# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_general _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- JPLangCIF.cif' _audit_creation_date 2011-04-10 _audit_creation_method 'SHELXL 97' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Jian-Ping Lang' _publ_contact_author_email jplang@suda.edu.cn _publ_contact_author_fax 86-512-65880089 _publ_contact_author_phone 86-512-65882865 _publ_contact_author_address ; College of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou 215123, Jiangsu, P. R. China ; _publ_requested_category FM _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Zhi-Gang Ren' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; 'Sha Sun' '' '' 'Ming Dai' '' '' 'Hui-Fang Wang' '' '' 'Chun-Ning Lu' '' '' 'Jian-Ping Lang' '' '' 'Zhenrong Sun' '' '' _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2001). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.00. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W., CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data_3^.^4MeCN^.^2CH~2~Cl~2~ _database_code_depnum_ccdc_archive 'CCDC 783842' #TrackingRef '- JPLangCIF.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C98 H112 Cu4 Mo4 N2 P4 S8, 4(Cl O4), 4(C2 H3 N), 2(C H2 Cl2)' _chemical_formula_sum 'C108 H128 Cl8 Cu4 Mo4 N6 O16 P4 S8' _chemical_formula_weight 3068.04 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.346(3) _cell_length_b 15.398(3) _cell_length_c 16.355(3) _cell_angle_alpha 92.10(3) _cell_angle_beta 100.34(3) _cell_angle_gamma 104.51(3) _cell_volume 3189.2(11) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9538 _cell_measurement_theta_min 3.0127 _cell_measurement_theta_max 27.4932 _exptl_crystal_description prism _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.79 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1554 _exptl_absorpt_coefficient_mu 1.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3953 _exptl_absorpt_correction_T_max 0.5826 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 21323 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11507 _reflns_number_gt 9236 _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^)+(0.0916P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11507 _refine_ls_number_parameters 699 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1583 _refine_ls_wR_factor_gt 0.1494 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 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 0.52462(3) 0.26228(3) 0.26387(2) 0.02694(13) Uani 1 1 d . A . Mo2 Mo 0.74747(3) 0.29009(3) 0.26471(2) 0.02901(13) Uani 1 1 d . A . Cu1 Cu 0.59944(5) 0.24894(4) 0.11395(3) 0.03054(16) Uani 1 1 d . . . Cu2 Cu 0.61237(5) 0.11392(4) 0.24745(3) 0.03012(16) Uani 1 1 d . . . S1 S 0.46056(9) 0.14659(8) 0.16400(7) 0.0282(3) Uani 1 1 d . A . S2 S 0.73961(9) 0.18168(8) 0.16590(7) 0.0308(3) Uani 1 1 d . A . S3 S 0.63411(10) 0.37562(8) 0.20356(7) 0.0308(3) Uani 1 1 d . A . S4 S 0.65021(10) 0.21746(8) 0.36123(7) 0.0314(3) Uani 1 1 d . A . P1 P 0.59031(10) 0.28455(8) -0.01934(7) 0.0282(3) Uani 1 1 d . A . P2 P 0.42025(10) 0.03215(8) -0.27681(7) 0.0268(3) Uani 1 1 d . . . N1 N 0.5269(3) 0.1248(3) -0.1234(2) 0.0293(9) Uani 1 1 d . A . C1 C 0.3942(5) 0.3437(5) 0.2531(4) 0.0535(16) Uani 1 1 d . . . C2 C 0.3421(5) 0.2537(5) 0.2602(4) 0.0614(19) Uani 1 1 d . A . C3 C 0.3844(4) 0.2282(4) 0.3396(4) 0.0472(15) Uani 1 1 d . . . C4 C 0.4596(4) 0.3058(4) 0.3825(3) 0.0381(12) Uani 1 1 d . A . C5 C 0.4654(5) 0.3761(4) 0.3294(4) 0.0447(14) Uani 1 1 d . A . C6 C 0.3730(8) 0.4031(7) 0.1831(5) 0.105(4) Uani 1 1 d . A . H6A H 0.3428 0.3654 0.1306 0.127 Uiso 1 1 calc R . . H6B H 0.4394 0.4455 0.1779 0.127 Uiso 1 1 calc R . . H6C H 0.3233 0.4365 0.1958 0.127 Uiso 1 1 calc R . . C7 C 0.2467(6) 0.1967(7) 0.1982(6) 0.117(4) Uani 1 1 d . . . H7A H 0.1820 0.1980 0.2180 0.140 Uiso 1 1 calc R A . H7B H 0.2520 0.1344 0.1932 0.140 Uiso 1 1 calc R . . H7C H 0.2449 0.2210 0.1436 0.140 Uiso 1 1 calc R . . C8 C 0.3495(7) 0.1387(4) 0.3752(5) 0.087(3) Uani 1 1 d . A . H8A H 0.4069 0.1305 0.4182 0.105 Uiso 1 1 calc R . . H8B H 0.3314 0.0900 0.3306 0.105 Uiso 1 1 calc R . . H8C H 0.2876 0.1378 0.3999 0.105 Uiso 1 1 calc R . . C9 C 0.5137(6) 0.3142(5) 0.4736(4) 0.069(2) Uani 1 1 d . . . H9A H 0.5740 0.3675 0.4846 0.083 Uiso 1 1 calc R A . H9B H 0.5385 0.2604 0.4857 0.083 Uiso 1 1 calc R . . H9C H 0.4636 0.3200 0.5092 0.083 Uiso 1 1 calc R . . C10 C 0.5278(7) 0.4745(4) 0.3531(5) 0.087(3) Uani 1 1 d . . . H10A H 0.4819 0.5087 0.3715 0.104 Uiso 1 1 calc R A . H10B H 0.5536 0.5003 0.3045 0.104 Uiso 1 1 calc R . . H10C H 0.5879 0.4773 0.3984 0.104 Uiso 1 1 calc R . . C21 C 0.6126(4) 0.2058(3) -0.1020(3) 0.0276(10) Uani 1 1 d . . . H21A H 0.6209 0.2378 -0.1527 0.033 Uiso 1 1 calc R A . H21B H 0.6790 0.1889 -0.0814 0.033 Uiso 1 1 calc R . . C22 C 0.4406(4) 0.1245(3) -0.1920(3) 0.0311(10) Uani 1 1 d . . . H22A H 0.4552 0.1833 -0.2161 0.037 Uiso 1 1 calc R A . H22B H 0.3747 0.1171 -0.1700 0.037 Uiso 1 1 calc R . . C23 C 0.5127(4) 0.0617(3) -0.0613(3) 0.0278(10) Uani 1 1 d . . . C24 C 0.4121(4) 0.0163(3) -0.0500(3) 0.0277(10) Uani 1 1 d . A . H24 H 0.3515 0.0270 -0.0839 0.033 Uiso 1 1 calc R . . C25 C 0.3999(4) -0.0450(3) 0.0110(3) 0.0287(10) Uani 1 1 d . . . H25 H 0.3310 -0.0754 0.0181 0.034 Uiso 1 1 calc R A . C26 C 0.4615(4) 0.2993(4) -0.0690(3) 0.0386(12) Uani 1 1 d . . . C27 C 0.4510(5) 0.3490(4) -0.1393(3) 0.0468(14) Uani 1 1 d . A . H27 H 0.5117 0.3841 -0.1566 0.056 Uiso 1 1 calc R . . C28 C 0.3504(6) 0.3457(5) -0.1832(4) 0.0634(19) Uani 1 1 d . . . H28 H 0.3430 0.3791 -0.2306 0.076 Uiso 1 1 calc R A . C29 C 0.2596(6) 0.2940(5) -0.1587(5) 0.0657(19) Uani 1 1 d . A . H29 H 0.1915 0.2930 -0.1891 0.079 Uiso 1 1 calc R . . C30 C 0.2697(5) 0.2442(4) -0.0896(4) 0.0545(16) Uani 1 1 d . . . H30 H 0.2090 0.2078 -0.0735 0.065 Uiso 1 1 calc R A . C31 C 0.3705(4) 0.2487(4) -0.0445(3) 0.0426(13) Uani 1 1 d . A . H31 H 0.3775 0.2168 0.0039 0.051 Uiso 1 1 calc R . . C32 C 0.6904(5) 0.3888(3) -0.0258(3) 0.0400(13) Uani 1 1 d . . . C33 C 0.6794(6) 0.4721(4) 0.0019(4) 0.0567(17) Uani 1 1 d . A . H33 H 0.6179 0.4758 0.0219 0.068 Uiso 1 1 calc R . . C34 C 0.7599(8) 0.5508(4) 0.0003(4) 0.084(3) Uani 1 1 d . . . H34 H 0.7525 0.6076 0.0191 0.101 Uiso 1 1 calc R A . C35 C 0.8484(8) 0.5458(6) -0.0284(5) 0.099(4) Uani 1 1 d . A . H35 H 0.9019 0.5994 -0.0298 0.119 Uiso 1 1 calc R . . C36 C 0.8615(6) 0.4643(5) -0.0553(4) 0.080(3) Uani 1 1 d . . . H36 H 0.9238 0.4618 -0.0747 0.096 Uiso 1 1 calc R A . C37 C 0.7818(5) 0.3844(4) -0.0540(4) 0.0569(17) Uani 1 1 d . A . H37 H 0.7904 0.3279 -0.0723 0.068 Uiso 1 1 calc R . . C38 C 0.5428(4) 0.0650(3) -0.3189(3) 0.0321(11) Uani 1 1 d . . . C39 C 0.6408(4) 0.0749(4) -0.2669(3) 0.0381(12) Uani 1 1 d . A . H39 H 0.6442 0.0626 -0.2101 0.046 Uiso 1 1 calc R . . C40 C 0.7347(4) 0.1031(4) -0.2978(4) 0.0523(16) Uani 1 1 d . . . H40 H 0.8011 0.1138 -0.2610 0.063 Uiso 1 1 calc R A . C41 C 0.7304(5) 0.1150(4) -0.3807(5) 0.0583(18) Uani 1 1 d . A . H41 H 0.7937 0.1330 -0.4017 0.070 Uiso 1 1 calc R . . C42 C 0.6327(6) 0.1007(5) -0.4345(4) 0.0628(19) Uani 1 1 d . . . H42 H 0.6299 0.1083 -0.4922 0.075 Uiso 1 1 calc R A . C43 C 0.5398(5) 0.0756(4) -0.4043(3) 0.0454(14) Uani 1 1 d . A . H43 H 0.4738 0.0654 -0.4415 0.054 Uiso 1 1 calc R . . C44 C 0.3187(4) 0.0604(4) -0.3551(3) 0.0344(11) Uani 1 1 d . . . C45 C 0.3286(4) 0.1514(4) -0.3738(3) 0.0402(12) Uani 1 1 d . A . H45 H 0.3883 0.1977 -0.3468 0.048 Uiso 1 1 calc R . . C46 C 0.2496(5) 0.1720(4) -0.4323(3) 0.0454(14) Uani 1 1 d . . . H46 H 0.2546 0.2327 -0.4442 0.054 Uiso 1 1 calc R A . C47 C 0.1633(5) 0.1032(5) -0.4734(4) 0.0530(16) Uani 1 1 d . A . H47 H 0.1099 0.1169 -0.5137 0.064 Uiso 1 1 calc R . . C48 C 0.1562(4) 0.0148(5) -0.4549(4) 0.0526(16) Uani 1 1 d . . . H48 H 0.0981 -0.0319 -0.4836 0.063 Uiso 1 1 calc R A . C49 C 0.2315(4) -0.0066(4) -0.3959(3) 0.0397(12) Uani 1 1 d . A . H49 H 0.2240 -0.0672 -0.3829 0.048 Uiso 1 1 calc R . . C50 C 1.0488(7) 0.1292(7) -0.2914(5) 0.097(3) Uani 1 1 d . . . H50A H 1.1211 0.1247 -0.2933 0.117 Uiso 1 1 calc R . . H50B H 1.0464 0.1445 -0.2326 0.117 Uiso 1 1 calc R . . Cl3 Cl 1.0214(2) 0.2196(2) -0.35347(19) 0.1167(9) Uani 1 1 d . . . Cl4 Cl 0.95722(17) 0.02211(19) -0.32698(15) 0.0978(7) Uani 1 1 d . . . Cl1 Cl 1.21751(13) 0.41165(12) 0.40648(10) 0.0603(4) Uani 1 1 d . . . O1 O 1.3083(4) 0.4775(6) 0.4414(5) 0.142(3) Uani 1 1 d . . . O2 O 1.1281(4) 0.4386(5) 0.4178(4) 0.107(2) Uani 1 1 d . . . O3 O 1.2108(6) 0.4068(6) 0.3183(4) 0.130(3) Uani 1 1 d . . . O4 O 1.2205(7) 0.3309(6) 0.4308(7) 0.207(6) Uani 1 1 d . . . Cl2 Cl 0.95072(14) 0.20420(13) -0.07594(11) 0.0636(4) Uani 1 1 d . . . O5 O 0.9543(6) 0.2756(5) -0.1288(4) 0.118(2) Uani 1 1 d . A . C53 C 1.0765(19) -0.0222(15) -0.0684(14) 0.43(2) Uani 1 1 d D . . H53A H 1.0677 -0.0849 -0.0552 0.515 Uiso 1 1 calc R . . H53B H 1.0078 -0.0082 -0.0768 0.515 Uiso 1 1 calc R . . H53C H 1.1249 0.0178 -0.0221 0.515 Uiso 1 1 calc R . . C54 C 1.1208(8) -0.0088(7) -0.1465(7) 0.091(3) Uani 1 1 d D . . N3 N 1.1678(7) 0.0098(6) -0.1879(5) 0.100(3) Uani 1 1 d D . . C51 C 0.7903(6) 0.3635(5) -0.2959(5) 0.080(2) Uani 1 1 d . . . H51A H 0.8261 0.3334 -0.2525 0.096 Uiso 1 1 calc R . . H51B H 0.8178 0.4289 -0.2842 0.096 Uiso 1 1 calc R . . H51C H 0.8029 0.3453 -0.3503 0.096 Uiso 1 1 calc R . . C52 C 0.6770(6) 0.3383(4) -0.2966(4) 0.0569(17) Uani 1 1 d . . . N2 N 0.5887(5) 0.3170(4) -0.2975(4) 0.0670(16) Uani 1 1 d . . . O6 O 0.9781(8) 0.1311(7) -0.1212(6) 0.099(3) Uiso 0.664(8) 1 d P A 1 O7 O 1.0371(6) 0.2276(6) -0.0038(6) 0.077(2) Uiso 0.664(8) 1 d P A 1 O8 O 0.8544(7) 0.1751(7) -0.0528(6) 0.091(3) Uiso 0.664(8) 1 d P A 1 O6A O 1.051(3) 0.182(2) -0.040(2) 0.185(13) Uiso 0.336(8) 1 d P A 2 O7A O 0.8851(17) 0.2249(16) -0.0130(15) 0.112(7) Uiso 0.336(8) 1 d P A 2 O8A O 0.8717(18) 0.1120(17) -0.1101(15) 0.130(9) Uiso 0.336(8) 1 d P A 2 C11 C 0.8636(3) 0.4268(3) 0.3319(3) 0.037(2) Uani 0.664(8) 1 d PG A 1 C12 C 0.8943(4) 0.4109(3) 0.2556(3) 0.043(2) Uani 0.664(8) 1 d PG A 1 C13 C 0.9287(4) 0.3373(3) 0.2584(3) 0.054(3) Uani 0.664(8) 1 d PG A 1 C14 C 0.9190(3) 0.2985(3) 0.3397(3) 0.046(3) Uani 0.664(8) 1 d PG A 1 C15 C 0.8799(3) 0.3588(3) 0.3848(3) 0.035(2) Uani 0.664(8) 1 d PG A 1 C16 C 0.8260(5) 0.5121(5) 0.3612(4) 0.083(2) Uani 0.664(8) 1 d PGU A 1 H16A H 0.8877 0.5600 0.3885 0.100 Uiso 0.664(8) 1 calc PR A 1 H16B H 0.7786 0.4943 0.4005 0.100 Uiso 0.664(8) 1 calc PR A 1 H16C H 0.7887 0.5342 0.3125 0.100 Uiso 0.664(8) 1 calc PR A 1 C17 C 0.8995(6) 0.4761(5) 0.1887(4) 0.083(2) Uani 0.664(8) 1 d PGU A 1 H17A H 0.9606 0.5280 0.2068 0.100 Uiso 0.664(8) 1 calc PR A 1 H17B H 0.8348 0.4966 0.1791 0.100 Uiso 0.664(8) 1 calc PR A 1 H17C H 0.9063 0.4460 0.1370 0.100 Uiso 0.664(8) 1 calc PR A 1 C18 C 0.9808(6) 0.3062(5) 0.1897(5) 0.083(2) Uani 0.664(8) 1 d PGU A 1 H18A H 0.9303 0.2934 0.1366 0.100 Uiso 0.664(8) 1 calc PR A 1 H18B H 1.0024 0.2516 0.2048 0.100 Uiso 0.664(8) 1 calc PR A 1 H18C H 1.0429 0.3539 0.1843 0.100 Uiso 0.664(8) 1 calc PR A 1 C19 C 0.9529(6) 0.2161(5) 0.3705(5) 0.083(2) Uani 0.664(8) 1 d PGU A 1 H19A H 0.9251 0.1992 0.4208 0.100 Uiso 0.664(8) 1 calc PR A 1 H19B H 1.0301 0.2302 0.3834 0.100 Uiso 0.664(8) 1 calc PR A 1 H19C H 0.9253 0.1660 0.3270 0.100 Uiso 0.664(8) 1 calc PR A 1 C20 C 0.8668(5) 0.3560(5) 0.4747(4) 0.083(2) Uani 0.664(8) 1 d PGU A 1 H20A H 0.8493 0.2933 0.4887 0.100 Uiso 0.664(8) 1 calc PR A 1 H20B H 0.8099 0.3832 0.4825 0.100 Uiso 0.664(8) 1 calc PR A 1 H20C H 0.9328 0.3896 0.5113 0.100 Uiso 0.664(8) 1 calc PR A 1 C11A C 0.8844(8) 0.4242(7) 0.2664(6) 0.048(3) Uani 0.336(8) 1 d PG A 2 C12A C 0.9320(7) 0.3485(7) 0.2424(6) 0.048(3) Uani 0.336(8) 1 d PG A 2 C13A C 0.9342(6) 0.2899(6) 0.3079(6) 0.048(3) Uani 0.336(8) 1 d PG A 2 C14A C 0.8992(6) 0.3197(6) 0.3706(5) 0.048(3) Uani 0.336(8) 1 d PG A 2 C15A C 0.8741(7) 0.4000(6) 0.3581(5) 0.048(3) Uani 0.336(8) 1 d PG A 2 C16A C 0.8837(12) 0.4984(10) 0.2081(9) 0.065(3) Uani 0.336(8) 1 d PG A 2 H16D H 0.9553 0.5377 0.2142 0.079 Uiso 0.336(8) 1 calc PR A 2 H16E H 0.8364 0.5338 0.2220 0.079 Uiso 0.336(8) 1 calc PR A 2 H16F H 0.8589 0.4718 0.1504 0.079 Uiso 0.336(8) 1 calc PR A 2 C17A C 0.9678(12) 0.3306(10) 0.1598(9) 0.065(3) Uani 0.336(8) 1 d PG A 2 H17D H 1.0422 0.3628 0.1644 0.079 Uiso 0.336(8) 1 calc PR A 2 H17E H 0.9248 0.3519 0.1138 0.079 Uiso 0.336(8) 1 calc PR A 2 H17F H 0.9591 0.2659 0.1489 0.079 Uiso 0.336(8) 1 calc PR A 2 C18A C 0.9666(10) 0.2005(9) 0.3117(9) 0.065(3) Uani 0.336(8) 1 d PG A 2 H18D H 1.0360 0.2104 0.3482 0.079 Uiso 0.336(8) 1 calc PR A 2 H18E H 0.9701 0.1787 0.2555 0.079 Uiso 0.336(8) 1 calc PR A 2 H18F H 0.9144 0.1557 0.3338 0.079 Uiso 0.336(8) 1 calc PR A 2 C19A C 0.9055(10) 0.2942(9) 0.4585(8) 0.065(3) Uani 0.336(8) 1 d PG A 2 H19D H 0.8926 0.2287 0.4587 0.079 Uiso 0.336(8) 1 calc PR A 2 H19E H 0.8521 0.3138 0.4830 0.079 Uiso 0.336(8) 1 calc PR A 2 H19F H 0.9758 0.3233 0.4913 0.079 Uiso 0.336(8) 1 calc PR A 2 C20A C 0.8343(11) 0.4755(9) 0.4006(8) 0.065(3) Uani 0.336(8) 1 d PG A 2 H20D H 0.7968 0.4504 0.4443 0.079 Uiso 0.336(8) 1 calc PR A 2 H20E H 0.7864 0.4973 0.3586 0.079 Uiso 0.336(8) 1 calc PR A 2 H20F H 0.8949 0.5256 0.4254 0.079 Uiso 0.336(8) 1 calc PR 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 0.0355(3) 0.0279(2) 0.0177(2) 0.00103(16) 0.01080(17) 0.00504(18) Mo2 0.0325(3) 0.0313(2) 0.0193(2) 0.00205(16) 0.00695(17) -0.00023(18) Cu1 0.0420(4) 0.0323(3) 0.0175(3) 0.0021(2) 0.0102(2) 0.0068(3) Cu2 0.0381(3) 0.0283(3) 0.0224(3) 0.0037(2) 0.0084(2) 0.0040(3) S1 0.0340(6) 0.0290(6) 0.0205(5) 0.0011(4) 0.0075(5) 0.0048(5) S2 0.0340(6) 0.0342(6) 0.0249(6) 0.0031(5) 0.0108(5) 0.0066(5) S3 0.0419(7) 0.0265(6) 0.0232(6) 0.0017(5) 0.0118(5) 0.0039(5) S4 0.0382(7) 0.0357(6) 0.0177(5) 0.0027(5) 0.0083(5) 0.0028(5) P1 0.0390(7) 0.0290(6) 0.0193(6) 0.0037(5) 0.0107(5) 0.0101(5) P2 0.0327(7) 0.0290(6) 0.0176(6) 0.0048(5) 0.0055(5) 0.0051(5) N1 0.038(2) 0.028(2) 0.0187(19) 0.0051(16) 0.0046(16) 0.0041(18) C1 0.068(4) 0.072(4) 0.040(3) 0.014(3) 0.027(3) 0.043(4) C2 0.043(3) 0.094(5) 0.049(4) -0.027(4) 0.014(3) 0.022(4) C3 