C23 C24 C29 126.0 . . ? C24 C25 C21 108.0 . . ? C24 C25 C30 126.0 . . ? C21 C25 C30 126.0 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C35 C31 C32 108.0 . . ? C35 C31 C36 126.0 . . ? C32 C31 C36 126.0 . . ? C33 C32 C31 108.0 . . ? C33 C32 C37 126.0 . . ? C31 C32 C37 126.0 . . ? C32 C33 C34 108.0 . . ? C32 C33 C38 126.0 . . ? C34 C33 C38 126.0 . . ? C35 C34 C33 108.0 . . ? C35 C34 C39 126.0 . . ? C33 C34 C39 126.0 . . ? C31 C35 C34 108.0 . . ? C31 C35 C40 126.0 . . ? C34 C35 C40 126.0 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 P1 115.7(5) . . ? C42 C41 H41A 108.4 . . ? P1 C41 H41A 108.4 . . ? C42 C41 H41B 108.4 . . ? P1 C41 H41B 108.4 . . ? H41A C41 H41B 107.4 . . ? C41 C42 C43 113.2(6) . . ? C41 C42 H42A 108.9 . . ? C43 C42 H42A 108.9 . . ? C41 C42 H42B 108.9 . . ? C43 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? C44 C43 C42 108.1(6) . . ? C44 C43 H43A 110.1 . . ? C42 C43 H43A 110.1 . . ? C44 C43 H43B 110.1 . . ? C42 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? C43 C44 P2 117.1(5) . . ? C43 C44 H44A 108.0 . . ? P2 C44 H44A 108.0 . . ? C43 C44 H44B 108.0 . . ? P2 C44 H44B 108.0 . . ? H44A C44 H44B 107.3 . . ? C46 C45 C50 120.0 . . ? C46 C45 P1 117.7(3) . . ? C50 C45 P1 122.0(3) . . ? C47 C46 C45 120.0 . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C48 C47 C46 120.0 . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 120.0 . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C45 120.0 . . ? C49 C50 H50 120.0 . . ? C45 C50 H50 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 P1 118.8(3) . . ? C56 C51 P1 121.2(3) . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C58 C57 C62 120.0 . . ? C58 C57 P2 118.4(3) . . ? C62 C57 P2 121.4(3) . . ? C59 C58 C57 120.0 . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C60 C59 C58 120.0 . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C61 C60 C59 120.0 . . ? C61 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C60 C61 C62 120.0 . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C61 C62 C57 120.0 . . ? C61 C62 H62 120.0 . . ? C57 C62 H62 120.0 . . ? C64 C63 C68 120.0 . . ? C64 C63 P2 121.6(2) . . ? C68 C63 P2 118.2(2) . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C67 C66 C65 120.0 . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C66 C67 C68 120.0 . . ? C66 C67 H67 120.0 . . ? C68 C67 H67 120.0 . . ? C67 C68 C63 120.0 . . ? C67 C68 H68 120.0 . . ? C63 C68 H68 120.0 . . ? C70 C69 P3 114.5(7) . . ? C70 C69 H69A 108.6 . . ? P3 C69 H69A 108.6 . . ? C70 C69 H69B 108.6 . . ? P3 C69 H69B 108.6 . . ? H69A C69 H69B 107.6 . . ? C71 C70 C69 119.7(10) . . ? C71 C70 H70A 107.4 . . ? C69 C70 H70A 107.4 . . ? C71 C70 H70B 107.4 . . ? C69 C70 H70B 107.4 . . ? H70A C70 H70B 106.9 . . ? C70 C71 C72 120.4(11) . . ? C70 C71 H71A 107.2 . . ? C72 C71 H71A 107.2 . . ? C70 C71 H71B 107.2 . . ? C72 C71 H71B 107.2 . . ? H71A C71 H71B 106.9 . . ? C71 C72 P4 109.1(7) . . ? C71 C72 H72A 109.9 . . ? P4 C72 H72A 109.9 . . ? C71 C72 H72B 109.9 . . ? P4 C72 H72B 109.9 . . ? H72A C72 H72B 108.3 . . ? C74 C73 C78 120.0 . . ? C74 C73 P3 118.1(3) . . ? C78 C73 P3 121.9(3) . . ? C75 C74 C73 120.0 . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C76 120.0 . . ? C74 C75 H75 120.0 . . ? C76 C75 H75 120.0 . . ? C77 C76 C75 120.0 . . ? C77 C76 H76 120.0 . . ? C75 C76 H76 120.0 . . ? C76 C77 C78 120.0 . . ? C76 C77 H77 120.0 . . ? C78 C77 H77 120.0 . . ? C77 C78 C73 120.0 . . ? C77 C78 H78 120.0 . . ? C73 C78 H78 120.0 . . ? C80 C79 C84 120.0 . . ? C80 C79 P3 122.3(3) . . ? C84 C79 P3 117.7(3) . . ? C79 C80 C81 120.0 . . ? C79 C80 H80 120.0 . . ? C81 C80 H80 120.0 . . ? C80 C81 C82 120.0 . . ? C80 C81 H81 120.0 . . ? C82 C81 H81 120.0 . . ? C83 C82 C81 120.0 . . ? C83 C82 H82 120.0 . . ? C81 C82 H82 120.0 . . ? C82 C83 C84 120.0 . . ? C82 C83 H83 120.0 . . ? C84 C83 H83 120.0 . . ? C83 C84 C79 120.0 . . ? C83 C84 H84 120.0 . . ? C79 C84 H84 120.0 . . ? C86 C85 C90 120.0 . . ? C86 C85 P4 120.8(3) . . ? C90 C85 P4 119.1(3) . . ? C85 C86 C87 120.0 . . ? C85 C86 H86 120.0 . . ? C87 C86 H86 120.0 . . ? C88 C87 C86 120.0 . . ? C88 C87 H87 120.0 . . ? C86 C87 H87 120.0 . . ? C87 C88 C89 120.0 . . ? C87 C88 H88 120.0 . . ? C89 C88 H88 120.0 . . ? C90 C89 C88 120.0 . . ? C90 C89 H89 120.0 . . ? C88 C89 H89 120.0 . . ? C89 C90 C85 120.0 . . ? C89 C90 H90 120.0 . . ? C85 C90 H90 120.0 . . ? C92 C91 C96 120.0 . . ? C92 C91 P4 120.7(4) . . ? C96 C91 P4 119.2(4) . . ? C91 C92 C93 120.0 . . ? C91 C92 H92 120.0 . . ? C93 C92 H92 120.0 . . ? C94 C93 C92 120.0 . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C93 C94 C95 120.0 . . ? C93 C94 H94 120.0 . . ? C95 C94 H94 120.0 . . ? C94 C95 C96 120.0 . . ? C94 C95 H95 120.0 . . ? C96 C95 H95 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 H96 120.0 . . ? C91 C96 H96 120.0 . . ? C98 C97 H97A 109.5 . . ? C98 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C98 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? N1 C98 C97 176(2) . . ? C100 C99 H99A 109.5 . . ? C100 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C100 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? N2 C100 C99 174(2) . . ? O1 Cl1 O3 104.7(7) . . ? O1 Cl1 O4 111.0(5) . . ? O3 Cl1 O4 109.3(5) . . ? O1 Cl1 O2 113.3(7) . . ? O3 Cl1 O2 107.7(6) . . ? O4 Cl1 O2 110.5(5) . . ? O8 Cl2 O6 109.5(6) . . ? O8 Cl2 O5 108.2(7) . . ? O6 Cl2 O5 109.3(7) . . ? O8 Cl2 O7 109.2(6) . . ? O6 Cl2 O7 111.8(5) . . ? O5 Cl2 O7 108.9(6) . . ? O11 Cl3 O12 110.7(5) . . ? O11 Cl3 O10 112.0(6) . . ? O12 Cl3 O10 111.1(6) . . ? O11 Cl3 O9 107.2(6) . . ? O12 Cl3 O9 104.4(6) . . ? O10 Cl3 O9 111.2(6) . . ? O14 Cl4 O16 112.9(5) . . ? O14 Cl4 O15 110.7(6) . . ? O16 Cl4 O15 108.5(6) . . ? O14 Cl4 O13 110.2(6) . . ? O16 Cl4 O13 107.5(6) . . ? O15 Cl4 O13 106.7(5) . . ? O14A Cl4A O16A 115.3(9) . . ? O14A Cl4A O15A 111.7(10) . . ? O16A Cl4A O15A 107.8(9) . . ? O14A Cl4A O13A 110.0(9) . . ? O16A Cl4A O13A 107.5(9) . . ? O15A Cl4A O13A 103.9(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.820 _refine_diff_density_min -2.799 _refine_diff_density_rms 0.166 #===END