0.053(3) 0.042(3) 0.054(4) -0.002(3) 0.039(3) 0.005(3) C4 0.052(3) 0.037(3) 0.030(3) -0.004(2) 0.022(2) 0.011(2) C5 0.064(4) 0.032(3) 0.044(3) -0.003(2) 0.034(3) 0.008(3) C6 0.137(8) 0.172(10) 0.064(5) 0.044(6) 0.047(5) 0.120(8) C7 0.050(4) 0.183(11) 0.105(7) -0.085(7) 0.007(4) 0.027(6) C8 0.125(7) 0.044(4) 0.112(7) 0.006(4) 0.098(6) 0.005(4) C9 0.100(5) 0.094(6) 0.029(3) -0.002(3) 0.025(3) 0.043(5) C10 0.120(7) 0.034(3) 0.121(7) -0.005(4) 0.081(6) 0.007(4) C21 0.038(3) 0.027(2) 0.018(2) 0.0047(18) 0.0123(19) 0.005(2) C22 0.042(3) 0.032(3) 0.025(2) 0.0082(19) 0.011(2) 0.016(2) C23 0.043(3) 0.024(2) 0.020(2) 0.0035(17) 0.013(2) 0.009(2) C24 0.029(2) 0.028(2) 0.025(2) 0.0036(19) 0.0036(19) 0.006(2) C25 0.032(3) 0.032(2) 0.019(2) 0.0016(18) 0.0070(19) 0.004(2) C26 0.049(3) 0.044(3) 0.032(3) 0.005(2) 0.016(2) 0.022(3) C27 0.059(4) 0.053(3) 0.036(3) 0.012(3) 0.011(3) 0.027(3) C28 0.079(5) 0.079(5) 0.050(4) 0.026(4) 0.017(4) 0.048(4) C29 0.061(4) 0.084(5) 0.063(4) 0.010(4) 0.004(4) 0.043(4) C30 0.045(3) 0.062(4) 0.061(4) 0.004(3) 0.012(3) 0.021(3) C31 0.051(3) 0.047(3) 0.041(3) 0.007(2) 0.018(3) 0.026(3) C32 0.067(4) 0.025(2) 0.021(2) 0.0012(19) 0.008(2) 0.000(2) C33 0.092(5) 0.036(3) 0.038(3) 0.002(3) -0.001(3) 0.019(3) C34 0.162(9) 0.022(3) 0.042(4) -0.003(3) -0.010(5) -0.001(4) C35 0.145(9) 0.061(5) 0.040(4) 0.014(4) -0.007(5) -0.051(6) C36 0.090(5) 0.065(5) 0.057(4) -0.001(4) 0.022(4) -0.037(4) C37 0.064(4) 0.046(3) 0.050(4) -0.004(3) 0.024(3) -0.013(3) C38 0.046(3) 0.029(2) 0.022(2) 0.0053(19) 0.010(2) 0.007(2) C39 0.042(3) 0.039(3) 0.032(3) -0.008(2) 0.010(2) 0.010(2) C40 0.037(3) 0.049(4) 0.067(4) -0.013(3) 0.013(3) 0.005(3) C41 0.057(4) 0.051(4) 0.083(5) 0.025(3) 0.045(4) 0.019(3) C42 0.080(5) 0.075(5) 0.058(4) 0.034(4) 0.047(4) 0.038(4) C43 0.050(3) 0.060(4) 0.035(3) 0.024(3) 0.019(3) 0.021(3) C44 0.038(3) 0.046(3) 0.021(2) 0.009(2) 0.010(2) 0.011(2) C45 0.047(3) 0.049(3) 0.027(3) 0.011(2) 0.007(2) 0.017(3) C46 0.055(4) 0.055(3) 0.033(3) 0.021(3) 0.009(3) 0.026(3) C47 0.043(3) 0.083(5) 0.038(3) 0.023(3) 0.006(3) 0.026(3) C48 0.030(3) 0.078(5) 0.043(3) 0.010(3) -0.003(3) 0.007(3) C49 0.037(3) 0.051(3) 0.028(3) 0.006(2) 0.003(2) 0.007(3) C50 0.080(6) 0.136(9) 0.068(6) 0.015(6) 0.004(4) 0.018(6) Cl3 0.0955(17) 0.142(2) 0.121(2) 0.0342(19) 0.0235(15) 0.0411(16) Cl4 0.0740(13) 0.135(2) 0.0798(15) -0.0140(14) 0.0096(11) 0.0266(14) Cl1 0.0537(9) 0.0648(10) 0.0533(9) -0.0092(8) 0.0119(7) -0.0002(8) O1 0.060(4) 0.188(8) 0.136(7) -0.065(6) 0.016(4) -0.032(4) O2 0.048(3) 0.147(6) 0.109(5) -0.057(4) 0.014(3) 0.007(3) O3 0.154(6) 0.191(8) 0.063(4) -0.024(4) 0.018(4) 0.084(6) O4 0.170(8) 0.169(9) 0.294(14) 0.167(10) 0.042(9) 0.047(7) Cl2 0.0622(10) 0.0700(11) 0.0622(10) -0.0009(8) 0.0191(8) 0.0197(9) O5 0.136(6) 0.125(6) 0.109(5) 0.058(5) 0.041(4) 0.043(5) C53 0.59(4) 0.43(3) 0.63(4) 0.45(3) 0.54(4) 0.45(3) C54 0.080(6) 0.082(6) 0.123(9) 0.026(6) 0.020(6) 0.039(5) N3 0.123(7) 0.119(7) 0.087(6) 0.039(5) 0.026(5) 0.077(6) C51 0.090(6) 0.073(5) 0.077(5) 0.026(4) 0.027(4) 0.009(4) C52 0.082(5) 0.051(4) 0.040(3) 0.011(3) 0.021(3) 0.013(4) N2 0.079(4) 0.068(4) 0.055(4) 0.014(3) 0.022(3) 0.015(3) C11 0.037(4) 0.027(4) 0.033(5) 0.000(3) -0.009(4) -0.006(3) C12 0.031(5) 0.041(5) 0.045(5) 0.014(4) 0.001(4) -0.009(4) C13 0.029(5) 0.074(7) 0.050(6) -0.008(5) 0.019(4) -0.011(5) C14 0.023(4) 0.034(5) 0.073(7) 0.006(5) -0.004(5) 0.003(4) C15 0.033(4) 0.038(5) 0.021(4) 0.008(3) -0.010(3) -0.006(4) C16 0.058(3) 0.082(4) 0.088(4) -0.002(3) -0.004(3) -0.007(3) C17 0.058(3) 0.082(4) 0.088(4) -0.002(3) -0.004(3) -0.007(3) C18 0.058(3) 0.082(4) 0.088(4) -0.002(3) -0.004(3) -0.007(3) C19 0.058(3) 0.082(4) 0.088(4) -0.002(3) -0.004(3) -0.007(3) C20 0.058(3) 0.082(4) 0.088(4) -0.002(3) -0.004(3) -0.007(3) C11A 0.036(6) 0.055(6) 0.042(5) -0.006(5) 0.009(4) -0.006(5) C12A 0.036(6) 0.055(6) 0.042(5) -0.006(5) 0.009(4) -0.006(5) C13A 0.036(6) 0.055(6) 0.042(5) -0.006(5) 0.009(4) -0.006(5) C14A 0.036(6) 0.055(6) 0.042(5) -0.006(5) 0.009(4) -0.006(5) C15A 0.036(6) 0.055(6) 0.042(5) -0.006(5) 0.009(4) -0.006(5) C16A 0.040(5) 0.072(7) 0.072(7) 0.016(5) 0.006(5) -0.006(5) C17A 0.040(5) 0.072(7) 0.072(7) 0.016(5) 0.006(5) -0.006(5) C18A 0.040(5) 0.072(7) 0.072(7) 0.016(5) 0.006(5) -0.006(5) C19A 0.040(5) 0.072(7) 0.072(7) 0.016(5) 0.006(5) -0.006(5) C20A 0.040(5) 0.072(7) 0.072(7) 0.016(5) 0.006(5) -0.006(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 2.2571(15) . ? Mo1 S3 2.3494(14) . ? Mo1 S4 2.3501(15) . ? Mo1 C1 2.374(6) . ? Mo1 C3 2.387(5) . ? Mo1 C5 2.389(5) . ? Mo1 C2 2.395(6) . ? Mo1 C4 2.402(5) . ? Mo1 Cu1 2.8277(9) . ? Mo1 Cu2 2.8408(10) . ? Mo1 Mo2 2.8940(9) . ? Mo2 S2 2.2502(15) . ? Mo2 C15A 2.347(9) . ? Mo2 C14A 2.351(8) . ? Mo2 S4 2.3589(14) . ? Mo2 S3 2.3612(15) . ? Mo2 C14 2.365(4) . ? Mo2 C13 2.368(5) . ? Mo2 C12 2.371(5) . ? Mo2 C11 2.372(4) . ? Mo2 C11A 2.386(10) . ? Mo2 C15 2.401(4) . ? Mo2 C13A 2.466(8) . ? Cu1 P1 2.2570(14) . ? Cu1 S3 2.2938(15) . ? Cu1 S2 2.3997(15) . ? Cu1 S1 2.4010(15) . ? Cu2 P2 2.2676(14) 2_655 ? Cu2 S4 2.3025(15) . ? Cu2 S2 2.4039(15) . ? Cu2 S1 2.4060(15) . ? P1 C32 1.833(5) . ? P1 C26 1.837(5) . ? P1 C21 1.895(5) . ? P2 C44 1.838(5) . ? P2 C38 1.850(5) . ? P2 C22 1.883(5) . ? P2 Cu2 2.2676(14) 2_655 ? N1 C23 1.435(5) . ? N1 C21 1.447(6) . ? N1 C22 1.455(6) . ? C1 C2 1.406(10) . ? C1 C5 1.414(8) . ? C1 C6 1.522(9) . ? C2 C3 1.430(9) . ? C2 C7 1.527(9) . ? C3 C4 1.418(8) . ? C3 C8 1.513(8) . ? C4 C5 1.409(7) . ? C4 C9 1.520(8) . ? C5 C10 1.532(8) . ? C23 C25 1.388(7) 2_655 ? C23 C24 1.398(6) . ? C24 C25 1.401(6) . ? C25 C23 1.388(7) 2_655 ? C26 C31 1.403(7) . ? C26 C27 1.410(7) . ? C27 C28 1.392(9) . ? C28 C29 1.407(10) . ? C29 C30 1.394(9) . ? C30 C31 1.397(8) . ? C32 C37 1.395(8) . ? C32 C33 1.396(8) . ? C33 C34 1.408(10) . ? C34 C35 1.366(13) . ? C35 C36 1.377(13) . ? C36 C37 1.415(8) . ? C38 C39 1.396(7) . ? C38 C43 1.406(7) . ? C39 C40 1.409(7) . ? C40 C41 1.368(9) . ? C41 C42 1.397(9) . ? C42 C43 1.388(8) . ? C44 C49 1.389(7) . ? C44 C45 1.425(7) . ? C45 C46 1.398(8) . ? C46 C47 1.400(9) . ? C47 C48 1.390(9) . ? C48 C49 1.375(8) . ? C50 Cl4 1.794(9) . ? C50 Cl3 1.825(9) . ? Cl1 O4 1.328(8) . ? Cl1 O1 1.385(6) . ? Cl1 O2 1.398(6) . ? Cl1 O3 1.427(6) . ? Cl2 O8 1.376(10) . ? Cl2 O5 1.420(6) . ? Cl2 O7 1.457(8) . ? Cl2 O6A 1.48(3) . ? Cl2 O6 1.480(10) . ? Cl2 O7A 1.54(2) . ? Cl2 O8A 1.56(2) . ? C53 C54 1.502(13) . ? C54 N3 1.006(10) . ? C51 C52 1.461(10) . ? C52 N2 1.138(8) . ? C11 C12 1.413(3) . ? C11 C15 1.417(3) . ? C11 C16 1.606(3) . ? C12 C13 1.325(3) . ? C12 C17 1.511(3) . ? C13 C14 1.492(3) . ? C13 C18 1.543(3) . ? C14 C15 1.417(3) . ? C14 C19 1.522(3) . ? C15 C20 1.513(3) . ? C11A C16A 1.515(5) . ? C11A C12A 1.532(5) . ? C11A C15A 1.581(6) . ? C12A C13A 1.426(5) . ? C12A C17A 1.549(6) . ? C13A C14A 1.313(5) . ? C13A C18A 1.542(6) . ? C14A C15A 1.372(5) . ? C14A C19A 1.498(5) . ? C15A C20A 1.582(6) . ? 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 105.35(5) . . ? S1 Mo1 S4 105.37(5) . . ? S3 Mo1 S4 101.00(5) . . ? S1 Mo1 C1 105.59(18) . . ? S3 Mo1 C1 90.89(17) . . ? S4 Mo1 C1 142.37(15) . . ? S1 Mo1 C3 97.96(15) . . ? S3 Mo1 C3 145.38(15) . . ? S4 Mo1 C3 96.97(16) . . ? C1 Mo1 C3 57.9(2) . . ? S1 Mo1 C5 138.96(16) . . ? S3 Mo1 C5 88.73(13) . . ? S4 Mo1 C5 109.48(16) . . ? C1 Mo1 C5 34.5(2) . . ? C3 Mo1 C5 57.28(19) . . ? S1 Mo1 C2 83.99(16) . . ? S3 Mo1 C2 122.6(2) . . ? S4 Mo1 C2 131.51(19) . . ? C1 Mo1 C2 34.3(2) . . ? C3 Mo1 C2 34.8(2) . . ? C5 Mo1 C2 56.7(2) . . ? S1 Mo1 C4 132.39(13) . . ? S3 Mo1 C4 117.92(13) . . ? S4 Mo1 C4 85.77(14) . . ? C1 Mo1 C4 57.4(2) . . ? C3 Mo1 C4 34.44(19) . . ? C5 Mo1 C4 34.21(18) . . ? C2 Mo1 C4 56.9(2) . . ? S1 Mo1 Cu1 54.98(4) . . ? S3 Mo1 Cu1 51.59(4) . . ? S4 Mo1 Cu1 102.41(4) . . ? C1 Mo1 Cu1 112.72(14) . . ? C3 Mo1 Cu1 150.02(15) . . ? C5 Mo1 Cu1 133.28(13) . . ? C2 Mo1 Cu1 120.36(16) . . ? C4 Mo1 Cu1 167.47(13) . . ? S1 Mo1 Cu2 54.89(4) . . ? S3 Mo1 Cu2 102.76(4) . . ? S4 Mo1 Cu2 51.61(4) . . ? C1 Mo1 Cu2 158.40(18) . . ? C3 Mo1 Cu2 111.59(15) . . ? C5 Mo1 Cu2 159.12(15) . . ? C2 Mo1 Cu2 125.99(19) . . ? C4 Mo1 Cu2 126.32(13) . . ? Cu1 Mo1 Cu2 65.86(3) . . ? S1 Mo1 Mo2 98.88(5) . . ? S3 Mo1 Mo2 52.28(4) . . ? S4 Mo1 Mo2 52.22(4) . . ? C1 Mo1 Mo2 140.37(18) . . ? C3 Mo1 Mo2 147.96(16) . . ? C5 Mo1 Mo2 119.41(14) . . ? C2 Mo1 Mo2 174.6(2) . . ? C4 Mo1 Mo2 122.53(14) . . ? Cu1 Mo1 Mo2 58.80(3) . . ? Cu2 Mo1 Mo2 59.09(3) . . ? S2 Mo2 C15A 139.4(2) . . ? S2 Mo2 C14A 114.1(3) . . ? C15A Mo2 C14A 33.97(15) . . ? S2 Mo2 S4 105.71(5) . . ? C15A Mo2 S4 98.4(2) . . ? C14A Mo2 S4 88.1(2) . . ? S2 Mo2 S3 105.98(5) . . ? C15A Mo2 S3 101.1(2) . . ? C14A Mo2 S3 135.0(2) . . ? S4 Mo2 S3 100.40(5) . . ? S2 Mo2 C14 97.64(13) . . ? C15A Mo2 C14 46.0(2) . . ? C14A Mo2 C14 17.4(2) . . ? S4 Mo2 C14 98.40(12) . . ? S3 Mo2 C14 144.33(11) . . ? S2 Mo2 C13 84.95(13) . . ? C15A Mo2 C13 55.3(2) . . ? C14A Mo2 C13 49.0(2) . . ? S4 Mo2 C13 135.12(12) . . ? S3 Mo2 C13 118.70(12) . . ? C14 Mo2 C13 36.75(9) . . ? S2 Mo2 C12 106.71(12) . . ? C15A Mo2 C12 43.6(2) . . ? C14A Mo2 C12 60.8(2) . . ? S4 Mo2 C12 142.03(11) . . ? S3 Mo2 C12 89.19(12) . . ? C14 Mo2 C12 58.14(13) . . ? C13 Mo2 C12 32.47(8) . . ? S2 Mo2 C11 139.97(11) . . ? C15A Mo2 C11 15.3(2) . . ? C14A Mo2 C11 48.1(2) . . ? S4 Mo2 C11 108.47(11) . . ? S3 Mo2 C11 87.79(11) . . ? C14 Mo2 C11 57.46(13) . . ? C13 Mo2 C11 56.03(13) . . ? C12 Mo2 C11 34.67(8) . . ? S2 Mo2 C11A 114.3(2) . . ? C15A Mo2 C11A 39.02(18) . . ? C14A Mo2 C11A 60.9(3) . . ? S4 Mo2 C11A 136.5(2) . . ? S3 Mo2 C11A 84.7(2) . . ? C14 Mo2 C11A 61.0(3) . . ? C13 Mo2 C11A 39.4(3) . . ? C12 Mo2 C11A 8.0(3) . . ? C11 Mo2 C11A 28.1(3) . . ? S2 Mo2 C15 132.14(13) . . ? C15A Mo2 C15 19.2(2) . . ? C14A Mo2 C15 18.3(2) . . ? S4 Mo2 C15 85.56(10) . . ? S3 Mo2 C15 117.68(12) . . ? C14 Mo2 C15 34.57(8) . . ? C13 Mo2 C15 58.03(13) . . ? C12 Mo2 C15 57.92(13) . . ? C11 Mo2 C15 34.53(8) . . ? C11A Mo2 C15 55.2(2) . . ? S2 Mo2 C13A 85.6(2) . . ? C15A Mo2 C13A 55.4(2) . . ? C14A Mo2 C13A 31.52(13) . . ? S4 Mo2 C13A 109.4(2) . . ? S3 Mo2 C13A 143.8(2) . . ? C14 Mo2 C13A 14.4(2) . . ? C13 Mo2 C13A 26.6(2) . . ? C12 Mo2 C13A 54.6(2) . . ? C11 Mo2 C13A 63.9(2) . . ? C11A Mo2 C13A 59.6(2) . . ? C15 Mo2 C13A 47.5(2) . . ? P1 Cu1 S3 110.90(5) . . ? P1 Cu1 S2 114.95(5) . . ? S3 Cu1 S2 103.36(6) . . ? P1 Cu1 S1 124.46(6) . . ? S3 Cu1 S1 102.56(5) . . ? S2 Cu1 S1 97.92(5) . . ? P1 Cu1 Mo2 137.74(4) . . ? S3 Cu1 Mo2 53.98(4) . . ? S2 Cu1 Mo2 50.44(4) . . ? S1 Cu1 Mo2 97.79(4) . . ? P1 Cu1 Mo1 146.76(4) . . ? S3 Cu1 Mo1 53.38(4) . . ? S2 Cu1 Mo1 97.94(4) . . ? S1 Cu1 Mo1 50.34(4) . . ? Mo2 Cu1 Mo1 61.78(2) . . ? P2 Cu2 S4 115.24(5) 2_655 . ? P2 Cu2 S2 123.83(6) 2_655 . ? S4 Cu2 S2 102.64(5) . . ? P2 Cu2 S1 112.01(6) 2_655 . ? S4 Cu2 S1 102.19(6) . . ? S2 Cu2 S1 97.67(5) . . ? P2 Cu2 Mo2 150.76(4) 2_655 . ? S4 Cu2 Mo2 53.56(4) . . ? S2 Cu2 Mo2 50.14(4) . . ? S1 Cu2 Mo2 97.17(4) . . ? P2 Cu2 Mo1 138.25(4) 2_655 . ? S4 Cu2 Mo1 53.13(4) . . ? S2 Cu2 Mo1 97.49(4) . . ? S1 Cu2 Mo1 50.12(4) . . ? Mo2 Cu2 Mo1 61.39(2) . . ? Mo1 S1 Cu1 74.68(5) . . ? Mo1 S1 Cu2 74.99(5) . . ? Cu1 S1 Cu2 79.74(5) . . ? Mo2 S2 Cu1 74.27(5) . . ? Mo2 S2 Cu2 74.76(5) . . ? Cu1 S2 Cu2 79.81(5) . . ? Cu1 S3 Mo1 75.02(4) . . ? Cu1 S3 Mo2 74.23(5) . . ? Mo1 S3 Mo2 75.81(4) . . ? Cu2 S4 Mo1 75.26(5) . . ? Cu2 S4 Mo2 74.70(4) . . ? Mo1 S4 Mo2 75.84(4) . . ? C32 P1 C26 107.6(3) . . ? C32 P1 C21 101.9(2) . . ? C26 P1 C21 100.4(2) . . ? C32 P1 Cu1 110.72(16) . . ? C26 P1 Cu1 114.09(17) . . ? C21 P1 Cu1 120.71(15) . . ? C44 P2 C38 105.0(2) . . ? C44 P2 C22 100.5(2) . . ? C38 P2 C22 102.8(2) . . ? C44 P2 Cu2 115.80(17) . 2_655 ? C38 P2 Cu2 110.43(16) . 2_655 ? C22 P2 Cu2 120.48(15) . 2_655 ? C23 N1 C21 117.7(4) . . ? C23 N1 C22 120.6(4) . . ? C21 N1 C22 118.4(4) . . ? C2 C1 C5 107.4(5) . . ? C2 C1 C6 128.8(7) . . ? C5 C1 C6 123.4(7) . . ? C2 C1 Mo1 73.7(4) . . ? C5 C1 Mo1 73.3(3) . . ? C6 C1 Mo1 123.9(4) . . ? C1 C2 C3 108.8(5) . . ? C1 C2 C7 125.3(8) . . ? C3 C2 C7 125.5(8) . . ? C1 C2 Mo1 72.0(3) . . ? C3 C2 Mo1 72.3(3) . . ? C7 C2 Mo1 127.7(4) . . ? C4 C3 C2 106.9(5) . . ? C4 C3 C8 125.8(6) . . ? C2 C3 C8 127.1(6) . . ? C4 C3 Mo1 73.3(3) . . ? C2 C3 Mo1 72.9(3) . . ? C8 C3 Mo1 123.3(4) . . ? C5 C4 C3 108.2(5) . . ? C5 C4 C9 126.0(5) . . ? C3 C4 C9 125.4(6) . . ? C5 C4 Mo1 72.4(3) . . ? C3 C4 Mo1 72.2(3) . . ? C9 C4 Mo1 126.9(4) . . ? C4 C5 C1 108.7(5) . . ? C4 C5 C10 126.0(6) . . ? C1 C5 C10 124.8(6) . . ? C4 C5 Mo1 73.4(3) . . ? C1 C5 Mo1 72.2(3) . . ? C10 C5 Mo1 126.1(4) . . ? N1 C21 P1 112.6(3) . . ? N1 C22 P2 112.9(3) . . ? C25 C23 C24 118.7(4) 2_655 . ? C25 C23 N1 119.8(4) 2_655 . ? C24 C23 N1 121.5(4) . . ? C23 C24 C25 120.6(4) . . ? C23 C25 C24 120.7(4) 2_655 . ? C31 C26 C27 119.2(5) . . ? C31 C26 P1 118.7(4) . . ? C27 C26 P1 121.3(4) . . ? C28 C27 C26 119.1(6) . . ? C27 C28 C29 121.3(6) . . ? C30 C29 C28 119.8(6) . . ? C29 C30 C31 119.1(6) . . ? C30 C31 C26 121.5(5) . . ? C37 C32 C33 119.5(6) . . ? C37 C32 P1 119.5(4) . . ? C33 C32 P1 120.9(5) . . ? C32 C33 C34 119.8(7) . . ? C35 C34 C33 120.2(7) . . ? C34 C35 C36 121.0(7) . . ? C35 C36 C37 119.7(8) . . ? C32 C37 C36 119.8(7) . . ? C39 C38 C43 118.3(5) . . ? C39 C38 P2 120.2(4) . . ? C43 C38 P2 121.3(4) . . ? C38 C39 C40 120.6(5) . . ? C41 C40 C39 120.1(6) . . ? C40 C41 C42 119.9(5) . . ? C43 C42 C41 120.5(6) . . ? C42 C43 C38 120.4(6) . . ? C49 C44 C45 119.6(5) . . ? C49 C44 P2 120.4(4) . . ? C45 C44 P2 120.0(4) . . ? C46 C45 C44 119.2(5) . . ? C45 C46 C47 120.1(6) . . ? C48 C47 C46 119.5(5) . . ? C49 C48 C47 121.3(6) . . ? C48 C49 C44 120.2(6) . . ? Cl4 C50 Cl3 112.9(4) . . ? O4 Cl1 O1 112.3(6) . . ? O4 Cl1 O2 114.9(6) . . ? O1 Cl1 O2 110.4(4) . . ? O4 Cl1 O3 107.2(6) . . ? O1 Cl1 O3 107.2(5) . . ? O2 Cl1 O3 104.1(4) . . ? O8 Cl2 O5 112.7(5) . . ? O8 Cl2 O7 111.7(5) . . ? O5 Cl2 O7 111.5(5) . . ? O8 Cl2 O6A 127.5(13) . . ? O5 Cl2 O6A 118.8(13) . . ? O7 Cl2 O6A 38.8(13) . . ? O8 Cl2 O6 111.9(6) . . ? O5 Cl2 O6 106.8(5) . . ? O7 Cl2 O6 101.6(5) . . ? O6A Cl2 O6 62.9(13) . . ? O8 Cl2 O7A 37.2(8) . . ? O5 Cl2 O7A 103.8(9) . . ? O7 Cl2 O7A 83.6(9) . . ? O6A Cl2 O7A 116.2(16) . . ? O6 Cl2 O7A 144.3(9) . . ? O8 Cl2 O8A 57.3(9) . . ? O5 Cl2 O8A 116.9(9) . . ? O7 Cl2 O8A 130.6(9) . . ? O6A Cl2 O8A 105.0(15) . . ? O6 Cl2 O8A 55.8(9) . . ? O7A Cl2 O8A 93.9(12) . . ? N3 C54 C53 164.6(17) . . ? N2 C52 C51 178.8(8) . . ? C12 C11 C15 109.5 . . ? C12 C11 C16 127.3 . . ? C15 C11 C16 123.0 . . ? C12 C11 Mo2 72.60(15) . . ? C15 C11 Mo2 73.86(14) . . ? C16 C11 Mo2 124.25(15) . . ? C13 C12 C11 108.8 . . ? C13 C12 C17 127.2 . . ? C11 C12 C17 123.5 . . ? C13 C12 Mo2 73.65(15) . . ? C11 C12 Mo2 72.73(15) . . ? C17 C12 Mo2 126.04(14) . . ? C12 C13 C14 109.4 . . ? C12 C13 C18 122.7 . . ? C14 C13 C18 127.6 . . ? C12 C13 Mo2 73.88(15) . . ? C14 C13 Mo2 71.54(14) . . ? C18 C13 Mo2 125.91(14) . . ? C15 C14 C13 105.3 . . ? C15 C14 C19 127.4 . . ? C13 C14 C19 127.1 . . ? C15 C14 Mo2 74.11(15) . . ? C13 C14 Mo2 71.72(15) . . ? C19 C14 Mo2 122.78(15) . . ? C14 C15 C11 106.9 . . ? C14 C15 C20 126.8 . . ? C11 C15 C20 126.1 . . ? C14 C15 Mo2 71.32(15) . . ? C11 C15 Mo2 71.61(14) . . ? C20 C15 Mo2 126.10(15) . . ? C16A C11A C12A 117.4 . . ? C16A C11A C15A 143.0 . . ? C12A C11A C15A 98.1 . . ? C16A C11A Mo2 127.1(3) . . ? C12A C11A Mo2 75.8(3) . . ? C15A C11A Mo2 69.1(3) . . ? C13A C12A C11A 109.1 . . ? C13A C12A C17A 122.7 . . ? C11A C12A C17A 128.1 . . ? C13A C12A Mo2 72.0(3) . . ? C11A C12A Mo2 67.8(3) . . ? C17A C12A Mo2 123.8(3) . . ? C14A C13A C12A 110.7 . . ? C14A C13A C18A 119.8 . . ? C12A C13A C18A 129.5 . . ? C14A C13A Mo2 69.4(3) . . ? C12A C13A Mo2 74.6(3) . . ? C18A C13A Mo2 120.6(3) . . ? C13A C14A C15A 112.9 . . ? C13A C14A C19A 131.1 . . ? C15A C14A C19A 114.2 . . ? C13A C14A Mo2 79.1(3) . . ? C15A C14A Mo2 72.9(3) . . ? C19A C14A Mo2 127.0(3) . . ? C14A C15A C11A 108.7 . . ? C14A C15A C20A 143.1 . . ? C11A C15A C20A 108.2 . . ? C14A C15A Mo2 73.2(3) . . ? C11A C15A Mo2 71.8(3) . . ? C20A C15A Mo2 117.1(3) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.538 _refine_diff_density_min -1.276 _refine_diff_density_rms 0.124 #===END #============================================================================== data_4^.^2MeCN^.^2CH~2~Cl~2~ _database_code_depnum_ccdc_archive 'CCDC 783843' #TrackingRef '- JPLangCIF.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H112 Cu4 Mo4 N2 P4 S8, 4(Cl O4), 2(C2 H3 N), 2(C H2 Cl2)' _chemical_formula_sum 'C100 H122 Cl8 Cu4 Mo4 N4 O16 P4 S8' _chemical_formula_weight 2937.90 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' 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' Cl Cl 0.1484 0.1585 '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' _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 36.180(7) _cell_length_b 17.208(3) _cell_length_c 23.247(5) _cell_angle_alpha 90.00 _cell_angle_beta 121.71(3) _cell_angle_gamma 90.00 _cell_volume 12313(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 27418 _cell_measurement_theta_min 3.0395 _cell_measurement_theta_max 27.5243 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5944 _exptl_absorpt_coefficient_mu 1.490 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5170 _exptl_absorpt_correction_T_max 0.6718 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _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 34960 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.49 _reflns_number_total 13875 _reflns_number_gt 11549 _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^)+(0.1250P)^2^+19.8642P] 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 13875 _refine_ls_number_parameters 649 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2446 _refine_ls_wR_factor_gt 0.2309 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.194 _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 0.132131(17) 0.60076(3) 0.73226(3) 0.04750(17) Uani 1 1 d . . . Mo2 Mo 0.159018(16) 0.74536(3) 0.70411(2) 0.04329(16) Uani 1 1 d . . . Cu1 Cu 0.21663(2) 0.64939(5) 0.81090(4) 0.0471(2) Uani 1 1 d . . . Cu2 Cu 0.14527(3) 0.72837(5) 0.81095(4) 0.0494(2) Uani 1 1 d . . . S1 S 0.17090(5) 0.60187(10) 0.84591(8) 0.0509(4) Uani 1 1 d . . . S2 S 0.20423(5) 0.78724(9) 0.80838(7) 0.0471(3) Uani 1 1 d . . . S3 S 0.18258(5) 0.62018(10) 0.69979(8) 0.0487(4) Uani 1 1 d . . . S4 S 0.09412(5) 0.71805(10) 0.69937(8) 0.0503(4) Uani 1 1 d . . . P1 P 0.28816(5) 0.64153(9) 0.87707(7) 0.0424(3) Uani 1 1 d . . . P2 P 0.36712(5) 0.69308(10) 1.12557(8) 0.0449(4) Uani 1 1 d . . . N1 N 0.29267(16) 0.7005(3) 0.9900(2) 0.0460(11) Uani 1 1 d . . . C1 C 0.0773(4) 0.5322(6) 0.6427(6) 0.1003(10) Uani 1 1 d . . . C2 C 0.0652(4) 0.5381(6) 0.6891(6) 0.1003(10) Uani 1 1 d . . . C3 C 0.0924(4) 0.4983(6) 0.7458(6) 0.1003(10) Uani 1 1 d . . . C4 C 0.1242(4) 0.4637(6) 0.7364(6) 0.1003(10) Uani 1 1 d . . . C5 C 0.1161(4) 0.4829(6) 0.6730(6) 0.1003(10) Uani 1 1 d . . . C6 C 0.0520(4) 0.5612(6) 0.5714(6) 0.1003(10) Uani 1 1 d . . . H6A H 0.0282 0.5257 0.5440 0.150 Uiso 1 1 calc R . . H6B H 0.0709 0.5644 0.5536 0.150 Uiso 1 1 calc R . . H6C H 0.0404 0.6123 0.5705 0.150 Uiso 1 1 calc R . . C7 C 0.0231(3) 0.5792(6) 0.6796(6) 0.1003(10) Uani 1 1 d . . . H7A H 0.0290 0.5982 0.7230 0.150 Uiso 1 1 calc R . . H7B H -0.0006 0.5421 0.6616 0.150 Uiso 1 1 calc R . . H7C H 0.0151 0.6225 0.6485 0.150 Uiso 1 1 calc R . . C8 C 0.0898(4) 0.4848(6) 0.8080(6) 0.1003(10) Uani 1 1 d . . . H8A H 0.0711 0.5238 0.8100 0.150 Uiso 1 1 calc R . . H8B H 0.1186 0.4884 0.8482 0.150 Uiso 1 1 calc R . . H8C H 0.0779 0.4335 0.8057 0.150 Uiso 1 1 calc R . . C9 C 0.1614(4) 0.4111(6) 0.7887(6) 0.1003(10) Uani 1 1 d . . . H9A H 0.1518 0.3574 0.7810 0.150 Uiso 1 1 calc R . . H9B H 0.1694 0.4264 0.8340 0.150 Uiso 1 1 calc R . . H9C H 0.1864 0.4163 0.7840 0.150 Uiso 1 1 calc R . . C10 C 0.1385(4) 0.4518(6) 0.6385(6) 0.1003(10) Uani 1 1 d . . . H10A H 0.1686 0.4399 0.6722 0.150 Uiso 1 1 calc R . . H10B H 0.1376 0.4906 0.6074 0.150 Uiso 1 1 calc R . . H10C H 0.1239 0.4050 0.6137 0.150 Uiso 1 1 calc R . . C11 C 0.1153(2) 0.8211(4) 0.6058(3) 0.0569(16) Uani 1 1 d . . . C12 C 0.1449(2) 0.8724(4) 0.6583(3) 0.0566(16) Uani 1 1 d . . . C13 C 0.1879(2) 0.8539(4) 0.6758(3) 0.0553(16) Uani 1 1 d . . . C14 C 0.1854(2) 0.7891(5) 0.6355(4) 0.0630(19) Uani 1 1 d . . . C15 C 0.1408(3) 0.7690(5) 0.5931(3) 0.065(2) Uani 1 1 d . . . C16 C 0.0671(3) 0.8274(6) 0.5674(4) 0.088(3) Uani 1 1 d . . . H16A H 0.0581 0.8537 0.5950 0.132 Uiso 1 1 calc R . . H16B H 0.0545 0.7758 0.5560 0.132 Uiso 1 1 calc R . . H16C H 0.0574 0.8569 0.5263 0.132 Uiso 1 1 calc R . . C17 C 0.1327(4) 0.9382(5) 0.6873(5) 0.086(3) Uani 1 1 d . . . H17A H 0.1553 0.9455 0.7344 0.129 Uiso 1 1 calc R . . H17B H 0.1055 0.9264 0.6841 0.129 Uiso 1 1 calc R . . H17C H 0.1295 0.9854 0.6622 0.129 Uiso 1 1 calc R . . C18 C 0.2281(3) 0.8978(6) 0.7236(5) 0.085(3) Uani 1 1 d . . . H18A H 0.2360 0.9315 0.6983 0.128 Uiso 1 1 calc R . . H18B H 0.2516 0.8616 0.7502 0.128 Uiso 1 1 calc R . . H18C H 0.2230 0.9290 0.7535 0.128 Uiso 1 1 calc R . . C19 C 0.2225(3) 0.7530(6) 0.6341(6) 0.095(4) Uani 1 1 d . . . H19A H 0.2306 0.7861 0.6088 0.142 Uiso 1 1 calc R . . H19B H 0.2138 0.7025 0.6125 0.142 Uiso 1 1 calc R . . H19C H 0.2470 0.7471 0.6799 0.142 Uiso 1 1 calc R . . C20 C 0.1233(4) 0.7073(6) 0.5374(4) 0.098(3) Uani 1 1 d . . . H20A H 0.1414 0.6612 0.5542 0.146 Uiso 1 1 calc R . . H20B H 0.1236 0.7275 0.4987 0.146 Uiso 1 1 calc R . . H20C H 0.0937 0.6940 0.5238 0.146 Uiso 1 1 calc R . . C21 C 0.31025(19) 0.7130(3) 0.9470(3) 0.0420(12) Uani 1 1 d . . . H21A H 0.3420 0.7085 0.9741 0.050 Uiso 1 1 calc R . . H21B H 0.3030 0.7657 0.9282 0.050 Uiso 1 1 calc R . . C22 C 0.31842(18) 0.6511(4) 1.0486(3) 0.0430(12) Uani 1 1 d . . . H22A H 0.3283 0.6066 1.0338 0.052 Uiso 1 1 calc R . . H22B H 0.2990 0.6306 1.0625 0.052 Uiso 1 1 calc R . . C23 C 0.2692(2) 0.7638(4) 0.9976(3) 0.0466(13) Uani 1 1 d . . . H23A H 0.2585 0.7989 0.9588 0.056 Uiso 1 1 calc R . . H23B H 0.2892 0.7933 1.0384 0.056 Uiso 1 1 calc R . . C24 C 0.3097(2) 0.5501(4) 0.9209(3) 0.0465(13) Uani 1 1 d . . . C25 C 0.2838(2) 0.5018(4) 0.9329(4) 0.0616(18) Uani 1 1 d . . . H25 H 0.2542 0.5141 0.9136 0.074 Uiso 1 1 calc R . . C26 C 0.3004(3) 0.4363(4) 0.9726(4) 0.069(2) Uani 1 1 d . . . H26 H 0.2825 0.4039 0.9802 0.083 Uiso 1 1 calc R . . C27 C 0.3443(3) 0.4189(5) 1.0013(4) 0.076(2) Uani 1 1 d . . . H27 H 0.3561 0.3747 1.0288 0.091 Uiso 1 1 calc R . . C28 C 0.3703(3) 0.4658(5) 0.9898(4) 0.070(2) Uani 1 1 d . . . H28 H 0.3999 0.4533 1.0092 0.084 Uiso 1 1 calc R . . C29 C 0.3534(2) 0.5312(4) 0.9498(3) 0.0548(16) Uani 1 1 d . . . H29 H 0.3714 0.5631 0.9420 0.066 Uiso 1 1 calc R . . C30 C 0.3165(2) 0.6619(4) 0.8336(3) 0.0514(15) Uani 1 1 d . . . C31 C 0.3511(3) 0.7146(5) 0.8576(4) 0.0642(19) Uani 1 1 d . . . H31 H 0.3608 0.7413 0.8984 0.077 Uiso 1 1 calc R . . C32 C 0.3710(3) 0.7273(5) 0.8215(5) 0.078(2) Uani 1 1 d . . . H32 H 0.3942 0.7627 0.8382 0.093 Uiso 1 1 calc R . . C33 C 0.3574(3) 0.6893(5) 0.7614(4) 0.071(2) Uani 1 1 d . . . H33 H 0.3713 0.6987 0.7375 0.086 Uiso 1 1 calc R . . C34 C 0.3232(3) 0.6371(5) 0.7364(4) 0.067(2) Uani 1 1 d . . . H34 H 0.3138 0.6108 0.6955 0.081 Uiso 1 1 calc R . . C35 C 0.3026(2) 0.6238(4) 0.7722(3) 0.0540(15) Uani 1 1 d . . . H35 H 0.2792 0.5888 0.7549 0.065 Uiso 1 1 calc R . . C36 C 0.4001(2) 0.7328(5) 1.0955(3) 0.0554(16) Uani 1 1 d . . . C37 C 0.4272(2) 0.6862(6) 1.0834(3) 0.067(2) Uani 1 1 d . . . H37 H 0.4312 0.6335 1.0957 0.080 Uiso 1 1 calc R . . C38 C 0.4480(3) 0.7179(9) 1.0533(5) 0.093(3) Uani 1 1 d . . . H38 H 0.4666 0.6870 1.0462 0.112 Uiso 1 1 calc R . . C39 C 0.4415(4) 0.7936(10) 1.0339(5) 0.108(5) Uani 1 1 d . . . H39 H 0.4550 0.8141 1.0119 0.130 Uiso 1 1 calc R . . C40 C 0.4160(4) 0.8402(7) 1.0458(5) 0.100(4) Uani 1 1 d . . . H40 H 0.4121 0.8926 1.0324 0.120 Uiso 1 1 calc R . . C41 C 0.3952(3) 0.8107(5) 1.0778(4) 0.069(2) Uani 1 1 d . . . H41 H 0.3782 0.8433 1.0871 0.083 Uiso 1 1 calc R . . C42 C 0.3957(2) 0.6070(4) 1.1743(3) 0.0559(17) Uani 1 1 d . . . C43 C 0.3776(3) 0.5329(4) 1.1576(4) 0.0647(19) Uani 1 1 d . . . H43 H 0.3492 0.5251 1.1207 0.078 Uiso 1 1 calc R . . C44 C 0.4028(3) 0.4704(5) 1.1971(4) 0.081(2) Uani 1 1 d . . . H44 H 0.3914 0.4198 1.1858 0.097 Uiso 1 1 calc R . . C45 C 0.4439(4) 0.4814(7) 1.2521(5) 0.092(3) Uani 1 1 d . . . H45 H 0.4602 0.4381 1.2773 0.111 Uiso 1 1 calc R . . C46 C 0.4615(3) 0.5539(7) 1.2710(5) 0.086(3) Uani 1 1 d . . . H46 H 0.4892 0.5611 1.3099 0.103 Uiso 1 1 calc R . . C47 C 0.4372(3) 0.6179(5) 1.2307(4) 0.068(2) Uani 1 1 d . . . H47 H 0.4491 0.6681 1.2421 0.082 Uiso 1 1 calc R . . C48 C -0.0379(3) 0.9025(7) 0.4100(6) 0.097(3) Uani 1 1 d . . . H48A H -0.0435 0.8968 0.4462 0.146 Uiso 1 1 calc R . . H48B H -0.0263 0.8543 0.4043 0.146 Uiso 1 1 calc R . . H48C H -0.0648 0.9151 0.3683 0.146 Uiso 1 1 calc R . . C49 C -0.0064(4) 0.9651(9) 0.4267(5) 0.103(4) Uani 1 1 d . . . N2 N 0.0199(4) 1.0188(10) 0.4445(7) 0.153(5) Uani 1 1 d . . . Cl2 Cl -0.01463(7) 0.65978(15) 0.39077(12) 0.0826(6) Uani 1 1 d . . . O5 O 0.0070(3) 0.7226(6) 0.4268(7) 0.192(6) Uani 1 1 d . . . O6 O -0.0443(3) 0.6767(8) 0.3236(4) 0.155(4) Uani 1 1 d . . . O7 O 0.0144(4) 0.6056(7) 0.3939(6) 0.170(5) Uani 1 1 d . . . O8 O -0.0399(3) 0.6271(6) 0.4155(5) 0.137(3) Uani 1 1 d . . . Cl1 Cl 0.22171(13) 0.4906(2) 0.56789(19) 0.1205(11) Uani 1 1 d . . . O1 O 0.2006(5) 0.4173(9) 0.5690(11) 0.266(10) Uani 1 1 d . A . O2 O 0.2041(18) 0.5492(14) 0.578(3) 0.20(2) Uani 0.478(11) 1 d P A 1 O3 O 0.2607(17) 0.514(4) 0.616(3) 0.34(4) Uani 0.478(11) 1 d P A 1 O4 O 0.2217(19) 0.487(3) 0.511(2) 0.24(2) Uani 0.478(11) 1 d P A 1 O2A O 0.2319(17) 0.517(3) 0.631(2) 0.208(18) Uani 0.522(11) 1 d P A 2 O3A O 0.2603(13) 0.4740(18) 0.581(3) 0.24(2) Uani 0.522(11) 1 d P A 2 O4A O 0.1859(17) 0.533(3) 0.519(3) 0.38(4) Uani 0.522(11) 1 d P A 2 C50 C 0.0584(7) 0.7533(14) 0.3286(15) 0.122(9) Uiso 0.478(11) 1 d PD A 1 H50A H 0.0467 0.7543 0.2799 0.146 Uiso 0.478(11) 1 calc PR A 1 H50B H 0.0475 0.7070 0.3396 0.146 Uiso 0.478(11) 1 calc PR A 1 Cl3 Cl 0.1159(6) 0.7558(11) 0.3755(10) 0.237(8) Uiso 0.478(11) 1 d PD A 1 Cl4 Cl 0.0452(4) 0.8379(7) 0.3552(6) 0.188(6) Uiso 0.478(11) 1 d PD A 1 C50A C 0.1360(9) 0.695(2) 0.391(2) 0.22(2) Uiso 0.522(11) 1 d PD A 2 H50C H 0.1366 0.6683 0.4285 0.265 Uiso 0.522(11) 1 calc PR A 2 H50D H 0.1346 0.6539 0.3606 0.265 Uiso 0.522(11) 1 calc PR A 2 Cl3A Cl 0.0848(10) 0.740(3) 0.346(2) 0.56(3) Uiso 0.522(11) 1 d PD A 2 Cl4A Cl 0.1875(7) 0.7347(11) 0.4257(10) 0.296(10) Uiso 0.522(11) 1 d PD 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 0.0403(3) 0.0519(3) 0.0445(3) -0.0066(2) 0.0183(2) -0.0033(2) Mo2 0.0422(3) 0.0542(3) 0.0310(3) 0.0013(2) 0.0175(2) 0.0040(2) Cu1 0.0399(4) 0.0596(5) 0.0351(4) -0.0005(3) 0.0151(3) 0.0004(3) Cu2 0.0533(4) 0.0580(5) 0.0387(4) -0.0032(3) 0.0253(3) 0.0027(4) S1 0.0515(9) 0.0558(9) 0.0455(8) 0.0042(7) 0.0257(7) -0.0008(7) S2 0.0473(8) 0.0534(8) 0.0363(7) -0.0014(6) 0.0191(6) -0.0013(7) S3 0.0461(8) 0.0599(9) 0.0374(8) -0.0048(6) 0.0200(6) 0.0031(7) S4 0.0412(8) 0.0619(10) 0.0426(8) -0.0015(7) 0.0186(6) 0.0030(7) P1 0.0411(8) 0.0498(8) 0.0344(7) 0.0019(6) 0.0186(6) 0.0018(6) P2 0.0451(8) 0.0555(9) 0.0355(7) 0.0008(6) 0.0222(6) 0.0024(7) N1 0.045(3) 0.057(3) 0.040(3) 0.006(2) 0.025(2) 0.012(2) C1 0.099(2) 0.083(2) 0.110(3) -0.0238(19) 0.049(2) -0.0234(17) C2 0.099(2) 0.083(2) 0.110(3) -0.0238(19) 0.049(2) -0.0234(17) C3 0.099(2) 0.083(2) 0.110(3) -0.0238(19) 0.049(2) -0.0234(17) C4 0.099(2) 0.083(2) 0.110(3) -0.0238(19) 0.049(2) -0.0234(17) C5 0.099(2) 0.083(2) 0.110(3) -0.0238(19) 0.049(2) -0.0234(17) C6 0.099(2) 0.083(2) 0.110(3) -0.0238(19) 0.049(2) -0.0234(17) C7 0.099(2) 0.083(2) 0.110(3) -0.0238(19) 0.049(2) -0.0234(17) C8 0.099(2) 0.083(2) 0.110(3) -0.0238(19) 0.049(2) -0.0234(17) C9 0.099(2) 0.083(2) 0.110(3) -0.0238(19) 0.049(2) -0.0234(17) C10 0.099(2) 0.083(2) 0.110(3) -0.0238(19) 0.049(2) -0.0234(17) C11 0.057(4) 0.072(4) 0.042(3) 0.017(3) 0.025(3) 0.017(3) C12 0.069(4) 0.063(4) 0.046(4) 0.013(3) 0.036(3) 0.013(3) C13 0.057(4) 0.061(4) 0.050(4) 0.015(3) 0.029(3) 0.005(3) C14 0.066(4) 0.088(5) 0.045(4) 0.028(4) 0.036(3) 0.020(4) C15 0.086(5) 0.080(5) 0.032(3) 0.006(3) 0.032(3) 0.015(4) C16 0.065(5) 0.117(8) 0.058(5) 0.033(5) 0.017(4) 0.030(5) C17 0.137(9) 0.063(5) 0.091(6) 0.013(4) 0.083(7) 0.017(5) C18 0.079(6) 0.099(7) 0.073(6) 0.024(5) 0.038(5) -0.020(5) C19 0.106(7) 0.119(8) 0.108(8) 0.057(6) 0.090(7) 0.058(6) C20 0.150(9) 0.091(6) 0.036(4) -0.007(4) 0.037(5) 0.005(6) C21 0.043(3) 0.047(3) 0.040(3) -0.001(2) 0.024(2) -0.005(2) C22 0.042(3) 0.051(3) 0.039(3) 0.004(2) 0.023(2) 0.001(3) C23 0.047(3) 0.056(3) 0.038(3) 0.000(2) 0.023(3) 0.004(3) C24 0.057(3) 0.046(3) 0.038(3) -0.004(2) 0.026(3) 0.000(3) C25 0.062(4) 0.060(4) 0.054(4) -0.001(3) 0.024(3) 0.001(3) C26 0.096(6) 0.048(4) 0.062(5) 0.006(3) 0.040(4) -0.004(4) C27 0.105(7) 0.056(4) 0.058(5) 0.011(3) 0.038(5) 0.023(4) C28 0.078(5) 0.074(5) 0.055(4) 0.011(4) 0.033(4) 0.028(4) C29 0.061(4) 0.060(4) 0.050(4) 0.001(3) 0.033(3) 0.011(3) C30 0.049(3) 0.058(4) 0.044(3) 0.008(3) 0.023(3) 0.012(3) C31 0.072(5) 0.073(5) 0.062(4) -0.008(4) 0.046(4) -0.015(4) C32 0.091(6) 0.080(5) 0.092(6) -0.004(5) 0.068(5) -0.013(5) C33 0.086(5) 0.080(5) 0.074(5) 0.016(4) 0.059(5) 0.018(5) C34 0.077(5) 0.076(5) 0.059(4) 0.004(4) 0.042(4) 0.020(4) C35 0.059(4) 0.060(4) 0.049(4) 0.002(3) 0.032(3) 0.003(3) C36 0.048(3) 0.077(5) 0.040(3) -0.008(3) 0.022(3) -0.010(3) C37 0.051(4) 0.106(6) 0.047(4) -0.004(4) 0.029(3) 0.004(4) C38 0.052(4) 0.175(12) 0.061(5) -0.014(6) 0.036(4) -0.022(6) C39 0.089(7) 0.192(13) 0.064(6) -0.029(7) 0.053(5) -0.069(8) C40 0.125(8) 0.116(8) 0.067(6) -0.015(5) 0.057(6) -0.065(7) C41 0.084(5) 0.070(5) 0.060(4) -0.020(4) 0.043(4) -0.029(4) C42 0.057(4) 0.074(5) 0.041(3) 0.012(3) 0.029(3) 0.020(3) C43 0.081(5) 0.062(4) 0.055(4) 0.010(3) 0.039(4) 0.017(4) C44 0.108(7) 0.070(5) 0.069(5) 0.019(4) 0.049(5) 0.023(5) C45 0.099(7) 0.112(8) 0.079(6) 0.037(6) 0.055(6) 0.063(7) C46 0.066(5) 0.119(8) 0.068(5) 0.023(5) 0.032(4) 0.033(5) C47 0.060(4) 0.086(5) 0.059(4) 0.009(4) 0.031(4) 0.012(4) C48 0.087(7) 0.099(7) 0.090(7) -0.003(6) 0.035(6) -0.008(6) C49 0.102(8) 0.142(11) 0.060(6) 0.025(6) 0.039(6) 0.047(8) N2 0.116(9) 0.213(15) 0.156(11) 0.039(10) 0.089(9) -0.011(9) Cl2 0.0626(11) 0.0953(16) 0.0729(14) -0.0197(11) 0.0240(10) -0.0074(11) O5 0.131(8) 0.116(7) 0.236(13) -0.064(8) 0.032(9) -0.052(6) O6 0.114(6) 0.259(13) 0.077(5) 0.018(7) 0.039(5) -0.005(8) O7 0.131(8) 0.195(11) 0.176(10) -0.007(8) 0.074(7) 0.073(8) O8 0.153(8) 0.156(8) 0.142(8) -0.013(6) 0.107(7) -0.023(7) Cl1 0.130(3) 0.121(2) 0.121(3) -0.026(2) 0.074(2) 0.021(2) O1 0.230(16) 0.147(11) 0.48(3) -0.129(15) 0.223(19) -0.054(11) O2 0.32(6) 0.089(13) 0.34(6) 0.01(2) 0.29(5) 0.06(2) O3 0.18(4) 0.52(11) 0.16(3) -0.07(5) -0.01(3) -0.13(5) O4 0.38(6) 0.27(4) 0.20(3) -0.12(3) 0.25(4) -0.11(4) O2A 0.27(5) 0.22(3) 0.20(3) -0.12(3) 0.17(4) -0.12(3) O3A 0.20(3) 0.17(2) 0.49(7) 0.01(4) 0.28(5) 0.05(2) O4A 0.32(5) 0.39(7) 0.28(6) 0.05(5) 0.06(4) 0.26(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 2.2476(19) . ? Mo1 C1 2.307(10) . ? Mo1 S4 2.3333(18) . ? Mo1 S3 2.3370(18) . ? Mo1 C2 2.340(11) . ? Mo1 C5 2.347(10) . ? Mo1 C4 2.384(11) . ? Mo1 C3 2.397(11) . ? Mo1 Cu2 2.7350(11) . ? Mo1 Cu1 2.7411(14) . ? Mo1 Mo2 2.8697(9) . ? Mo2 S2 2.2141(18) . ? Mo2 S3 2.3382(18) . ? Mo2 C15 2.339(6) . ? Mo2 S4 2.3398(17) . ? Mo2 C12 2.367(7) . ? Mo2 C14 2.370(6) . ? Mo2 C11 2.372(6) . ? Mo2 C13 2.394(7) . ? Mo2 Cu1 2.7920(13) . ? Mo2 Cu2 2.7929(10) . ? Cu1 P1 2.2128(19) . ? Cu1 S3 2.2574(18) . ? Cu1 S1 2.3420(18) . ? Cu1 S2 2.4093(19) . ? Cu1 Cu2 2.9185(12) . ? Cu2 P2 2.2141(18) 7_567 ? Cu2 S4 2.267(2) . ? Cu2 S1 2.3381(19) . ? Cu2 S2 2.3904(19) . ? P1 C30 1.812(7) . ? P1 C24 1.813(6) . ? P1 C21 1.851(6) . ? P2 C36 1.804(7) . ? P2 C42 1.820(7) . ? P2 C22 1.875(6) . ? P2 Cu2 2.2141(18) 7_567 ? N1 C23 1.447(8) . ? N1 C22 1.453(7) . ? N1 C21 1.457(7) . ? C1 C2 1.364(16) . ? C1 C5 1.465(16) . ? C1 C6 1.496(15) . ? C2 C3 1.345(16) . ? C2 C7 1.588(16) . ? C3 C4 1.412(16) . ? C3 C8 1.517(15) . ? C4 C5 1.383(16) . ? C4 C9 1.546(16) . ? C5 C10 1.508(15) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C15 1.424(10) . ? C11 C12 1.428(11) . ? C11 C16 1.488(10) . ? C12 C13 1.422(10) . ? C12 C17 1.497(11) . ? C13 C14 1.428(11) . ? C13 C18 1.493(11) . ? C14 C15 1.420(12) . ? C14 C19 1.494(11) . ? C15 C20 1.532(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C23 1.530(12) 7_567 ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.387(10) . ? C24 C29 1.392(9) . ? C25 C26 1.379(10) . ? C25 H25 0.9400 . ? C26 C27 1.392(13) . ? C26 H26 0.9400 . ? C27 C28 1.370(13) . ? C27 H27 0.9400 . ? C28 C29 1.382(10) . ? C28 H28 0.9400 . ? C29 H29 0.9400 . ? C30 C35 1.402(9) . ? C30 C31 1.403(10) . ? C31 C32 1.379(10) . ? C31 H31 0.9400 . ? C32 C33 1.379(12) . ? C32 H32 0.9400 . ? C33 C34 1.386(12) . ? C33 H33 0.9400 . ? C34 C35 1.397(10) . ? C34 H34 0.9400 . ? C35 H35 0.9400 . ? C36 C41 1.386(11) . ? C36 C37 1.406(10) . ? C37 C38 1.380(12) . ? C37 H37 0.9400 . ? C38 C39 1.358(18) . ? C38 H38 0.9400 . ? C39 C40 1.357(18) . ? C39 H39 0.9400 . ? C40 C41 1.400(12) . ? C40 H40 0.9400 . ? C41 H41 0.9400 . ? C42 C43 1.392(11) . ? C42 C47 1.394(11) . ? C43 C44 1.397(11) . ? C43 H43 0.9400 . ? C44 C45 1.370(14) . ? C44 H44 0.9400 . ? C45 C46 1.365(16) . ? C45 H45 0.9400 . ? C46 C47 1.413(12) . ? C46 H46 0.9400 . ? C47 H47 0.9400 . ? C48 C49 1.465(18) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 N2 1.232(18) . ? Cl2 O5 1.340(9) . ? Cl2 O7 1.377(9) . ? Cl2 O6 1.383(9) . ? Cl2 O8 1.427(9) . ? Cl1 O2 1.277(19) . ? Cl1 O3A 1.29(2) . ? Cl1 O4 1.32(2) . ? Cl1 O3 1.32(3) . ? Cl1 O2A 1.38(3) . ? Cl1 O4A 1.39(3) . ? Cl1 O1 1.482(16) . ? C50 Cl4 1.742(17) . ? C50 Cl3 1.770(18) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50A Cl4A 1.736(19) . ? C50A Cl3A 1.757(19) . ? C50A H50C 0.9800 . ? C50A H50D 0.9800 . ? 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 C1 140.7(3) . . ? S1 Mo1 S4 105.90(6) . . ? C1 Mo1 S4 93.9(3) . . ? S1 Mo1 S3 105.52(6) . . ? C1 Mo1 S3 103.2(3) . . ? S4 Mo1 S3 101.33(6) . . ? S1 Mo1 C2 111.9(3) . . ? C1 Mo1 C2 34.1(4) . . ? S4 Mo1 C2 87.7(3) . . ? S3 Mo1 C2 137.3(3) . . ? S1 Mo1 C5 120.4(3) . . ? C1 Mo1 C5 36.7(4) . . ? S4 Mo1 C5 129.3(3) . . ? S3 Mo1 C5 85.9(3) . . ? C2 Mo1 C5 58.0(4) . . ? S1 Mo1 C4 88.6(3) . . ? C1 Mo1 C4 57.7(4) . . ? S4 Mo1 C4 143.8(3) . . ? S3 Mo1 C4 106.6(3) . . ? C2 Mo1 C4 56.1(4) . . ? C5 Mo1 C4 34.0(4) . . ? S1 Mo1 C3 84.2(3) . . ? C1 Mo1 C3 56.7(4) . . ? S4 Mo1 C3 112.8(3) . . ? S3 Mo1 C3 140.5(3) . . ? C2 Mo1 C3 33.0(4) . . ? C5 Mo1 C3 57.4(4) . . ? C4 Mo1 C3 34.4(4) . . ? S1 Mo1 Cu2 54.92(5) . . ? C1 Mo1 Cu2 141.2(3) . . ? S4 Mo1 Cu2 52.41(5) . . ? S3 Mo1 Cu2 102.16(5) . . ? C2 Mo1 Cu2 115.7(3) . . ? C5 Mo1 Cu2 171.5(3) . . ? C4 Mo1 Cu2 138.6(3) . . ? C3 Mo1 Cu2 114.1(3) . . ? S1 Mo1 Cu1 54.93(5) . . ? C1 Mo1 Cu1 152.5(3) . . ? S4 Mo1 Cu1 102.31(5) . . ? S3 Mo1 Cu1 52.05(4) . . ? C2 Mo1 Cu1 165.1(3) . . ? C5 Mo1 Cu1 120.0(3) . . ? C4 Mo1 Cu1 113.0(3) . . ? C3 Mo1 Cu1 132.2(3) . . ? Cu2 Mo1 Cu1 64.41(3) . . ? S1 Mo1 Mo2 100.59(5) . . ? C1 Mo1 Mo2 118.2(3) . . ? S4 Mo1 Mo2 52.22(5) . . ? S3 Mo1 Mo2 52.15(5) . . ? C2 Mo1 Mo2 134.4(3) . . ? C5 Mo1 Mo2 128.6(3) . . ? C4 Mo1 Mo2 158.3(3) . . ? C3 Mo1 Mo2 165.0(3) . . ? Cu2 Mo1 Mo2 59.72(3) . . ? Cu1 Mo1 Mo2 59.63(3) . . ? S2 Mo2 S3 105.70(6) . . ? S2 Mo2 C15 140.2(2) . . ? S3 Mo2 C15 90.6(2) . . ? S2 Mo2 S4 105.22(7) . . ? S3 Mo2 S4 101.10(6) . . ? C15 Mo2 S4 106.8(2) . . ? S2 Mo2 C12 93.01(19) . . ? S3 Mo2 C12 145.99(17) . . ? C15 Mo2 C12 58.2(3) . . ? S4 Mo2 C12 100.97(18) . . ? S2 Mo2 C14 107.8(2) . . ? S3 Mo2 C14 88.8(2) . . ? C15 Mo2 C14 35.1(3) . . ? S4 Mo2 C14 141.33(19) . . ? C12 Mo2 C14 58.1(3) . . ? S2 Mo2 C11 127.6(2) . . ? S3 Mo2 C11 122.59(19) . . ? C15 Mo2 C11 35.2(3) . . ? S4 Mo2 C11 85.47(18) . . ? C12 Mo2 C11 35.1(3) . . ? C14 Mo2 C11 58.5(2) . . ? S2 Mo2 C13 82.51(18) . . ? S3 Mo2 C13 119.01(18) . . ? C15 Mo2 C13 58.1(3) . . ? S4 Mo2 C13 135.69(17) . . ? C12 Mo2 C13 34.7(2) . . ? C14 Mo2 C13 34.9(3) . . ? C11 Mo2 C13 58.1(2) . . ? S2 Mo2 Cu1 56.12(5) . . ? S3 Mo2 Cu1 51.28(4) . . ? C15 Mo2 Cu1 136.8(2) . . ? S4 Mo2 Cu1 100.65(5) . . ? C12 Mo2 Cu1 146.12(19) . . ? C14 Mo2 Cu1 114.18(17) . . ? C11 Mo2 Cu1 171.89(17) . . ? C13 Mo2 Cu1 118.44(17) . . ? S2 Mo2 Cu2 55.59(5) . . ? S3 Mo2 Cu2 100.44(5) . . ? C15 Mo2 Cu2 157.1(2) . . ? S4 Mo2 Cu2 51.49(5) . . ? C12 Mo2 Cu2 113.55(16) . . ? C14 Mo2 Cu2 162.6(2) . . ? C11 Mo2 Cu2 125.07(17) . . ? C13 Mo2 Cu2 129.32(18) . . ? Cu1 Mo2 Cu2 63.01(3) . . ? S2 Mo2 Mo1 100.16(5) . . ? S3 Mo2 Mo1 52.12(5) . . ? C15 Mo2 Mo1 118.0(2) . . ? S4 Mo2 Mo1 52.01(5) . . ? C12 Mo2 Mo1 152.19(18) . . ? C14 Mo2 Mo1 137.1(2) . . ? C11 Mo2 Mo1 124.23(19) . . ? C13 Mo2 Mo1 171.10(18) . . ? Cu1 Mo2 Mo1 57.89(3) . . ? Cu2 Mo2 Mo1 57.74(2) . . ? P1 Cu1 S3 121.15(7) . . ? P1 Cu1 S1 121.25(7) . . ? S3 Cu1 S1 105.04(7) . . ? P1 Cu1 S2 102.24(6) . . ? S3 Cu1 S2 102.05(6) . . ? S1 Cu1 S2 101.27(6) . . ? P1 Cu1 Mo1 158.72(6) . . ? S3 Cu1 Mo1 54.72(5) . . ? S1 Cu1 Mo1 51.76(5) . . ? S2 Cu1 Mo1 98.98(5) . . ? P1 Cu1 Mo2 135.07(6) . . ? S3 Cu1 Mo2 53.92(5) . . ? S1 Cu1 Mo2 100.48(5) . . ? S2 Cu1 Mo2 49.72(4) . . ? Mo1 Cu1 Mo2 62.48(3) . . ? P1 Cu1 Cu2 137.72(5) . . ? S3 Cu1 Cu2 98.82(6) . . ? S1 Cu1 Cu2 51.36(5) . . ? S2 Cu1 Cu2 52.26(4) . . ? Mo1 Cu1 Cu2 57.69(3) . . ? Mo2 Cu1 Cu2 58.51(3) . . ? P2 Cu2 S4 118.75(7) 7_567 . ? P2 Cu2 S1 121.26(7) 7_567 . ? S4 Cu2 S1 105.12(7) . . ? P2 Cu2 S2 104.71(7) 7_567 . ? S4 Cu2 S2 101.96(7) . . ? S1 Cu2 S2 101.96(7) . . ? P2 Cu2 Mo1 155.66(6) 7_567 . ? S4 Cu2 Mo1 54.65(5) . . ? S1 Cu2 Mo1 51.88(5) . . ? S2 Cu2 Mo1 99.62(5) . . ? P2 Cu2 Mo2 136.22(6) 7_567 . ? S4 Cu2 Mo2 53.88(5) . . ? S1 Cu2 Mo2 100.55(5) . . ? S2 Cu2 Mo2 49.83(5) . . ? Mo1 Cu2 Mo2 62.54(2) . . ? P2 Cu2 Cu1 140.70(6) 7_567 . ? S4 Cu2 Cu1 98.82(6) . . ? S1 Cu2 Cu1 51.48(5) . . ? S2 Cu2 Cu1 52.85(5) . . ? Mo1 Cu2 Cu1 57.90(3) . . ? Mo2 Cu2 Cu1 58.48(3) . . ? Mo1 S1 Cu2 73.20(5) . . ? Mo1 S1 Cu1 73.31(6) . . ? Cu2 S1 Cu1 77.16(6) . . ? Mo2 S2 Cu2 74.57(6) . . ? Mo2 S2 Cu1 74.16(5) . . ? Cu2 S2 Cu1 74.90(5) . . ? Cu1 S3 Mo1 73.23(6) . . ? Cu1 S3 Mo2 74.80(6) . . ? Mo1 S3 Mo2 75.73(5) . . ? Cu2 S4 Mo1 72.95(6) . . ? Cu2 S4 Mo2 74.63(6) . . ? Mo1 S4 Mo2 75.77(5) . . ? C30 P1 C24 106.2(3) . . ? C30 P1 C21 104.6(3) . . ? C24 P1 C21 102.9(3) . . ? C30 P1 Cu1 113.5(2) . . ? C24 P1 Cu1 116.4(2) . . ? C21 P1 Cu1 112.2(2) . . ? C36 P2 C42 106.0(3) . . ? C36 P2 C22 104.9(3) . . ? C42 P2 C22 102.8(3) . . ? C36 P2 Cu2 115.7(3) . 7_567 ? C42 P2 Cu2 109.2(2) . 7_567 ? C22 P2 Cu2 117.0(2) . 7_567 ? C23 N1 C22 117.1(5) . . ? C23 N1 C21 117.8(5) . . ? C22 N1 C21 115.7(5) . . ? C2 C1 C5 106.7(12) . . ? C2 C1 C6 125.9(12) . . ? C5 C1 C6 126.8(11) . . ? C2 C1 Mo1 74.3(7) . . ? C5 C1 Mo1 73.2(6) . . ? C6 C1 Mo1 124.3(7) . . ? C3 C2 C1 111.3(12) . . ? C3 C2 C7 121.1(12) . . ? C1 C2 C7 127.4(12) . . ? C3 C2 Mo1 75.9(7) . . ? C1 C2 Mo1 71.6(7) . . ? C7 C2 Mo1 123.8(7) . . ? C2 C3 C4 107.4(12) . . ? C2 C3 C8 129.2(12) . . ? C4 C3 C8 123.2(12) . . ? C2 C3 Mo1 71.2(7) . . ? C4 C3 Mo1 72.3(7) . . ? C8 C3 Mo1 125.5(7) . . ? C5 C4 C3 109.3(12) . . ? C5 C4 C9 126.0(11) . . ? C3 C4 C9 124.7(12) . . ? C5 C4 Mo1 71.6(6) . . ? C3 C4 Mo1 73.3(7) . . ? C9 C4 Mo1 122.6(7) . . ? C4 C5 C1 105.3(11) . . ? C4 C5 C10 127.6(12) . . ? C1 C5 C10 126.7(11) . . ? C4 C5 Mo1 74.4(6) . . ? C1 C5 Mo1 70.2(6) . . ? C10 C5 Mo1 125.6(7) . . ? 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 106.9(6) . . ? C15 C11 C16 127.2(8) . . ? C12 C11 C16 125.6(7) . . ? C15 C11 Mo2 71.2(4) . . ? C12 C11 Mo2 72.3(4) . . ? C16 C11 Mo2 126.5(5) . . ? C13 C12 C11 108.7(6) . . ? C13 C12 C17 125.2(8) . . ? C11 C12 C17 126.0(7) . . ? C13 C12 Mo2 73.7(4) . . ? C11 C12 Mo2 72.6(4) . . ? C17 C12 Mo2 122.8(5) . . ? C12 C13 C14 107.8(7) . . ? C12 C13 C18 126.3(8) . . ? C14 C13 C18 125.8(7) . . ? C12 C13 Mo2 71.6(4) . . ? C14 C13 Mo2 71.6(4) . . ? C18 C13 Mo2 125.9(5) . . ? C15 C14 C13 107.6(6) . . ? C15 C14 C19 126.0(9) . . ? C13 C14 C19 126.2(9) . . ? C15 C14 Mo2 71.3(4) . . ? C13 C14 Mo2 73.5(4) . . ? C19 C14 Mo2 124.5(5) . . ? C14 C15 C11 109.0(7) . . ? C14 C15 C20 124.7(8) . . ? C11 C15 C20 125.9(8) . . ? C14 C15 Mo2 73.6(4) . . ? C11 C15 Mo2 73.6(4) . . ? C20 C15 Mo2 124.3(6) . . ? 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 . . ? N1 C21 P1 111.2(4) . . ? N1 C21 H21A 109.4 . . ? P1 C21 H21A 109.4 . . ? N1 C21 H21B 109.4 . . ? P1 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? N1 C22 P2 119.1(4) . . ? N1 C22 H22A 107.5 . . ? P2 C22 H22A 107.5 . . ? N1 C22 H22B 107.5 . . ? P2 C22 H22B 107.5 . . ? H22A C22 H22B 107.0 . . ? N1 C23 C23 112.8(7) . 7_567 ? N1 C23 H23A 109.0 . . ? C23 C23 H23A 109.0 7_567 . ? N1 C23 H23B 109.0 . . ? C23 C23 H23B 109.0 7_567 . ? H23A C23 H23B 107.8 . . ? C25 C24 C29 118.6(6) . . ? C25 C24 P1 119.8(5) . . ? C29 C24 P1 121.2(5) . . ? C26 C25 C24 121.4(7) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 118.8(8) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C28 C27 C26 120.6(7) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 120.2(8) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C24 120.3(7) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? C35 C30 C31 118.3(6) . . ? C35 C30 P1 118.2(5) . . ? C31 C30 P1 123.4(5) . . ? C32 C31 C30 120.1(7) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C33 C32 C31 121.3(8) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 119.8(7) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C33 C34 C35 119.6(7) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C30 120.8(7) . . ? C34 C35 H35 119.6 . . ? C30 C35 H35 119.6 . . ? C41 C36 C37 118.9(7) . . ? C41 C36 P2 118.4(6) . . ? C37 C36 P2 122.4(6) . . ? C38 C37 C36 120.0(10) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C39 C38 C37 120.2(10) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C40 C39 C38 121.0(9) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C39 C40 C41 120.5(11) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C36 C41 C40 119.3(9) . . ? C36 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C43 C42 C47 120.1(7) . . ? C43 C42 P2 122.8(6) . . ? C47 C42 P2 117.0(6) . . ? C42 C43 C44 118.2(8) . . ? C42 C43 H43 120.9 . . ? C44 C43 H43 120.9 . . ? C45 C44 C43 121.4(10) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C46 C45 C44 121.4(9) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C45 C46 C47 118.4(9) . . ? C45 C46 H46 120.8 . . ? C47 C46 H46 120.8 . . ? C42 C47 C46 120.4(9) . . ? C42 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C49 C48 H48A 109.5 . . ? C49 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C49 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N2 C49 C48 175.6(13) . . ? O5 Cl2 O7 109.5(8) . . ? O5 Cl2 O6 112.8(8) . . ? O7 Cl2 O6 108.7(7) . . ? O5 Cl2 O8 110.7(8) . . ? O7 Cl2 O8 110.1(8) . . ? O6 Cl2 O8 104.8(6) . . ? O2 Cl1 O3A 135(3) . . ? O2 Cl1 O4 119(3) . . ? O3A Cl1 O4 70(2) . . ? O2 Cl1 O3 91(4) . . ? O3A Cl1 O3 48(3) . . ? O4 Cl1 O3 108(3) . . ? O2 Cl1 O2A 56(2) . . ? O3A Cl1 O2A 100(3) . . ? O4 Cl1 O2A 159(2) . . ? O3 Cl1 O2A 55(3) . . ? O2 Cl1 O4A 53(2) . . ? O3A Cl1 O4A 137(3) . . ? O4 Cl1 O4A 73(3) . . ? O3 Cl1 O4A 131(4) . . ? O2A Cl1 O4A 108(3) . . ? O2 Cl1 O1 111.0(17) . . ? O3A Cl1 O1 108.0(16) . . ? O4 Cl1 O1 104.3(17) . . ? O3 Cl1 O1 125(3) . . ? O2A Cl1 O1 96.4(17) . . ? O4A Cl1 O1 101(3) . . ? Cl4 C50 Cl3 102.3(13) . . ? Cl4 C50 H50A 111.3 . . ? Cl3 C50 H50A 111.3 . . ? Cl4 C50 H50B 111.3 . . ? Cl3 C50 H50B 111.3 . . ? H50A C50 H50B 109.2 . . ? Cl4A C50A Cl3A 130(3) . . ? Cl4A C50A H50C 104.8 . . ? Cl3A C50A H50C 104.8 . . ? Cl4A C50A H50D 104.8 . . ? Cl3A C50A H50D 104.8 . . ? H50C C50A H50D 105.8 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.340 _refine_diff_density_min -1.127 _refine_diff_density_rms 0.117 #===END #============================================================================== data_5^.^3MeCN^.^0.5CH~2~Cl~2~ _database_code_depnum_ccdc_archive 'CCDC 783844' #TrackingRef '- JPLangCIF.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C102 H116 Cu4 Mo4 N4 P4 S8), 8(Cl O4), 6(C2 H3 N), C H2 Cl2' _chemical_formula_sum 'C108.50 H126 Cl5 Cu4 Mo4 N7 O16 P4 S8' _chemical_formula_weight 2979.69 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 c' _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 11.882(2) _cell_length_b 25.205(5) _cell_length_c 20.961(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.50(3) _cell_angle_gamma 90.00 _cell_volume 6191(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7406 _cell_measurement_theta_min 3.3256 _cell_measurement_theta_max 27.4894 _exptl_crystal_description prism _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3022 _exptl_absorpt_coefficient_mu 1.421 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7089 _exptl_absorpt_correction_T_max 0.8594 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 31212 _diffrn_reflns_av_R_equivalents 0.0948 _diffrn_reflns_av_sigmaI/netI 0.1458 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 17313 _reflns_number_gt 13080 _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^)+(0.0571P)^2^+24.4702P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00074(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.13(3) _refine_ls_number_reflns 17313 _refine_ls_number_parameters 1380 _refine_ls_number_restraints 752 _refine_ls_R_factor_all 0.1211 _refine_ls_R_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.2091 _refine_ls_wR_factor_gt 0.1861 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.071 _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 0.87188(13) 0.26768(6) 1.05623(7) 0.0321(4) Uani 1 1 d . . . Mo2 Mo 0.63129(13) 0.25373(6) 1.01633(7) 0.0327(4) Uani 1 1 d . . . Mo3 Mo 0.89783(13) 0.23314(6) 0.51640(7) 0.0319(4) Uani 1 1 d . . . Mo4 Mo 0.65513(13) 0.24523(6) 0.48576(7) 0.0334(4) Uani 1 1 d . . . Cu1 Cu 0.78652(19) 0.21096(8) 0.94518(10) 0.0369(5) Uani 1 1 d . . . Cu2 Cu 0.75286(19) 0.32706(8) 0.95574(9) 0.0339(5) Uani 1 1 d . . . Cu3 Cu 0.7546(2) 0.17285(8) 0.57827(10) 0.0369(5) Uani 1 1 d . . . Cu4 Cu 0.77632(19) 0.29030(8) 0.59589(10) 0.0356(5) Uani 1 1 d . . . S1 S 0.9261(4) 0.27831(17) 0.9597(2) 0.0376(11) Uani 1 1 d . . . S2 S 0.6197(5) 0.26197(17) 0.9094(2) 0.0387(11) Uani 1 1 d . . . S3 S 0.7682(4) 0.18840(16) 1.0468(2) 0.0332(10) Uani 1 1 d . . . S4 S 0.7267(4) 0.32967(16) 1.0602(2) 0.0329(10) Uani 1 1 d . . . S5 S 0.9132(4) 0.22325(18) 0.6237(2) 0.0388(11) Uani 1 1 d . . . S6 S 0.6090(4) 0.23747(17) 0.5844(2) 0.0348(11) Uani 1 1 d . . . S7 S 0.7632(4) 0.17081(17) 0.4712(2) 0.0350(10) Uani 1 1 d . . . S8 S 0.7945(4) 0.31178(18) 0.4934(2) 0.0391(11) Uani 1 1 d . . . P1 P 0.7964(4) 0.14616(17) 0.8743(2) 0.0355(11) Uani 1 1 d . . . P2 P 0.7159(5) 0.09717(17) 0.6243(2) 0.0386(11) Uani 1 1 d . . . P3 P 0.7253(4) 0.40422(17) 0.9040(2) 0.0361(11) Uani 1 1 d . . . P4 P 0.7659(4) 0.35487(18) 0.6655(2) 0.0394(12) Uani 1 1 d . . . N1 N 0.8285(13) 0.1332(6) 0.7443(7) 0.045(4) Uani 1 1 d . . . N2 N 0.9577(17) 0.0826(7) 0.7025(8) 0.064(4) Uani 1 1 d U . . N3 N 0.8142(12) 0.3579(5) 0.8027(6) 0.031(3) Uani 1 1 d . . . N4 N 0.9767(16) 0.3035(7) 0.7943(8) 0.062(4) Uani 1 1 d U . . C1 C 0.9718(18) 0.2299(7) 1.1510(8) 0.043(3) Uani 1 1 d U . . C2 C 1.0512(16) 0.2381(7) 1.1083(8) 0.041(3) Uani 1 1 d U . . C3 C 1.0637(16) 0.2911(7) 1.0988(8) 0.039(3) Uani 1 1 d U . . C4 C 0.9906(15) 0.3188(7) 1.1339(8) 0.037(3) Uani 1 1 d U . . C5 C 0.9342(16) 0.2808(7) 1.1672(8) 0.039(3) Uani 1 1 d U . . C6 C 0.947(2) 0.1782(7) 1.1845(8) 0.059(5) Uani 1 1 d U . . H6A H 0.9477 0.1484 1.1545 0.089 Uiso 1 1 calc R . . H6B H 0.8715 0.1805 1.1977 0.089 Uiso 1 1 calc R . . H6C H 1.0051 0.1726 1.2228 0.089 Uiso 1 1 calc R . . C7 C 1.1257(18) 0.1940(8) 1.0846(10) 0.059(5) Uani 1 1 d U . . H7A H 1.1386 0.2023 1.0407 0.088 Uiso 1 1 calc R . . H7B H 1.0864 0.1598 1.0845 0.088 Uiso 1 1 calc R . . H7C H 1.1992 0.1921 1.1137 0.088 Uiso 1 1 calc R . . C8 C 1.150(2) 0.3167(9) 1.0628(12) 0.068(6) Uani 1 1 d U . . H8A H 1.2188 0.3255 1.0933 0.102 Uiso 1 1 calc R . . H8B H 1.1170 0.3492 1.0416 0.102 Uiso 1 1 calc R . . H8C H 1.1690 0.2920 1.0301 0.102 Uiso 1 1 calc R . . C9 C 0.9862(18) 0.3783(7) 1.1438(9) 0.052(5) Uani 1 1 d U . . H9A H 1.0344 0.3878 1.1847 0.078 Uiso 1 1 calc R . . H9B H 0.9073 0.3891 1.1449 0.078 Uiso 1 1 calc R . . H9C H 1.0140 0.3964 1.1080 0.078 Uiso 1 1 calc R . . C10 C 0.8612(17) 0.2930(8) 1.2155(8) 0.050(5) Uani 1 1 d U . . H10A H 0.9088 0.3050 1.2556 0.076 Uiso 1 1 calc R . . H10B H 0.8191 0.2611 1.2241 0.076 Uiso 1 1 calc R . . H10C H 0.8072 0.3211 1.1989 0.076 Uiso 1 1 calc R . . C11 C 0.5244(16) 0.2198(7) 1.0911(8) 0.037(4) Uani 1 1 d . . . C12 C 0.4851(15) 0.1947(6) 1.0310(9) 0.037(4) Uani 1 1 d . . . C13 C 0.4325(16) 0.2355(8) 0.9888(8) 0.042(5) Uani 1 1 d . . . C14 C 0.4440(19) 0.2838(7) 1.0216(9) 0.049(5) Uani 1 1 d . . . C15 C 0.4976(16) 0.2745(8) 1.0879(9) 0.043(5) Uani 1 1 d . . . C16 C 0.5742(19) 0.1919(7) 1.1555(9) 0.052(5) Uani 1 1 d . . . H16A H 0.6375 0.2130 1.1784 0.078 Uiso 1 1 calc R . . H16B H 0.6019 0.1566 1.1463 0.078 Uiso 1 1 calc R . . H16C H 0.5146 0.1886 1.1825 0.078 Uiso 1 1 calc R . . C17 C 0.4871(17) 0.1348(7) 1.0204(9) 0.053(5) Uani 1 1 d U . . H17A H 0.4654 0.1270 0.9742 0.079 Uiso 1 1 calc R . . H17B H 0.4331 0.1176 1.0445 0.079 Uiso 1 1 calc R . . H17C H 0.5642 0.1212 1.0357 0.079 Uiso 1 1 calc R . . C18 C 0.3709(16) 0.2220(7) 0.9210(8) 0.048(5) Uani 1 1 d U . . H18A H 0.3788 0.1840 0.9129 0.072 Uiso 1 1 calc R . . H18B H 0.4044 0.2425 0.8890 0.072 Uiso 1 1 calc R . . H18C H 0.2898 0.2310 0.9175 0.072 Uiso 1 1 calc R . . C19 C 0.408(2) 0.3347(8) 0.9925(9) 0.065(6) Uani 1 1 d . . . H19A H 0.4456 0.3409 0.9549 0.097 Uiso 1 1 calc R . . H19B H 0.4286 0.3630 1.0243 0.097 Uiso 1 1 calc R . . H19C H 0.3250 0.3345 0.9786 0.097 Uiso 1 1 calc R . . C20 C 0.5099(15) 0.3151(7) 1.1383(8) 0.041(4) Uani 1 1 d . . . H20A H 0.4470 0.3121 1.1630 0.061 Uiso 1 1 calc R . . H20B H 0.5084 0.3504 1.1184 0.061 Uiso 1 1 calc R . . H20C H 0.5827 0.3102 1.1674 0.061 Uiso 1 1 calc R . . C21 C 1.0480(17) 0.1816(7) 0.4835(9) 0.045(5) Uani 1 1 d . . . C22 C 1.0036(16) 0.2172(8) 0.4318(8) 0.043(5) Uani 1 1 d . . . C23 C 1.0265(16) 0.2707(7) 0.4529(10) 0.043(5) Uani 1 1 d U . . C24 C 1.0865(18) 0.2667(8) 0.5183(9) 0.053(6) Uani 1 1 d . . . C25 C 1.0992(16) 0.2131(7) 0.5374(9) 0.043(5) Uani 1 1 d . . . C26 C 1.0480(17) 0.1245(6) 0.4790(9) 0.050(5) Uani 1 1 d . . . H26A H 1.1225 0.1123 0.4706 0.075 Uiso 1 1 calc R . . H26B H 0.9885 0.1131 0.4435 0.075 Uiso 1 1 calc R . . H26C H 1.0328 0.1092 0.5197 0.075 Uiso 1 1 calc R . . C27 C 0.9559(17) 0.2000(7) 0.3657(8) 0.047(5) Uani 1 1 d . . . H27A H 0.8888 0.2216 0.3491 0.071 Uiso 1 1 calc R . . H27B H 0.9335 0.1626 0.3663 0.071 Uiso 1 1 calc R . . H27C H 1.0135 0.2044 0.3376 0.071 Uiso 1 1 calc R . . C28 C 1.0054(19) 0.3192(7) 0.4116(10) 0.057(6) Uani 1 1 d . . . H28A H 0.9967 0.3500 0.4389 0.085 Uiso 1 1 calc R . . H28B H 0.9357 0.3143 0.3800 0.085 Uiso 1 1 calc R . . H28C H 1.0702 0.3249 0.3889 0.085 Uiso 1 1 calc R . . C29 C 1.1334(18) 0.3131(9) 0.5579(10) 0.066(6) Uani 1 1 d . . . H29A H 1.1675 0.3011 0.6012 0.099 Uiso 1 1 calc R . . H29B H 1.0718 0.3383 0.5612 0.099 Uiso 1 1 calc R . . H29C H 1.1919 0.3305 0.5372 0.099 Uiso 1 1 calc R . . C30 C 1.159(2) 0.1945(9) 0.5983(10) 0.071(7) Uani 1 1 d . . . H30A H 1.2341 0.1807 0.5925 0.106 Uiso 1 1 calc R . . H30B H 1.1152 0.1661 0.6146 0.106 Uiso 1 1 calc R . . H30C H 1.1695 0.2238 0.6294 0.106 Uiso 1 1 calc R . . C31 C 0.5444(19) 0.3045(8) 0.4138(9) 0.058(4) Uani 1 1 d U . . C32 C 0.469(2) 0.2854(10) 0.4539(9) 0.065(4) Uani 1 1 d U . . C33 C 0.459(2) 0.2283(10) 0.4474(9) 0.061(4) Uani 1 1 d U . . C34 C 0.5244(17) 0.2120(7) 0.3972(8) 0.046(3) Uani 1 1 d U . . C35 C 0.5757(19) 0.2588(8) 0.3786(9) 0.048(4) Uani 1 1 d U . . C36 C 0.567(2) 0.3606(8) 0.4014(10) 0.072(6) Uani 1 1 d U . . H36A H 0.4993 0.3765 0.3755 0.108 Uiso 1 1 calc R . . H36B H 0.6317 0.3631 0.3779 0.108 Uiso 1 1 calc R . . H36C H 0.5854 0.3795 0.4427 0.108 Uiso 1 1 calc R . . C37 C 0.406(2) 0.3169(11) 0.4984(11) 0.097(8) Uani 1 1 d U . . H37A H 0.4299 0.3541 0.4983 0.145 Uiso 1 1 calc R . . H37B H 0.4250 0.3026 0.5424 0.145 Uiso 1 1 calc R . . H37C H 0.3241 0.3142 0.4834 0.145 Uiso 1 1 calc R . . C38 C 0.380(2) 0.1909(12) 0.4780(11) 0.091(8) Uani 1 1 d U . . H38A H 0.3897 0.1972 0.5247 0.137 Uiso 1 1 calc R . . H38B H 0.3985 0.1540 0.4698 0.137 Uiso 1 1 calc R . . H38C H 0.3000 0.1979 0.4588 0.137 Uiso 1 1 calc R . . C39 C 0.5224(19) 0.1593(8) 0.3658(10) 0.062(5) Uani 1 1 d U . . H39A H 0.4612 0.1585 0.3282 0.093 Uiso 1 1 calc R . . H39B H 0.5087 0.1318 0.3966 0.093 Uiso 1 1 calc R . . H39C H 0.5958 0.1529 0.3517 0.093 Uiso 1 1 calc R . . C40 C 0.6469(19) 0.2613(9) 0.3231(8) 0.061(5) Uani 1 1 d U . . H40A H 0.6791 0.2262 0.3172 0.092 Uiso 1 1 calc R . . H40B H 0.7089 0.2871 0.3341 0.092 Uiso 1 1 calc R . . H40C H 0.5978 0.2722 0.2830 0.092 Uiso 1 1 calc R . . C41 C 0.7982(17) 0.1720(6) 0.7924(8) 0.041(5) Uani 1 1 d U . . H41A H 0.7218 0.1867 0.7756 0.050 Uiso 1 1 calc R . . H41B H 0.8533 0.2018 0.7957 0.050 Uiso 1 1 calc R . . C42 C 0.7417(17) 0.0979(7) 0.7146(8) 0.042(5) Uani 1 1 d U . . H42A H 0.6694 0.1073 0.7294 0.050 Uiso 1 1 calc R . . H42B H 0.7622 0.0615 0.7301 0.050 Uiso 1 1 calc R . . C43 C 0.9407(19) 0.1251(8) 0.7401(8) 0.051(4) Uani 1 1 d U . . C44 C 1.0339(18) 0.1512(8) 0.7719(9) 0.056(4) Uani 1 1 d U . . H44 H 1.0215 0.1806 0.7983 0.067 Uiso 1 1 calc R . . C45 C 1.142(2) 0.1378(10) 0.7683(10) 0.072(5) Uani 1 1 d U . . H45 H 1.2062 0.1564 0.7910 0.086 Uiso 1 1 calc R . . C46 C 1.154(2) 0.0931(11) 0.7273(11) 0.080(5) Uani 1 1 d U . . H46 H 1.2277 0.0818 0.7217 0.096 Uiso 1 1 calc R . . C47 C 1.059(2) 0.0662(11) 0.6957(11) 0.081(5) Uani 1 1 d U . . H47 H 1.0684 0.0362 0.6695 0.097 Uiso 1 1 calc R . . C48 C 0.9183(16) 0.1052(6) 0.8926(8) 0.034(3) Uani 1 1 d U . . C49 C 1.0152(15) 0.1238(7) 0.9369(8) 0.038(3) Uani 1 1 d U . . H49 H 1.0108 0.1569 0.9583 0.046 Uiso 1 1 calc R . . C50 C 1.1145(17) 0.0948(7) 0.9492(9) 0.047(4) Uani 1 1 d U . . H50 H 1.1774 0.1078 0.9790 0.056 Uiso 1 1 calc R . . C51 C 1.1240(18) 0.0459(7) 0.9179(9) 0.051(4) Uani 1 1 d U . . H51 H 1.1930 0.0262 0.9263 0.062 Uiso 1 1 calc R . . C52 C 1.0335(17) 0.0270(7) 0.8754(8) 0.044(4) Uani 1 1 d U . . H52 H 1.0391 -0.0061 0.8545 0.053 Uiso 1 1 calc R . . C53 C 0.9338(16) 0.0560(6) 0.8627(7) 0.036(3) Uani 1 1 d U . . H53 H 0.8725 0.0422 0.8324 0.043 Uiso 1 1 calc R . . C54 C 0.6725(16) 0.1035(7) 0.8663(8) 0.037(3) Uani 1 1 d U . . C55 C 0.6717(17) 0.0526(7) 0.8949(8) 0.044(3) Uani 1 1 d U . . H55 H 0.7413 0.0378 0.9163 0.053 Uiso 1 1 calc R . . C56 C 0.5733(18) 0.0245(7) 0.8924(9) 0.052(4) Uani 1 1 d U . . H56 H 0.5745 -0.0091 0.9129 0.062 Uiso 1 1 calc R . . C57 C 0.4734(19) 0.0445(8) 0.8606(9) 0.055(4) Uani 1 1 d U . . H57 H 0.4062 0.0236 0.8565 0.066 Uiso 1 1 calc R . . C58 C 0.4683(19) 0.0951(8) 0.8340(9) 0.056(4) Uani 1 1 d U . . H58 H 0.3971 0.1091 0.8136 0.067 Uiso 1 1 calc R . . C59 C 0.5649(17) 0.1248(7) 0.8372(8) 0.045(4) Uani 1 1 d U . . H59 H 0.5607 0.1597 0.8199 0.053 Uiso 1 1 calc R . . C60 C 0.7790(16) 0.0374(6) 0.6004(8) 0.036(4) Uani 1 1 d . . . C61 C 0.762(2) -0.0090(8) 0.6280(9) 0.063(7) Uani 1 1 d . . . H61 H 0.7148 -0.0105 0.6604 0.075 Uiso 1 1 calc R . . C62 C 0.8145(19) -0.0567(7) 0.6096(8) 0.055(6) Uani 1 1 d . . . H62 H 0.8013 -0.0896 0.6292 0.066 Uiso 1 1 calc R . . C63 C 0.8836(17) -0.0543(8) 0.5634(9) 0.050(5) Uani 1 1 d U . . H63 H 0.9225 -0.0855 0.5536 0.060 Uiso 1 1 calc R . . C64 C 0.8989(15) -0.0063(6) 0.5296(8) 0.041(4) Uani 1 1 d . . . H64 H 0.9432 -0.0050 0.4959 0.049 Uiso 1 1 calc R . . C65 C 0.8434(17) 0.0398(7) 0.5496(8) 0.049(5) Uani 1 1 d . . . H65 H 0.8500 0.0726 0.5283 0.059 Uiso 1 1 calc R . . C66 C 0.5651(15) 0.0807(6) 0.6054(8) 0.046(4) Uani 1 1 d DU . . C67 C 0.4879(15) 0.1076(8) 0.6358(11) 0.064(4) Uani 1 1 d DU . . H67 H 0.5117 0.1349 0.6663 0.077 Uiso 1 1 calc R . . C68 C 0.3733(17) 0.0931(9) 0.6201(11) 0.076(5) Uani 1 1 d DU . . H68 H 0.3213 0.1087 0.6446 0.092 Uiso 1 1 calc R . . C69 C 0.329(2) 0.0576(8) 0.5714(11) 0.080(5) Uani 1 1 d DU . . H69 H 0.2496 0.0505 0.5605 0.097 Uiso 1 1 calc R . . C70 C 0.4074(16) 0.0337(9) 0.5407(12) 0.077(5) Uani 1 1 d DU . . H70 H 0.3831 0.0087 0.5074 0.092 Uiso 1 1 calc R . . C71 C 0.5217(17) 0.0452(8) 0.5571(9) 0.062(4) Uani 1 1 d DU . . H71 H 0.5736 0.0278 0.5342 0.074 Uiso 1 1 calc R . . C72 C 0.7697(15) 0.4066(6) 0.8225(8) 0.032(4) Uani 1 1 d U . . H72A H 0.7029 0.4169 0.7901 0.038 Uiso 1 1 calc R . . H72B H 0.8283 0.4346 0.8228 0.038 Uiso 1 1 calc R . . C73 C 0.7547(15) 0.3268(6) 0.7494(7) 0.033(4) Uani 1 1 d . . . H73A H 0.6731 0.3246 0.7536 0.039 Uiso 1 1 calc R . . H73B H 0.7859 0.2903 0.7525 0.039 Uiso 1 1 calc R . . C74 C 0.9316(18) 0.3483(7) 0.8219(8) 0.044(4) Uani 1 1 d U . . C75 C 0.9967(19) 0.3801(7) 0.8651(9) 0.053(4) Uani 1 1 d U . . H75 H 0.9642 0.4094 0.8841 0.064 Uiso 1 1 calc R . . C76 C 1.111(2) 0.3689(9) 0.8808(10) 0.065(4) Uani 1 1 d U . . H76 H 1.1570 0.3906 0.9118 0.078 Uiso 1 1 calc R . . C77 C 1.163(2) 0.3268(9) 0.8531(12) 0.075(5) Uani 1 1 d U . . H77 H 1.2427 0.3199 0.8619 0.090 Uiso 1 1 calc R . . C78 C 1.085(2) 0.2961(9) 0.8110(12) 0.069(5) Uani 1 1 d U . . H78 H 1.1161 0.2661 0.7925 0.083 Uiso 1 1 calc R . . C79 C 0.7954(19) 0.4605(6) 0.9469(8) 0.046(4) Uani 1 1 d U . . C80 C 0.799(2) 0.5110(7) 0.9127(10) 0.060(5) Uani 1 1 d U . . H80 H 0.7634 0.5150 0.8689 0.072 Uiso 1 1 calc R . . C81 C 0.856(2) 0.5526(8) 0.9469(11) 0.074(5) Uani 1 1 d U . . H81 H 0.8567 0.5863 0.9267 0.089 Uiso 1 1 calc R . . C82 C 0.913(2) 0.5464(8) 1.0108(11) 0.074(5) Uani 1 1 d U . . H82 H 0.9512 0.5753 1.0340 0.088 Uiso 1 1 calc R . . C83 C 0.910(2) 0.4998(7) 1.0369(9) 0.061(5) Uani 1 1 d U . . H83 H 0.9492 0.4960 1.0800 0.073 Uiso 1 1 calc R . . C84 C 0.8568(19) 0.4550(7) 1.0078(8) 0.054(4) Uani 1 1 d U . . H84 H 0.8626 0.4217 1.0293 0.065 Uiso 1 1 calc R . . C85 C 0.5783(16) 0.4249(7) 0.8877(9) 0.042(4) Uani 1 1 d U . . C86 C 0.5013(17) 0.3957(8) 0.8433(9) 0.052(4) Uani 1 1 d U . . H86 H 0.5268 0.3647 0.8241 0.063 Uiso 1 1 calc R . . C87 C 0.3880(18) 0.4114(9) 0.8268(11) 0.058(4) Uani 1 1 d U . . H87 H 0.3379 0.3936 0.7937 0.070 Uiso 1 1 calc R . . C88 C 0.348(2) 0.4552(9) 0.8608(11) 0.067(5) Uani 1 1 d U . . H88 H 0.2719 0.4674 0.8500 0.081 Uiso 1 1 calc R . . C89 C 0.421(2) 0.4786(9) 0.9079(11) 0.070(5) Uani 1 1 d U . . H89 H 0.3929 0.5049 0.9337 0.084 Uiso 1 1 calc R . . C90 C 0.5370(18) 0.4654(8) 0.9204(10) 0.056(4) Uani 1 1 d U . . H90 H 0.5874 0.4847 0.9520 0.067 Uiso 1 1 calc R . . C91 C 0.8917(17) 0.3984(7) 0.6792(8) 0.043(4) Uani 1 1 d U . . C92 C 0.8846(19) 0.4506(7) 0.7028(8) 0.051(4) Uani 1 1 d U . . H92 H 0.8144 0.4658 0.7096 0.061 Uiso 1 1 calc R . . C93 C 0.989(2) 0.4788(8) 0.7156(8) 0.059(4) Uani 1 1 d U . . H93 H 0.9867 0.5144 0.7301 0.071 Uiso 1 1 calc R . . C94 C 1.087(2) 0.4589(9) 0.7087(9) 0.064(5) Uani 1 1 d U . . H94 H 1.1540 0.4798 0.7184 0.077 Uiso 1 1 calc R . . C95 C 1.094(2) 0.4064(10) 0.6870(10) 0.071(5) Uani 1 1 d U . . H95 H 1.1657 0.3919 0.6816 0.085 Uiso 1 1 calc R . . C96 C 0.9938(18) 0.3754(8) 0.6732(9) 0.054(4) Uani 1 1 d U . . H96 H 0.9973 0.3394 0.6601 0.064 Uiso 1 1 calc R . . C97 C 0.642(2) 0.3972(8) 0.6430(9) 0.053(4) Uani 1 1 d U . . C98 C 0.643(2) 0.4417(8) 0.6092(9) 0.057(4) Uani 1 1 d U . . H98 H 0.7118 0.4524 0.5958 0.069 Uiso 1 1 calc R . . C99 C 0.548(2) 0.4733(9) 0.5926(11) 0.075(5) Uani 1 1 d U . . H99 H 0.5538 0.5078 0.5755 0.090 Uiso 1 1 calc R . . C100 C 0.441(2) 0.4530(9) 0.6016(12) 0.080(5) Uani 1 1 d U . . H100 H 0.3737 0.4719 0.5845 0.096 Uiso 1 1 calc R . . C101 C 0.433(2) 0.4065(10) 0.6345(11) 0.078(5) Uani 1 1 d U . . H101 H 0.3614 0.3945 0.6435 0.094 Uiso 1 1 calc R . . C102 C 0.535(2) 0.3764(8) 0.6549(10) 0.060(4) Uani 1 1 d U . . H102 H 0.5324 0.3433 0.6761 0.072 Uiso 1 1 calc R . . Cl1 Cl 0.7873(5) 0.07442(18) 0.2978(2) 0.0533(13) Uani 1 1 d . . . Cl2 Cl 0.4145(4) 0.25036(18) 0.7295(2) 0.0483(12) Uani 1 1 d . . . Cl3 Cl 0.7209(6) 0.4281(2) 1.2447(3) 0.0689(18) Uani 1 1 d . . . O1 O 0.7287(14) 0.1208(6) 0.2655(8) 0.084(5) Uani 1 1 d . . . O2 O 0.7969(15) 0.0769(6) 0.3674(6) 0.072(5) Uani 1 1 d . . . O3 O 0.8970(14) 0.0701(6) 0.2791(8) 0.076(5) Uani 1 1 d . . . O4 O 0.7207(14) 0.0270(5) 0.2761(6) 0.064(4) Uani 1 1 d . . . O5 O 0.5377(12) 0.2447(7) 0.7416(7) 0.079(5) Uani 1 1 d . . . O6 O 0.3726(14) 0.2679(7) 0.6657(7) 0.084(5) Uani 1 1 d . . . O7 O 0.367(2) 0.1992(7) 0.7399(12) 0.142(9) Uani 1 1 d . . . O8 O 0.386(2) 0.2873(10) 0.7742(9) 0.164(11) Uani 1 1 d . . . O9 O 0.654(2) 0.3849(6) 1.2586(10) 0.133(10) Uani 1 1 d . . . O10 O 0.7237(19) 0.4259(6) 1.1762(8) 0.100(7) Uani 1 1 d . . . O11 O 0.8358(19) 0.4237(8) 1.2829(10) 0.125(9) Uani 1 1 d . . . O12 O 0.6678(15) 0.4788(5) 1.2612(7) 0.074(5) Uani 1 1 d . . . Cl4 Cl 0.2533(7) 0.2717(3) 0.2800(4) 0.100(2) Uiso 1 1 d D . . O13 O 0.242(2) 0.2420(11) 0.3381(12) 0.122(15) Uiso 0.57(3) 1 d PD A 1 O14 O 0.3581(19) 0.3021(10) 0.2917(15) 0.121(15) Uiso 0.57(3) 1 d PD A 1 O15 O 0.1556(18) 0.3059(9) 0.2627(13) 0.098(12) Uiso 0.57(3) 1 d PD A 1 O16 O 0.261(3) 0.2344(12) 0.2279(14) 0.24(3) Uiso 0.57(3) 1 d PD A 1 O14A O 0.342(3) 0.2319(16) 0.280(2) 0.25(4) Uiso 0.43(3) 1 d PD A 2 O13A O 0.144(3) 0.2466(18) 0.279(2) 0.16(3) Uiso 0.43(3) 1 d PD A 2 O16A O 0.249(4) 0.3035(16) 0.2206(15) 0.17(3) Uiso 0.43(3) 1 d PD A 2 O15A O 0.282(4) 0.3063(15) 0.3351(15) 0.15(2) Uiso 0.43(3) 1 d PD A 2 N5 N 1.292(2) -0.0641(10) 0.8780(12) 0.106(8) Uiso 1 1 d D . . C103 C 1.175(4) -0.094(2) 0.7720(17) 0.23(2) Uiso 1 1 d D . . H10D H 1.0988 -0.0779 0.7677 0.342 Uiso 1 1 calc R . . H10E H 1.1677 -0.1322 0.7650 0.342 Uiso 1 1 calc R . . H10F H 1.2164 -0.0782 0.7399 0.342 Uiso 1 1 calc R . . C104 C 1.238(2) -0.0835(11) 0.8372(13) 0.096(9) Uiso 1 1 d D . . N6 N 0.287(3) -0.0837(16) 0.6340(19) 0.201(16) Uiso 1 1 d D . . C105 C 0.467(3) -0.0436(13) 0.7074(16) 0.135(13) Uiso 1 1 d D . . H10G H 0.4888 -0.0107 0.6879 0.202 Uiso 1 1 calc R . . H10H H 0.5317 -0.0681 0.7139 0.202 Uiso 1 1 calc R . . H10I H 0.4437 -0.0357 0.7491 0.202 Uiso 1 1 calc R . . C106 C 0.370(3) -0.0683(16) 0.6639(19) 0.153(15) Uiso 1 1 d D . . N7 N 0.280(3) 0.5654(11) 0.6311(14) 0.132(10) Uiso 1 1 d D . . C107 C 0.387(3) 0.5714(17) 0.7496(16) 0.171(17) Uiso 1 1 d D . . H10J H 0.3843 0.5369 0.7707 0.257 Uiso 1 1 calc R . . H10K H 0.3548 0.5987 0.7745 0.257 Uiso 1 1 calc R . . H10L H 0.4670 0.5804 0.7474 0.257 Uiso 1 1 calc R . . C108 C 0.322(3) 0.5691(13) 0.6839(15) 0.115(10) Uiso 1 1 d D . . C109 C 0.098(6) 0.547(3) 0.873(2) 0.18(4) Uiso 0.50 1 d PD . . H10M H 0.0992 0.5082 0.8636 0.217 Uiso 0.50 1 calc PR . . H10N H 0.0181 0.5570 0.8760 0.217 Uiso 0.50 1 calc PR . . Cl6 Cl 0.187(4) 0.5607(16) 0.9448(18) 0.283(17) Uiso 0.50 1 d PD . . Cl5 Cl 0.149(5) 0.583(2) 0.815(2) 0.36(2) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0394(10) 0.0347(8) 0.0214(7) 0.0003(6) 0.0021(7) 0.0005(7) Mo2 0.0388(10) 0.0354(8) 0.0238(8) -0.0010(6) 0.0049(7) -0.0018(7) Mo3 0.0370(10) 0.0346(8) 0.0242(8) 0.0022(6) 0.0056(7) 0.0015(6) Mo4 0.0358(10) 0.0429(8) 0.0214(7) -0.0015(6) 0.0043(7) 0.0015(7) Cu1 0.0486(15) 0.0357(11) 0.0260(11) -0.0060(9) 0.0047(10) 0.0023(10) Cu2 0.0459(15) 0.0311(11) 0.0248(11) 0.0027(9) 0.0064(10) 0.0023(9) Cu3 0.0511(16) 0.0333(11) 0.0273(11) -0.0013(9) 0.0096(10) -0.0018(10) Cu4 0.0418(14) 0.0382(12) 0.0269(11) -0.0022(9) 0.0056(10) -0.0005(9) S1 0.049(3) 0.035(2) 0.029(2) -0.0037(19) 0.007(2) 0.003(2) S2 0.045(3) 0.040(2) 0.031(2) -0.0002(18) 0.007(2) 0.001(2) S3 0.038(3) 0.029(2) 0.031(2) 0.0030(17) 0.002(2) -0.0014(17) S4 0.036(3) 0.034(2) 0.029(2) -0.0011(17) 0.0071(19) 0.0019(18) S5 0.048(3) 0.043(2) 0.025(2) 0.0029(19) 0.005(2) 0.000(2) S6 0.035(3) 0.041(2) 0.031(2) -0.0027(18) 0.014(2) 0.0020(19) S7 0.043(3) 0.040(2) 0.021(2) -0.0008(17) 0.0023(19) -0.0026(19) S8 0.051(3) 0.038(3) 0.031(2) 0.0035(19) 0.014(2) 0.008(2) P1 0.039(3) 0.037(2) 0.030(2) 0.0012(19) 0.008(2) 0.000(2) P2 0.052(3) 0.039(2) 0.027(2) -0.0011(19) 0.014(2) -0.002(2) P3 0.045(3) 0.035(2) 0.030(2) 0.0012(19) 0.010(2) -0.001(2) P4 0.047(3) 0.043(3) 0.029(2) -0.001(2) 0.008(2) 0.003(2) N1 0.043(11) 0.058(10) 0.039(9) -0.004(7) 0.022(8) 0.000(8) N2 0.071(10) 0.077(9) 0.042(8) -0.007(7) 0.001(8) 0.004(8) N3 0.035(9) 0.039(8) 0.017(6) 0.004(5) -0.002(6) 0.005(6) N4 0.066(9) 0.057(8) 0.068(9) -0.001(7) 0.025(8) -0.003(7) C1 0.054(10) 0.045(6) 0.023(7) -0.006(6) -0.012(6) 0.000(6) C2 0.042(9) 0.043(6) 0.032(8) -0.002(6) -0.015(6) 0.011(6) C3 0.042(9) 0.051(7) 0.023(7) -0.004(6) -0.003(6) -0.002(6) C4 0.034(9) 0.044(6) 0.028(7) -0.004(6) -0.006(6) 0.001(6) C5 0.048(9) 0.049(6) 0.021(7) 0.004(6) 0.005(6) 0.005(6) C6 0.093(16) 0.046(8) 0.027(9) 0.012(7) -0.021(9) -0.004(9) C7 0.045(13) 0.065(10) 0.061(12) -0.006(10) -0.005(9) 0.020(9) C8 0.055(15) 0.073(13) 0.081(16) -0.002(11) 0.024(11) -0.006(10) C9 0.070(15) 0.040(7) 0.040(10) -0.008(8) -0.010(9) 0.002(8) C10 0.047(12) 0.075(12) 0.032(10) -0.012(8) 0.013(8) -0.020(9) C11 0.037(12) 0.045(10) 0.032(10) 0.010(8) 0.015(8) 0.006(8) C12 0.027(11) 0.028(8) 0.058(12) 0.005(8) 0.013(9) -0.004(7) C13 0.027(11) 0.070(13) 0.029(10) -0.002(9) 0.005(8) 0.001(9) C14 0.076(16) 0.040(10) 0.038(11) 0.005(8) 0.027(11) 0.011(9) C15 0.027(11) 0.059(12) 0.040(11) 0.004(9) -0.002(8) -0.007(8) C16 0.077(17) 0.042(10) 0.042(11) -0.010(9) 0.021(11) -0.010(10) C17 0.045(13) 0.057(11) 0.054(12) -0.005(9) -0.001(10) -0.023(9) C18 0.039(12) 0.052(11) 0.045(11) 0.011(9) -0.017(9) -0.007(9) C19 0.09(2) 0.064(14) 0.043(12) 0.003(10) 0.020(12) 0.008(12) C20 0.036(12) 0.050(11) 0.039(10) -0.016(8) 0.012(8) -0.005(8) C21 0.048(13) 0.036(10) 0.055(12) -0.007(9) 0.023(10) 0.013(8) C22 0.031(12) 0.068(12) 0.032(10) -0.009(9) 0.013(8) -0.015(9) C23 0.032(8) 0.042(7) 0.054(8) -0.002(7) 0.007(7) 0.002(6) C24 0.043(14) 0.065(14) 0.047(12) -0.037(10) -0.001(10) -0.005(10) C25 0.034(12) 0.052(11) 0.051(12) 0.012(10) 0.032(10) 0.011(9) C26 0.057(14) 0.041(10) 0.054(12) 0.005(9) 0.017(10) 0.012(9) C27 0.063(15) 0.050(11) 0.034(10) 0.004(8) 0.024(10) -0.002(9) C28 0.076(17) 0.036(10) 0.066(14) 0.013(10) 0.037(12) 0.004(10) C29 0.041(14) 0.101(17) 0.068(14) -0.005(13) 0.041(12) -0.012(12) C30 0.082(19) 0.079(16) 0.056(14) 0.004(12) 0.026(13) 0.017(13) C31 0.064(11) 0.065(7) 0.042(9) -0.008(7) -0.006(7) 0.020(8) C32 0.059(11) 0.094(9) 0.037(9) -0.003(8) -0.003(7) 0.030(8) C33 0.060(10) 0.094(8) 0.030(8) 0.013(7) 0.008(7) 0.019(8) C34 0.041(7) 0.060(6) 0.033(6) 0.001(5) -0.008(5) -0.001(6) C35 0.058(10) 0.062(7) 0.021(7) -0.005(6) -0.003(6) -0.006(7) C36 0.078(16) 0.056(8) 0.065(13) 0.010(9) -0.037(11) 0.034(9) C37 0.075(17) 0.154(18) 0.055(14) -0.033(13) -0.003(11) 0.051(16) C38 0.083(18) 0.144(17) 0.047(13) 0.019(14) 0.012(11) -0.018(14) C39 0.055(14) 0.069(9) 0.059(12) -0.015(9) 0.004(10) -0.019(10) C40 0.075(15) 0.086(14) 0.022(9) 0.003(8) 0.005(8) 0.012(10) C41 0.049(12) 0.035(9) 0.038(10) -0.019(8) 0.002(9) 0.016(8) C42 0.059(13) 0.038(10) 0.026(9) -0.020(7) 0.001(9) -0.014(8) C43 0.067(10) 0.067(9) 0.019(8) 0.004(6) -0.001(7) -0.012(8) C44 0.054(10) 0.074(10) 0.037(9) 0.005(7) 0.003(8) -0.014(8) C45 0.062(9) 0.103(12) 0.050(10) 0.003(8) 0.007(9) -0.007(10) C46 0.067(10) 0.114(13) 0.059(11) 0.002(9) 0.011(10) 0.016(10) C47 0.080(12) 0.099(12) 0.060(11) -0.007(9) 0.003(10) 0.016(10) C48 0.043(8) 0.036(7) 0.022(7) 0.000(6) -0.002(6) 0.008(6) C49 0.041(9) 0.041(8) 0.031(8) 0.002(6) 0.000(6) 0.013(6) C50 0.046(9) 0.054(8) 0.042(8) -0.001(7) 0.013(7) 0.020(7) C51 0.054(9) 0.054(9) 0.045(9) 0.002(7) 0.007(7) 0.025(7) C52 0.054(10) 0.041(8) 0.038(8) 0.011(6) 0.008(7) 0.012(6) C53 0.048(8) 0.040(7) 0.019(7) 0.004(5) 0.007(6) 0.005(6) C54 0.048(8) 0.039(7) 0.030(8) -0.010(6) 0.022(7) -0.003(6) C55 0.062(8) 0.040(7) 0.035(8) -0.012(6) 0.022(7) -0.006(6) C56 0.067(9) 0.047(8) 0.047(9) -0.005(7) 0.024(8) -0.013(6) C57 0.059(7) 0.058(7) 0.053(7) -0.007(6) 0.019(6) -0.019(6) C58 0.056(9) 0.064(8) 0.048(9) -0.005(7) 0.009(8) -0.020(7) C59 0.052(9) 0.044(8) 0.038(8) -0.016(7) 0.009(7) -0.010(6) C60 0.067(14) 0.014(7) 0.031(9) 0.009(7) 0.020(9) 0.008(7) C61 0.11(2) 0.055(13) 0.034(11) -0.006(9) 0.041(12) 0.008(12) C62 0.093(18) 0.039(10) 0.036(11) -0.009(8) 0.017(11) 0.012(10) C63 0.050(9) 0.052(8) 0.045(8) -0.006(7) -0.001(7) -0.004(7) C64 0.037(12) 0.041(10) 0.045(10) -0.010(8) 0.008(9) 0.018(8) C65 0.069(16) 0.051(11) 0.033(10) -0.007(8) 0.025(10) 0.005(10) C66 0.046(9) 0.032(8) 0.061(10) 0.008(7) 0.018(7) -0.005(6) C67 0.053(10) 0.068(10) 0.073(11) 0.003(8) 0.020(9) 0.009(8) C68 0.053(9) 0.087(12) 0.093(12) 0.022(8) 0.024(10) 0.000(9) C69 0.045(9) 0.079(11) 0.113(13) 0.024(9) -0.002(9) 0.002(8) C70 0.066(8) 0.073(8) 0.083(8) 0.006(7) -0.011(7) -0.003(7) C71 0.060(8) 0.066(10) 0.059(10) -0.001(7) 0.010(9) 0.002(8) C72 0.026(7) 0.040(7) 0.030(7) 0.004(6) 0.005(6) 0.001(6) C73 0.042(12) 0.026(8) 0.029(9) 0.003(7) 0.004(8) 0.001(7) C74 0.067(10) 0.035(8) 0.031(8) 0.013(6) 0.005(7) 0.004(6) C75 0.076(10) 0.040(8) 0.040(9) 0.014(6) -0.002(8) -0.011(7) C76 0.071(10) 0.071(10) 0.050(10) 0.021(8) 0.003(9) -0.018(8) C77 0.062(10) 0.082(11) 0.085(12) 0.025(9) 0.020(9) -0.016(8) C78 0.066(10) 0.058(10) 0.089(12) 0.013(8) 0.028(10) -0.004(8) C79 0.082(12) 0.032(7) 0.026(7) -0.012(6) 0.011(7) -0.010(7) C80 0.095(13) 0.041(8) 0.041(8) 0.000(6) 0.002(9) -0.010(8) C81 0.117(14) 0.039(8) 0.062(9) 0.004(7) 0.003(10) -0.020(9) C82 0.116(14) 0.047(8) 0.056(9) -0.008(8) 0.007(9) -0.025(9) C83 0.108(13) 0.043(8) 0.029(8) -0.011(6) 0.001(8) -0.015(9) C84 0.097(12) 0.036(7) 0.029(7) -0.007(6) 0.008(8) -0.012(8) C85 0.034(8) 0.047(9) 0.047(9) 0.010(7) 0.010(6) 0.003(6) C86 0.040(8) 0.067(9) 0.051(9) 0.005(7) 0.010(7) -0.002(7) C87 0.038(7) 0.073(8) 0.066(8) 0.012(6) 0.016(6) -0.009(6) C88 0.046(9) 0.084(11) 0.074(11) 0.013(8) 0.015(8) 0.014(8) C89 0.057(10) 0.084(11) 0.070(11) 0.002(8) 0.014(9) 0.023(9) C90 0.048(9) 0.065(10) 0.055(10) 0.003(7) 0.011(8) 0.008(8) C91 0.053(9) 0.049(8) 0.027(8) -0.003(7) 0.007(8) -0.018(7) C92 0.069(9) 0.045(8) 0.038(8) 0.001(7) 0.008(8) -0.023(7) C93 0.077(11) 0.071(9) 0.030(8) 0.002(7) 0.013(9) -0.043(7) C94 0.073(10) 0.080(10) 0.041(9) 0.004(8) 0.014(9) -0.049(9) C95 0.063(10) 0.092(10) 0.058(10) -0.011(9) 0.009(9) -0.032(8) C96 0.053(10) 0.071(9) 0.039(9) -0.017(8) 0.015(8) -0.024(7) C97 0.068(10) 0.052(9) 0.036(9) 0.000(7) 0.002(8) 0.010(8) C98 0.076(10) 0.053(9) 0.046(9) 0.004(7) 0.019(9) 0.021(7) C99 0.099(12) 0.059(10) 0.067(11) -0.003(8) 0.016(10) 0.035(8) C100 0.084(11) 0.071(11) 0.081(12) -0.006(9) 0.004(11) 0.040(9) C101 0.075(10) 0.094(11) 0.066(11) 0.003(9) 0.016(10) 0.029(9) C102 0.070(11) 0.057(9) 0.053(10) 0.004(8) 0.013(9) 0.014(7) Cl1 0.077(4) 0.038(2) 0.047(3) 0.002(2) 0.013(3) 0.002(2) Cl2 0.052(3) 0.054(3) 0.038(2) 0.006(2) 0.007(2) -0.003(2) Cl3 0.121(6) 0.044(3) 0.044(3) -0.013(2) 0.018(3) 0.005(3) O1 0.096(15) 0.049(9) 0.102(13) 0.041(9) 0.007(11) -0.002(9) O2 0.113(14) 0.077(10) 0.024(7) -0.007(7) 0.008(8) -0.008(9) O3 0.065(12) 0.073(10) 0.098(12) -0.003(9) 0.041(10) 0.005(8) O4 0.109(14) 0.040(8) 0.041(7) -0.013(6) 0.006(8) -0.015(8) O5 0.034(9) 0.139(14) 0.061(10) 0.033(10) -0.005(7) 0.005(9) O6 0.066(11) 0.126(14) 0.051(9) 0.032(9) -0.013(8) -0.038(10) O7 0.14(2) 0.064(11) 0.19(2) 0.051(13) -0.040(17) -0.059(12) O8 0.23(3) 0.18(2) 0.074(13) -0.066(14) 0.002(15) 0.118(19) O9 0.24(3) 0.061(10) 0.130(16) -0.026(11) 0.135(18) -0.066(14) O10 0.19(2) 0.069(11) 0.043(9) -0.007(8) 0.035(11) 0.029(12) O11 0.129(19) 0.124(16) 0.105(15) -0.056(12) -0.024(14) 0.089(14) O12 0.114(15) 0.049(8) 0.058(9) -0.017(7) 0.008(9) 0.018(8) _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(5) . ? Mo1 S4 2.339(5) . ? Mo1 S3 2.339(4) . ? Mo1 C1 2.342(18) . ? Mo1 C5 2.345(16) . ? Mo1 C2 2.349(18) . ? Mo1 C4 2.354(17) . ? Mo1 C3 2.381(19) . ? Mo1 Cu2 2.774(3) . ? Mo1 Cu1 2.777(3) . ? Mo1 Mo2 2.864(2) . ? Mo2 S2 2.233(5) . ? Mo2 S3 2.328(5) . ? Mo2 S4 2.334(5) . ? Mo2 C11 2.338(16) . ? Mo2 C12 2.346(16) . ? Mo2 C14 2.37(2) . ? Mo2 C13 2.382(19) . ? Mo2 C15 2.416(19) . ? Mo2 Cu1 2.774(3) . ? Mo2 Cu2 2.779(3) . ? Mo3 S5 2.241(5) . ? Mo3 S7 2.329(5) . ? Mo3 S8 2.340(5) . ? Mo3 C22 2.371(17) . ? Mo3 C23 2.384(19) . ? Mo3 C24 2.39(2) . ? Mo3 C21 2.399(16) . ? Mo3 C25 2.414(18) . ? Mo3 Cu3 2.760(3) . ? Mo3 Cu4 2.780(3) . ? Mo3 Mo4 2.865(2) . ? Mo4 S6 2.234(4) . ? Mo4 C35 2.314(19) . ? Mo4 S7 2.322(5) . ? Mo4 S8 2.344(5) . ? Mo4 C31 2.36(2) . ? Mo4 C34 2.368(18) . ? Mo4 C33 2.38(2) . ? Mo4 C32 2.43(2) . ? Mo4 Cu4 2.756(3) . ? Mo4 Cu3 2.780(3) . ? Cu1 P1 2.224(5) . ? Cu1 S3 2.249(5) . ? Cu1 S1 2.357(5) . ? Cu1 S2 2.378(6) . ? Cu1 Cu2 2.967(3) . ? Cu2 P3 2.224(5) . ? Cu2 S4 2.262(5) . ? Cu2 S2 2.374(5) . ? Cu2 S1 2.387(5) . ? Cu3 P2 2.219(5) . ? Cu3 S7 2.265(5) . ? Cu3 S5 2.341(6) . ? Cu3 S6 2.394(5) . ? Cu3 Cu4 2.989(3) . ? Cu4 P4 2.203(5) . ? Cu4 S8 2.261(5) . ? Cu4 S5 2.351(5) . ? Cu4 S6 2.371(5) . ? P1 C48 1.769(17) . ? P1 C54 1.809(18) . ? P1 C41 1.839(18) . ? P2 C60 1.792(15) . ? P2 C66 1.818(19) . ? P2 C42 1.867(16) . ? P3 C85 1.801(19) . ? P3 C79 1.806(17) . ? P3 C72 1.871(16) . ? P4 C97 1.81(2) . ? P4 C91 1.838(19) . ? P4 C73 1.920(16) . ? N1 C43 1.37(2) . ? N1 C42 1.43(2) . ? N1 C41 1.49(2) . ? N2 C47 1.31(3) . ? N2 C43 1.37(2) . ? N3 C74 1.41(2) . ? N3 C72 1.426(19) . ? N3 C73 1.45(2) . ? N4 C78 1.29(3) . ? N4 C74 1.41(2) . ? C1 C5 1.42(2) . ? C1 C2 1.42(3) . ? C1 C6 1.53(2) . ? C2 C3 1.36(2) . ? C2 C7 1.55(2) . ? C3 C4 1.41(2) . ? C3 C8 1.51(3) . ? C4 C5 1.42(2) . ? C4 C9 1.52(2) . ? C5 C10 1.47(2) . ? C11 C15 1.42(2) . ? C11 C12 1.42(2) . ? C11 C16 1.55(2) . ? C12 C13 1.43(2) . ? C12 C17 1.53(2) . ? C13 C14 1.40(3) . ? C13 C18 1.52(2) . ? C14 C15 1.45(3) . ? C14 C19 1.45(3) . ? C15 C20 1.46(2) . ? C21 C25 1.43(3) . ? C21 C22 1.44(3) . ? C21 C26 1.44(2) . ? C22 C23 1.43(2) . ? C22 C27 1.47(2) . ? C23 C24 1.44(3) . ? C23 C28 1.49(2) . ? C24 C25 1.41(3) . ? C24 C29 1.49(3) . ? C25 C30 1.43(3) . ? C31 C32 1.41(3) . ? C31 C35 1.45(3) . ? C31 C36 1.47(3) . ? C32 C33 1.45(3) . ? C32 C37 1.51(3) . ? C33 C34 1.47(3) . ? C33 C38 1.54(3) . ? C34 C35 1.41(3) . ? C34 C39 1.48(3) . ? C35 C40 1.55(3) . ? C43 C44 1.36(3) . ? C44 C45 1.35(3) . ? C45 C46 1.44(3) . ? C46 C47 1.38(3) . ? C48 C53 1.42(2) . ? C48 C49 1.43(2) . ? C49 C50 1.38(2) . ? C50 C51 1.41(2) . ? C51 C52 1.36(3) . ? C52 C53 1.38(2) . ? C54 C55 1.42(2) . ? C54 C59 1.43(3) . ? C55 C56 1.36(2) . ? C56 C57 1.36(3) . ? C57 C58 1.39(3) . ? C58 C59 1.36(3) . ? C60 C61 1.34(2) . ? C60 C65 1.41(2) . ? C61 C62 1.43(2) . ? C62 C63 1.37(3) . ? C63 C64 1.43(2) . ? C64 C65 1.43(2) . ? C66 C67 1.379(14) . ? C66 C71 1.385(14) . ? C67 C68 1.395(15) . ? C68 C69 1.395(15) . ? C69 C70 1.357(15) . ? C70 C71 1.375(15) . ? C74 C75 1.35(3) . ? C75 C76 1.37(3) . ? C76 C77 1.40(3) . ? C77 C78 1.40(3) . ? C79 C84 1.37(3) . ? C79 C80 1.46(2) . ? C80 C81 1.38(3) . ? C81 C82 1.40(3) . ? C82 C83 1.30(3) . ? C83 C84 1.39(2) . ? C85 C90 1.37(2) . ? C85 C86 1.40(3) . ? C86 C87 1.39(3) . ? C87 C88 1.43(3) . ? C88 C89 1.34(3) . ? C89 C90 1.40(3) . ? C91 C96 1.37(3) . ? C91 C92 1.41(2) . ? C92 C93 1.41(3) . ? C93 C94 1.30(3) . ? C94 C95 1.40(3) . ? C95 C96 1.42(3) . ? C97 C98 1.33(3) . ? C97 C102 1.43(3) . ? C98 C99 1.38(3) . ? C99 C100 1.40(3) . ? C100 C101 1.37(3) . ? C101 C102 1.44(3) . ? Cl1 O3 1.426(15) . ? Cl1 O2 1.446(14) . ? Cl1 O4 1.464(13) . ? Cl1 O1 1.467(14) . ? Cl2 O8 1.401(16) . ? Cl2 O6 1.418(14) . ? Cl2 O7 1.439(16) . ? Cl2 O5 1.451(15) . ? Cl3 O9 1.406(15) . ? Cl3 O10 1.442(16) . ? Cl3 O11 1.47(2) . ? Cl3 O12 1.491(14) . ? Cl4 O13A 1.44(2) . ? Cl4 O15A 1.442(19) . ? Cl4 O15 1.442(18) . ? Cl4 O14 1.449(18) . ? Cl4 O16 1.455(19) . ? Cl4 O14A 1.45(2) . ? Cl4 O13 1.455(18) . ? Cl4 O16A 1.474(19) . ? N5 C104 1.095(17) . ? C103 C104 1.468(19) . ? N6 C106 1.148(19) . ? C105 C106 1.479(19) . ? N7 C108 1.141(18) . ? C107 C108 1.467(19) . ? C109 Cl5 1.72(2) . ? C109 Cl6 1.72(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 S4 106.01(17) . . ? S1 Mo1 S3 104.58(17) . . ? S4 Mo1 S3 101.10(17) . . ? S1 Mo1 C1 129.4(5) . . ? S4 Mo1 C1 121.0(5) . . ? S3 Mo1 C1 84.9(5) . . ? S1 Mo1 C5 142.1(5) . . ? S4 Mo1 C5 89.1(5) . . ? S3 Mo1 C5 106.3(5) . . ? C1 Mo1 C5 35.2(6) . . ? S1 Mo1 C2 94.8(5) . . ? S4 Mo1 C2 144.4(4) . . ? S3 Mo1 C2 101.1(4) . . ? C1 Mo1 C2 35.2(7) . . ? C5 Mo1 C2 58.0(6) . . ? S1 Mo1 C4 109.3(4) . . ? S4 Mo1 C4 88.3(4) . . ? S3 Mo1 C4 140.7(4) . . ? C1 Mo1 C4 58.3(6) . . ? C5 Mo1 C4 35.1(6) . . ? C2 Mo1 C4 57.2(6) . . ? S1 Mo1 C3 84.8(4) . . ? S4 Mo1 C3 119.2(4) . . ? S3 Mo1 C3 134.6(4) . . ? C1 Mo1 C3 57.5(6) . . ? C5 Mo1 C3 57.8(6) . . ? C2 Mo1 C3 33.5(6) . . ? C4 Mo1 C3 34.7(6) . . ? S1 Mo1 Cu2 55.64(14) . . ? S4 Mo1 Cu2 51.67(12) . . ? S3 Mo1 Cu2 101.60(13) . . ? C1 Mo1 Cu2 170.8(4) . . ? C5 Mo1 Cu2 135.6(4) . . ? C2 Mo1 Cu2 146.5(5) . . ? C4 Mo1 Cu2 113.7(4) . . ? C3 Mo1 Cu2 119.2(4) . . ? S1 Mo1 Cu1 54.81(13) . . ? S4 Mo1 Cu1 101.77(13) . . ? S3 Mo1 Cu1 51.29(12) . . ? C1 Mo1 Cu1 124.4(4) . . ? C5 Mo1 Cu1 156.3(4) . . ? C2 Mo1 Cu1 113.8(4) . . ? C4 Mo1 Cu1 162.9(4) . . ? C3 Mo1 Cu1 129.5(4) . . ? Cu2 Mo1 Cu1 64.62(7) . . ? S1 Mo1 Mo2 99.96(14) . . ? S4 Mo1 Mo2 52.13(12) . . ? S3 Mo1 Mo2 51.97(12) . . ? C1 Mo1 Mo2 122.6(5) . . ? C5 Mo1 Mo2 116.3(5) . . ? C2 Mo1 Mo2 151.8(5) . . ? C4 Mo1 Mo2 136.4(4) . . ? C3 Mo1 Mo2 170.9(4) . . ? Cu2 Mo1 Mo2 59.03(7) . . ? Cu1 Mo1 Mo2 58.89(7) . . ? S2 Mo2 S3 105.39(17) . . ? S2 Mo2 S4 105.33(17) . . ? S3 Mo2 S4 101.55(17) . . ? S2 Mo2 C11 139.2(5) . . ? S3 Mo2 C11 89.4(4) . . ? S4 Mo2 C11 108.6(5) . . ? S2 Mo2 C12 105.5(5) . . ? S3 Mo2 C12 90.8(4) . . ? S4 Mo2 C12 142.2(4) . . ? C11 Mo2 C12 35.2(6) . . ? S2 Mo2 C14 96.5(5) . . ? S3 Mo2 C14 146.3(5) . . ? S4 Mo2 C14 96.8(5) . . ? C11 Mo2 C14 57.9(6) . . ? C12 Mo2 C14 58.4(6) . . ? S2 Mo2 C13 83.1(4) . . ? S3 Mo2 C13 123.4(5) . . ? S4 Mo2 C13 130.7(5) . . ? C11 Mo2 C13 57.7(6) . . ? C12 Mo2 C13 35.2(6) . . ? C14 Mo2 C13 34.1(7) . . ? S2 Mo2 C15 131.7(5) . . ? S3 Mo2 C15 119.0(5) . . ? S4 Mo2 C15 84.5(4) . . ? C11 Mo2 C15 34.6(6) . . ? C12 Mo2 C15 58.6(6) . . ? C14 Mo2 C15 35.2(6) . . ? C13 Mo2 C15 57.7(6) . . ? S2 Mo2 Cu1 55.45(14) . . ? S3 Mo2 Cu1 51.40(12) . . ? S4 Mo2 Cu1 101.97(13) . . ? C11 Mo2 Cu1 134.5(4) . . ? C12 Mo2 Cu1 113.4(4) . . ? C14 Mo2 Cu1 149.5(5) . . ? C13 Mo2 Cu1 121.0(4) . . ? C15 Mo2 Cu1 169.1(5) . . ? S2 Mo2 Cu2 55.25(14) . . ? S3 Mo2 Cu2 101.73(13) . . ? S4 Mo2 Cu2 51.62(12) . . ? C11 Mo2 Cu2 158.6(5) . . ? C12 Mo2 Cu2 159.1(5) . . ? C14 Mo2 Cu2 111.8(4) . . ? C13 Mo2 Cu2 125.9(5) . . ? C15 Mo2 Cu2 125.7(5) . . ? Cu1 Mo2 Cu2 64.59(7) . . ? S2 Mo2 Mo1 100.08(15) . . ? S3 Mo2 Mo1 52.31(12) . . ? S4 Mo2 Mo1 52.27(12) . . ? C11 Mo2 Mo1 118.4(5) . . ? C12 Mo2 Mo1 139.9(4) . . ? C14 Mo2 Mo1 147.8(5) . . ? C13 Mo2 Mo1 175.1(5) . . ? C15 Mo2 Mo1 121.3(4) . . ? Cu1 Mo2 Mo1 58.98(6) . . ? Cu2 Mo2 Mo1 58.85(6) . . ? S5 Mo3 S7 105.68(17) . . ? S5 Mo3 S8 104.74(17) . . ? S7 Mo3 S8 100.69(18) . . ? S5 Mo3 C22 140.0(5) . . ? S7 Mo3 C22 89.7(4) . . ? S8 Mo3 C22 108.3(5) . . ? S5 Mo3 C23 130.7(5) . . ? S7 Mo3 C23 120.1(5) . . ? S8 Mo3 C23 84.9(4) . . ? C22 Mo3 C23 35.1(6) . . ? S5 Mo3 C24 95.9(5) . . ? S7 Mo3 C24 145.5(4) . . ? S8 Mo3 C24 99.4(5) . . ? C22 Mo3 C24 57.4(6) . . ? C23 Mo3 C24 35.1(7) . . ? S5 Mo3 C21 106.7(5) . . ? S7 Mo3 C21 90.6(5) . . ? S8 Mo3 C21 142.1(5) . . ? C22 Mo3 C21 35.1(6) . . ? C23 Mo3 C21 58.6(6) . . ? C24 Mo3 C21 57.1(6) . . ? S5 Mo3 C25 83.1(4) . . ? S7 Mo3 C25 121.8(5) . . ? S8 Mo3 C25 133.3(5) . . ? C22 Mo3 C25 57.9(6) . . ? C23 Mo3 C25 58.5(6) . . ? C24 Mo3 C25 34.1(6) . . ? C21 Mo3 C25 34.6(6) . . ? S5 Mo3 Cu3 54.65(14) . . ? S7 Mo3 Cu3 52.00(12) . . ? S8 Mo3 Cu3 102.71(14) . . ? C22 Mo3 Cu3 134.6(5) . . ? C23 Mo3 Cu3 169.6(4) . . ? C24 Mo3 Cu3 146.8(5) . . ? C21 Mo3 Cu3 112.5(4) . . ? C25 Mo3 Cu3 117.9(4) . . ? S5 Mo3 Cu4 54.57(14) . . ? S7 Mo3 Cu4 101.75(13) . . ? S8 Mo3 Cu4 51.53(11) . . ? C22 Mo3 Cu4 158.1(5) . . ? C23 Mo3 Cu4 125.0(4) . . ? C24 Mo3 Cu4 112.7(4) . . ? C21 Mo3 Cu4 159.6(5) . . ? C25 Mo3 Cu4 126.6(5) . . ? Cu3 Mo3 Cu4 65.30(7) . . ? S5 Mo3 Mo4 98.57(15) . . ? S7 Mo3 Mo4 51.85(12) . . ? S8 Mo3 Mo4 52.35(14) . . ? C22 Mo3 Mo4 119.2(5) . . ? C23 Mo3 Mo4 123.2(5) . . ? C24 Mo3 Mo4 150.8(5) . . ? C21 Mo3 Mo4 139.6(5) . . ? C25 Mo3 Mo4 173.6(5) . . ? Cu3 Mo3 Mo4 59.20(7) . . ? Cu4 Mo3 Mo4 58.41(6) . . ? S6 Mo4 C35 142.1(6) . . ? S6 Mo4 S7 106.06(16) . . ? C35 Mo4 S7 97.9(5) . . ? S6 Mo4 S8 106.15(17) . . ? C35 Mo4 S8 97.5(5) . . ? S7 Mo4 S8 100.81(18) . . ? S6 Mo4 C31 116.8(5) . . ? C35 Mo4 C31 36.1(7) . . ? S7 Mo4 C31 133.5(5) . . ? S8 Mo4 C31 84.5(6) . . ? S6 Mo4 C34 117.7(5) . . ? C35 Mo4 C34 35.1(6) . . ? S7 Mo4 C34 85.2(5) . . ? S8 Mo4 C34 132.2(5) . . ? C31 Mo4 C34 60.0(7) . . ? S6 Mo4 C33 85.4(5) . . ? C35 Mo4 C33 58.6(7) . . ? S7 Mo4 C33 110.1(6) . . ? S8 Mo4 C33 142.6(6) . . ? C31 Mo4 C33 59.1(8) . . ? C34 Mo4 C33 36.0(6) . . ? S6 Mo4 C32 86.5(5) . . ? C35 Mo4 C32 57.5(7) . . ? S7 Mo4 C32 143.2(6) . . ? S8 Mo4 C32 108.8(6) . . ? C31 Mo4 C32 34.2(7) . . ? C34 Mo4 C32 58.7(7) . . ? C33 Mo4 C32 35.1(8) . . ? S6 Mo4 Cu4 55.57(14) . . ? C35 Mo4 Cu4 145.6(5) . . ? S7 Mo4 Cu4 102.69(13) . . ? S8 Mo4 Cu4 51.87(12) . . ? C31 Mo4 Cu4 115.7(5) . . ? C34 Mo4 Cu4 170.7(5) . . ? C33 Mo4 Cu4 134.8(5) . . ? C32 Mo4 Cu4 112.7(5) . . ? S6 Mo4 Cu3 55.78(13) . . ? C35 Mo4 Cu3 146.4(5) . . ? S7 Mo4 Cu3 51.76(11) . . ? S8 Mo4 Cu3 102.01(14) . . ? C31 Mo4 Cu3 171.1(6) . . ? C34 Mo4 Cu3 117.6(5) . . ? C33 Mo4 Cu3 113.5(5) . . ? C32 Mo4 Cu3 136.9(6) . . ? Cu4 Mo4 Cu3 65.36(7) . . ? S6 Mo4 Mo3 100.06(14) . . ? C35 Mo4 Mo3 117.9(5) . . ? S7 Mo4 Mo3 52.10(12) . . ? S8 Mo4 Mo3 52.22(12) . . ? C31 Mo4 Mo3 130.1(6) . . ? C34 Mo4 Mo3 130.1(5) . . ? C33 Mo4 Mo3 162.1(6) . . ? C32 Mo4 Mo3 160.9(6) . . ? Cu4 Mo4 Mo3 59.25(7) . . ? Cu3 Mo4 Mo3 58.52(7) . . ? P1 Cu1 S3 118.09(18) . . ? P1 Cu1 S1 120.10(19) . . ? S3 Cu1 S1 103.64(18) . . ? P1 Cu1 S2 108.63(19) . . ? S3 Cu1 S2 103.26(18) . . ? S1 Cu1 S2 100.57(18) . . ? P1 Cu1 Mo2 139.25(17) . . ? S3 Cu1 Mo2 54.00(13) . . ? S1 Cu1 Mo2 99.59(13) . . ? S2 Cu1 Mo2 50.65(12) . . ? P1 Cu1 Mo1 152.35(17) . . ? S3 Cu1 Mo1 54.24(12) . . ? S1 Cu1 Mo1 50.89(11) . . ? S2 Cu1 Mo1 99.00(14) . . ? Mo2 Cu1 Mo1 62.13(6) . . ? P1 Cu1 Cu2 142.83(15) . . ? S3 Cu1 Cu2 98.25(13) . . ? S1 Cu1 Cu2 51.73(13) . . ? S2 Cu1 Cu2 51.30(13) . . ? Mo2 Cu1 Cu2 57.78(6) . . ? Mo1 Cu1 Cu2 57.64(6) . . ? P3 Cu2 S4 114.43(17) . . ? P3 Cu2 S2 111.74(19) . . ? S4 Cu2 S2 103.15(18) . . ? P3 Cu2 S1 121.58(19) . . ? S4 Cu2 S1 103.69(17) . . ? S2 Cu2 S1 99.86(18) . . ? P3 Cu2 Mo1 149.03(16) . . ? S4 Cu2 Mo1 54.21(12) . . ? S2 Cu2 Mo1 99.20(14) . . ? S1 Cu2 Mo1 50.73(12) . . ? P3 Cu2 Mo2 139.35(16) . . ? S4 Cu2 Mo2 54.01(12) . . ? S2 Cu2 Mo2 50.62(12) . . ? S1 Cu2 Mo2 98.74(13) . . ? Mo1 Cu2 Mo2 62.12(6) . . ? P3 Cu2 Cu1 146.81(14) . . ? S4 Cu2 Cu1 98.20(13) . . ? S2 Cu2 Cu1 51.43(13) . . ? S1 Cu2 Cu1 50.85(13) . . ? Mo1 Cu2 Cu1 57.74(6) . . ? Mo2 Cu2 Cu1 57.63(6) . . ? P2 Cu3 S7 117.23(18) . . ? P2 Cu3 S5 120.0(2) . . ? S7 Cu3 S5 104.52(18) . . ? P2 Cu3 S6 110.98(19) . . ? S7 Cu3 S6 102.71(18) . . ? S5 Cu3 S6 98.57(18) . . ? P2 Cu3 Mo3 149.92(16) . . ? S7 Cu3 Mo3 54.16(13) . . ? S5 Cu3 Mo3 51.31(12) . . ? S6 Cu3 Mo3 99.07(13) . . ? P2 Cu3 Mo4 140.57(17) . . ? S7 Cu3 Mo4 53.63(13) . . ? S5 Cu3 Mo4 98.55(14) . . ? S6 Cu3 Mo4 50.48(12) . . ? Mo3 Cu3 Mo4 62.29(7) . . ? P2 Cu3 Cu4 144.83(14) . . ? S7 Cu3 Cu4 97.35(13) . . ? S5 Cu3 Cu4 50.58(13) . . ? S6 Cu3 Cu4 50.81(13) . . ? Mo3 Cu3 Cu4 57.68(6) . . ? Mo4 Cu3 Cu4 56.93(7) . . ? P4 Cu4 S8 118.50(19) . . ? P4 Cu4 S5 118.6(2) . . ? S8 Cu4 S5 103.73(18) . . ? P4 Cu4 S6 110.15(19) . . ? S8 Cu4 S6 104.4(2) . . ? S5 Cu4 S6 98.95(18) . . ? P4 Cu4 Mo4 141.32(17) . . ? S8 Cu4 Mo4 54.63(14) . . ? S5 Cu4 Mo4 98.98(14) . . ? S6 Cu4 Mo4 50.98(12) . . ? P4 Cu4 Mo3 150.59(18) . . ? S8 Cu4 Mo3 54.12(13) . . ? S5 Cu4 Mo3 50.94(12) . . ? S6 Cu4 Mo3 99.08(13) . . ? Mo4 Cu4 Mo3 62.33(6) . . ? P4 Cu4 Cu3 143.18(15) . . ? S8 Cu4 Cu3 98.02(14) . . ? S5 Cu4 Cu3 50.29(13) . . ? S6 Cu4 Cu3 51.50(12) . . ? Mo4 Cu4 Cu3 57.71(7) . . ? Mo3 Cu4 Cu3 57.02(6) . . ? Mo1 S1 Cu1 74.30(15) . . ? Mo1 S1 Cu2 73.62(15) . . ? Cu1 S1 Cu2 77.42(17) . . ? Mo2 S2 Cu2 74.13(16) . . ? Mo2 S2 Cu1 73.90(16) . . ? Cu2 S2 Cu1 77.27(18) . . ? Cu1 S3 Mo2 74.59(14) . . ? Cu1 S3 Mo1 74.47(14) . . ? Mo2 S3 Mo1 75.73(14) . . ? Cu2 S4 Mo2 74.38(14) . . ? Cu2 S4 Mo1 74.13(14) . . ? Mo2 S4 Mo1 75.61(13) . . ? Mo3 S5 Cu3 74.04(16) . . ? Mo3 S5 Cu4 74.49(16) . . ? Cu3 S5 Cu4 79.14(18) . . ? Mo4 S6 Cu4 73.45(15) . . ? Mo4 S6 Cu3 73.74(14) . . ? Cu4 S6 Cu3 77.69(16) . . ? Cu3 S7 Mo4 74.61(15) . . ? Cu3 S7 Mo3 73.84(14) . . ? Mo4 S7 Mo3 76.06(14) . . ? Cu4 S8 Mo3 74.35(15) . . ? Cu4 S8 Mo4 73.50(15) . . ? Mo3 S8 Mo4 75.44(15) . . ? C48 P1 C54 107.3(8) . . ? C48 P1 C41 105.9(8) . . ? C54 P1 C41 105.0(9) . . ? C48 P1 Cu1 114.5(6) . . ? C54 P1 Cu1 111.5(5) . . ? C41 P1 Cu1 111.9(5) . . ? C60 P2 C66 101.0(8) . . ? C60 P2 C42 106.5(8) . . ? C66 P2 C42 102.4(8) . . ? C60 P2 Cu3 118.4(5) . . ? C66 P2 Cu3 111.7(6) . . ? C42 P2 Cu3 114.9(6) . . ? C85 P3 C79 102.8(9) . . ? C85 P3 C72 103.1(8) . . ? C79 P3 C72 104.6(8) . . ? C85 P3 Cu2 113.9(6) . . ? C79 P3 Cu2 115.2(6) . . ? C72 P3 Cu2 115.6(5) . . ? C97 P4 C91 106.9(10) . . ? C97 P4 C73 106.2(9) . . ? C91 P4 C73 104.7(8) . . ? C97 P4 Cu4 113.2(7) . . ? C91 P4 Cu4 114.3(6) . . ? C73 P4 Cu4 110.8(5) . . ? C43 N1 C42 121.4(15) . . ? C43 N1 C41 119.2(16) . . ? C42 N1 C41 117.9(15) . . ? C47 N2 C43 123(2) . . ? C74 N3 C72 117.6(14) . . ? C74 N3 C73 117.5(13) . . ? C72 N3 C73 122.1(14) . . ? C78 N4 C74 116(2) . . ? C5 C1 C2 106.6(15) . . ? C5 C1 C6 124.6(17) . . ? C2 C1 C6 127.8(17) . . ? C5 C1 Mo1 72.5(10) . . ? C2 C1 Mo1 72.7(10) . . ? C6 C1 Mo1 128.7(13) . . ? C3 C2 C1 109.6(16) . . ? C3 C2 C7 124.9(18) . . ? C1 C2 C7 124.8(16) . . ? C3 C2 Mo1 74.5(11) . . ? C1 C2 Mo1 72.1(11) . . ? C7 C2 Mo1 126.8(12) . . ? C2 C3 C4 108.5(16) . . ? C2 C3 C8 126.2(18) . . ? C4 C3 C8 125.0(17) . . ? C2 C3 Mo1 72.0(11) . . ? C4 C3 Mo1 71.6(10) . . ? C8 C3 Mo1 127.1(13) . . ? C3 C4 C5 107.6(15) . . ? C3 C4 C9 126.8(17) . . ? C5 C4 C9 124.9(16) . . ? C3 C4 Mo1 73.7(10) . . ? C5 C4 Mo1 72.1(10) . . ? C9 C4 Mo1 127.3(12) . . ? C1 C5 C4 107.6(15) . . ? C1 C5 C10 126.7(17) . . ? C4 C5 C10 125.3(16) . . ? C1 C5 Mo1 72.3(10) . . ? C4 C5 Mo1 72.8(9) . . ? C10 C5 Mo1 125.9(13) . . ? C15 C11 C12 110.6(15) . . ? C15 C11 C16 122.3(16) . . ? C12 C11 C16 126.5(15) . . ? C15 C11 Mo2 75.7(10) . . ? C12 C11 Mo2 72.7(9) . . ? C16 C11 Mo2 125.3(13) . . ? C11 C12 C13 106.1(14) . . ? C11 C12 C17 124.0(16) . . ? C13 C12 C17 129.4(17) . . ? C11 C12 Mo2 72.1(9) . . ? C13 C12 Mo2 73.8(10) . . ? C17 C12 Mo2 125.3(12) . . ? C14 C13 C12 108.9(16) . . ? C14 C13 C18 130.3(18) . . ? C12 C13 C18 120.7(17) . . ? C14 C13 Mo2 72.5(12) . . ? C12 C13 Mo2 71.0(10) . . ? C18 C13 Mo2 125.0(12) . . ? C13 C14 C15 108.8(17) . . ? C13 C14 C19 124.5(18) . . ? C15 C14 C19 126.7(18) . . ? C13 C14 Mo2 73.4(11) . . ? C15 C14 Mo2 74.1(12) . . ? C19 C14 Mo2 118.5(14) . . ? C11 C15 C14 105.3(16) . . ? C11 C15 C20 130.8(17) . . ? C14 C15 C20 123.8(17) . . ? C11 C15 Mo2 69.7(10) . . ? C14 C15 Mo2 70.7(11) . . ? C20 C15 Mo2 127.1(12) . . ? C25 C21 C22 107.7(15) . . ? C25 C21 C26 126.9(18) . . ? C22 C21 C26 125.2(18) . . ? C25 C21 Mo3 73.3(9) . . ? C22 C21 Mo3 71.4(10) . . ? C26 C21 Mo3 124.5(13) . . ? C23 C22 C21 109.1(16) . . ? C23 C22 C27 126.2(17) . . ? C21 C22 C27 124.2(17) . . ? C23 C22 Mo3 72.9(10) . . ? C21 C22 Mo3 73.5(9) . . ? C27 C22 Mo3 125.7(13) . . ? C22 C23 C24 105.4(16) . . ? C22 C23 C28 125.9(18) . . ? C24 C23 C28 128.2(18) . . ? C22 C23 Mo3 72.0(10) . . ? C24 C23 Mo3 72.7(12) . . ? C28 C23 Mo3 125.9(13) . . ? C25 C24 C23 110.6(16) . . ? C25 C24 C29 126(2) . . ? C23 C24 C29 124(2) . . ? C25 C24 Mo3 73.9(11) . . ? C23 C24 Mo3 72.2(11) . . ? C29 C24 Mo3 123.4(13) . . ? C24 C25 C30 126(2) . . ? C24 C25 C21 107.1(16) . . ? C30 C25 C21 127.2(18) . . ? C24 C25 Mo3 72.0(11) . . ? C30 C25 Mo3 124.3(13) . . ? C21 C25 Mo3 72.1(11) . . ? C32 C31 C35 106.0(19) . . ? C32 C31 C36 126(2) . . ? C35 C31 C36 127(2) . . ? C32 C31 Mo4 75.3(12) . . ? C35 C31 Mo4 70.2(11) . . ? C36 C31 Mo4 128.4(15) . . ? C31 C32 C33 109.5(18) . . ? C31 C32 C37 128(2) . . ? C33 C32 C37 123(2) . . ? C31 C32 Mo4 70.4(12) . . ? C33 C32 Mo4 70.6(12) . . ? C37 C32 Mo4 124.6(15) . . ? C32 C33 C34 107.4(18) . . ? C32 C33 C38 128(2) . . ? C34 C33 C38 124(2) . . ? C32 C33 Mo4 74.2(14) . . ? C34 C33 Mo4 71.6(12) . . ? C38 C33 Mo4 126.9(15) . . ? C35 C34 C33 105.6(17) . . ? C35 C34 C39 127.0(18) . . ? C33 C34 C39 126.7(19) . . ? C35 C34 Mo4 70.4(10) . . ? C33 C34 Mo4 72.4(12) . . ? C39 C34 Mo4 128.8(14) . . ? C34 C35 C31 111.3(18) . . ? C34 C35 C40 123.7(18) . . ? C31 C35 C40 124.7(19) . . ? C34 C35 Mo4 74.5(10) . . ? C31 C35 Mo4 73.8(11) . . ? C40 C35 Mo4 123.3(14) . . ? N1 C41 P1 116.1(12) . . ? N1 C42 P2 115.8(12) . . ? N2 C43 N1 113.2(18) . . ? N2 C43 C44 118(2) . . ? N1 C43 C44 128.2(19) . . ? C45 C44 C43 124(2) . . ? C44 C45 C46 114(2) . . ? C47 C46 C45 122(3) . . ? N2 C47 C46 119(2) . . ? C53 C48 C49 115.1(16) . . ? C53 C48 P1 125.3(14) . . ? C49 C48 P1 119.4(12) . . ? C50 C49 C48 121.2(16) . . ? C49 C50 C51 120.7(19) . . ? C52 C51 C50 119.6(18) . . ? C51 C52 C53 120.0(17) . . ? C52 C53 C48 123.3(17) . . ? C55 C54 C59 117.0(17) . . ? C55 C54 P1 124.2(15) . . ? C59 C54 P1 118.2(13) . . ? C56 C55 C54 121(2) . . ? C57 C56 C55 120.1(19) . . ? C56 C57 C58 121(2) . . ? C59 C58 C57 120(2) . . ? C58 C59 C54 120.1(19) . . ? C61 C60 C65 120.3(16) . . ? C61 C60 P2 121.1(13) . . ? C65 C60 P2 118.6(12) . . ? C60 C61 C62 120.9(17) . . ? C63 C62 C61 119.4(18) . . ? C62 C63 C64 121.8(18) . . ? C63 C64 C65 116.1(16) . . ? C60 C65 C64 121.3(16) . . ? C67 C66 C71 117.4(18) . . ? C67 C66 P2 119.6(13) . . ? C71 C66 P2 122.8(13) . . ? C66 C67 C68 117(2) . . ? C69 C68 C67 125(2) . . ? C70 C69 C68 115(2) . . ? C69 C70 C71 121(2) . . ? C70 C71 C66 124(2) . . ? N3 C72 P3 114.3(11) . . ? N3 C73 P4 114.1(11) . . ? C75 C74 N3 121.3(17) . . ? C75 C74 N4 122(2) . . ? N3 C74 N4 116.4(16) . . ? C74 C75 C76 118(2) . . ? C75 C76 C77 123(2) . . ? C76 C77 C78 113(2) . . ? N4 C78 C77 128(2) . . ? C84 C79 C80 119.3(17) . . ? C84 C79 P3 121.1(14) . . ? C80 C79 P3 119.1(14) . . ? C81 C80 C79 117.2(19) . . ? C80 C81 C82 121.8(19) . . ? C83 C82 C81 117.5(19) . . ? C82 C83 C84 126(2) . . ? C79 C84 C83 117.6(17) . . ? C90 C85 C86 118.5(18) . . ? C90 C85 P3 122.5(16) . . ? C86 C85 P3 118.8(14) . . ? C87 C86 C85 121(2) . . ? C86 C87 C88 119(2) . . ? C89 C88 C87 119(2) . . ? C88 C89 C90 122(2) . . ? C85 C90 C89 120(2) . . ? C96 C91 C92 122.1(18) . . ? C96 C91 P4 116.3(14) . . ? C92 C91 P4 121.1(16) . . ? C93 C92 C91 116(2) . . ? C94 C93 C92 124(2) . . ? C93 C94 C95 120(2) . . ? C94 C95 C96 120(2) . . ? C91 C96 C95 118(2) . . ? C98 C97 C102 119(2) . . ? C98 C97 P4 124.4(19) . . ? C102 C97 P4 116.2(15) . . ? C97 C98 C99 123(2) . . ? C98 C99 C100 118(2) . . ? C101 C100 C99 121(2) . . ? C100 C101 C102 118(3) . . ? C97 C102 C101 119(2) . . ? O3 Cl1 O2 111.0(11) . . ? O3 Cl1 O4 108.9(9) . . ? O2 Cl1 O4 107.3(9) . . ? O3 Cl1 O1 108.6(10) . . ? O2 Cl1 O1 112.6(10) . . ? O4 Cl1 O1 108.4(9) . . ? O8 Cl2 O6 109.7(12) . . ? O8 Cl2 O7 110.5(18) . . ? O6 Cl2 O7 109.7(11) . . ? O8 Cl2 O5 107.3(14) . . ? O6 Cl2 O5 112.5(9) . . ? O7 Cl2 O5 107.1(12) . . ? O9 Cl3 O10 106.4(12) . . ? O9 Cl3 O11 109.6(15) . . ? O10 Cl3 O11 111.5(13) . . ? O9 Cl3 O12 109.9(12) . . ? O10 Cl3 O12 110.2(9) . . ? O11 Cl3 O12 109.3(10) . . ? O13A Cl4 O15A 111.7(12) . . ? O13A Cl4 O15 65(2) . . ? O15A Cl4 O15 85(2) . . ? O13A Cl4 O14 169.2(18) . . ? O15A Cl4 O14 57.6(18) . . ? O15 Cl4 O14 111.0(10) . . ? O13A Cl4 O16 83(2) . . ? O15A Cl4 O16 163(2) . . ? O15 Cl4 O16 110.1(11) . . ? O14 Cl4 O16 108.2(11) . . ? O13A Cl4 O14A 110.3(12) . . ? O15A Cl4 O14A 110.1(12) . . ? O15 Cl4 O14A 165(2) . . ? O14 Cl4 O14A 76(2) . . ? O16 Cl4 O14A 55(2) . . ? O13A Cl4 O13 65.3(19) . . ? O15A Cl4 O13 71.4(19) . . ? O15 Cl4 O13 109.8(10) . . ? O14 Cl4 O13 108.9(11) . . ? O16 Cl4 O13 108.7(11) . . ? O14A Cl4 O13 79(2) . . ? O13A Cl4 O16A 108.9(11) . . ? O15A Cl4 O16A 108.6(11) . . ? O15 Cl4 O16A 63(2) . . ? O14 Cl4 O16A 76(2) . . ? O16 Cl4 O16A 73(2) . . ? O14A Cl4 O16A 107.2(11) . . ? O13 Cl4 O16A 173(2) . . ? N5 C104 C103 161(4) . . ? N6 C106 C105 172(5) . . ? N7 C108 C107 174(4) . . ? Cl5 C109 Cl6 105(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.154 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.142 #===END #============================================================================== data_6^.^2CH~2~Cl~2~ _database_code_depnum_ccdc_archive 'CCDC 783845' #TrackingRef '- JPLangCIF.cif' #============================================================================== # CHEMICAL DATA _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H94 Cu4 Mo4 N4 P2 S8, 2(C H2 Cl2), 4(P F6)' _chemical_formula_sum 'C78 H98 Cl4 Cu4 F24 Mo4 N4 P6 S8' _chemical_formula_weight 2769.62 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' 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.490(3) _cell_length_b 13.234(3) _cell_length_c 18.823(4) _cell_angle_alpha 75.91(3) _cell_angle_beta 73.76(3) _cell_angle_gamma 71.05(3) _cell_volume 2785.1(13) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13054 _cell_measurement_theta_min 3.0021 _cell_measurement_theta_max 27.4739 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.79 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 1.595 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3655 _exptl_absorpt_correction_T_max 0.6912 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24479 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.44 _reflns_number_total 12434 _reflns_number_gt 9136 _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 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0993P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12434 _refine_ls_number_parameters 531 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.2073 _refine_ls_wR_factor_gt 0.1896 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.061 _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 0.76980(4) 0.26489(4) 0.18213(2) 0.03944(15) Uani 1 1 d . A . Mo2 Mo 0.75387(4) 0.48008(4) 0.19723(2) 0.03672(15) Uani 1 1 d . . . Cu1 Cu 0.56309(6) 0.39525(6) 0.25109(3) 0.03982(19) Uani 1 1 d . A . Cu2 Cu 0.67135(6) 0.44233(7) 0.08662(4) 0.0466(2) Uani 1 1 d . . . S1 S 0.59727(13) 0.29607(14) 0.15472(8) 0.0464(4) Uani 1 1 d . A . S2 S 0.57778(12) 0.56566(12) 0.17344(7) 0.0411(3) Uani 1 1 d . A . S3 S 0.73047(12) 0.33388(13) 0.29285(7) 0.0424(3) Uani 1 1 d . A . S4 S 0.85909(12) 0.38914(13) 0.09672(7) 0.0429(3) Uani 1 1 d . A . P1 P 0.39935(12) 0.41530(12) 0.33890(7) 0.0351(3) Uani 1 1 d . . . P2 P 0.0468(3) 0.7889(2) 0.2014(2) 0.1182(12) Uani 1 1 d . . . P3 P 0.3105(3) 0.0671(2) 0.3246(2) 0.1131(11) Uani 1 1 d . . . F1 F 0.0278(11) 0.8421(9) 0.2677(6) 0.229(5) Uani 1 1 d U . . F2 F 0.0733(10) 0.7376(7) 0.1271(6) 0.210(5) Uani 1 1 d U . . F3 F -0.0807(8) 0.8212(8) 0.1999(8) 0.228(5) Uani 1 1 d U . . F4 F 0.0499(8) 0.6729(6) 0.2444(5) 0.172(3) Uani 1 1 d U . . F5 F 0.1805(7) 0.7581(6) 0.1950(7) 0.188(4) Uani 1 1 d U . . F6 F 0.0511(8) 0.9007(6) 0.1516(6) 0.173(3) Uani 1 1 d U . . F7 F 0.2939(12) 0.0210(8) 0.4109(5) 0.219(5) Uani 1 1 d U . . F8 F 0.3178(13) 0.1144(7) 0.2418(5) 0.225(6) Uani 1 1 d U . . F9 F 0.3950(8) 0.1290(7) 0.3263(6) 0.186(4) Uani 1 1 d U . . F10 F 0.2074(8) 0.1724(6) 0.3407(6) 0.172(3) Uani 1 1 d U . . F11 F 0.2234(9) 0.0089(7) 0.3258(7) 0.211(5) Uani 1 1 d U . . F12 F 0.4135(8) -0.0361(6) 0.3107(5) 0.162(3) Uani 1 1 d U . . N1 N 0.2928(4) 0.3674(4) 0.2453(2) 0.0443(11) Uani 1 1 d . . . H1 H 0.2955 0.2990 0.2574 0.053 Uiso 1 1 calc R A . N2 N 0.3445(4) 0.4934(4) 0.0161(2) 0.0459(12) Uani 1 1 d . . . C11 C 0.7955(7) 0.5539(7) 0.2846(4) 0.066(2) Uani 1 1 d . A . C12 C 0.7402(6) 0.6451(7) 0.2344(5) 0.075(3) Uani 1 1 d . A . C13 C 0.8134(8) 0.6414(7) 0.1626(4) 0.071(2) Uani 1 1 d . A . C14 C 0.9132(6) 0.5534(7) 0.1684(4) 0.063(2) Uani 1 1 d . A . C15 C 0.8999(6) 0.5017(7) 0.2419(4) 0.0640(19) Uani 1 1 d . A . C16 C 0.7515(10) 0.5309(10) 0.3681(6) 0.1091(16) Uani 1 1 d . . . H16A H 0.7701 0.4532 0.3852 0.164 Uiso 1 1 calc R A . H16B H 0.6681 0.5617 0.3803 0.164 Uiso 1 1 calc R . . H16C H 0.7879 0.5629 0.3928 0.164 Uiso 1 1 calc R . . C17 C 0.6336(9) 0.7276(10) 0.2575(6) 0.1091(16) Uani 1 1 d . . . H17A H 0.5770 0.6932 0.2923 0.164 Uiso 1 1 calc R A . H17B H 0.6031 0.7686 0.2138 0.164 Uiso 1 1 calc R . . H17C H 0.6497 0.7760 0.2820 0.164 Uiso 1 1 calc R . . C18 C 0.7961(10) 0.7220(10) 0.0936(6) 0.1091(16) Uani 1 1 d . . . H18A H 0.8413 0.7725 0.0860 0.164 Uiso 1 1 calc R A . H18B H 0.7146 0.7611 0.0989 0.164 Uiso 1 1 calc R . . H18C H 0.8211 0.6848 0.0508 0.164 Uiso 1 1 calc R . . C19 C 1.0219(9) 0.5260(10) 0.1068(6) 0.1091(16) Uani 1 1 d . . . H19A H 1.0770 0.5620 0.1092 0.164 Uiso 1 1 calc R A . H19B H 1.0014 0.5504 0.0582 0.164 Uiso 1 1 calc R . . H19C H 1.0567 0.4482 0.1138 0.164 Uiso 1 1 calc R . . C20 C 0.9909(9) 0.4063(9) 0.2751(6) 0.1091(16) Uani 1 1 d . . . H20A H 1.0499 0.4329 0.2829 0.164 Uiso 1 1 calc R A . H20B H 1.0266 0.3547 0.2407 0.164 Uiso 1 1 calc R . . H20C H 0.9538 0.3711 0.3228 0.164 Uiso 1 1 calc R . . C21 C 0.2674(5) 0.4263(6) 0.3051(3) 0.0460(14) Uani 1 1 d . A . H21A H 0.2114 0.3991 0.3472 0.055 Uiso 1 1 calc R . . H21B H 0.2310 0.5029 0.2880 0.055 Uiso 1 1 calc R . . C22 C 0.3133(5) 0.4102(5) 0.1703(3) 0.0379(12) Uani 1 1 d . A . C23 C 0.3346(5) 0.3430(5) 0.1165(3) 0.0462(14) Uani 1 1 d . . . H23 H 0.3385 0.2690 0.1319 0.055 Uiso 1 1 calc R A . C24 C 0.3492(5) 0.3877(5) 0.0425(3) 0.0478(14) Uani 1 1 d . A . H24 H 0.3635 0.3423 0.0075 0.057 Uiso 1 1 calc R . . C25 C 0.3269(5) 0.5558(5) 0.0675(3) 0.0440(13) Uani 1 1 d . A . H25 H 0.3240 0.6293 0.0505 0.053 Uiso 1 1 calc R . . C26 C 0.3129(5) 0.5180(5) 0.1433(3) 0.0400(12) Uani 1 1 d . . . H26 H 0.3031 0.5645 0.1767 0.048 Uiso 1 1 calc R A . C27 C 0.4032(5) 0.3078(5) 0.4212(3) 0.0431(13) Uani 1 1 d . A . C28 C 0.3042(6) 0.3083(6) 0.4778(3) 0.0573(17) Uani 1 1 d . . . H28 H 0.2350 0.3634 0.4739 0.069 Uiso 1 1 calc R A . C29 C 0.3083(8) 0.2252(8) 0.5414(4) 0.073(2) Uani 1 1 d . A . H29 H 0.2419 0.2247 0.5802 0.087 Uiso 1 1 calc R . . C30 C 0.4100(8) 0.1454(7) 0.5460(4) 0.073(2) Uani 1 1 d . . . H30 H 0.4125 0.0903 0.5883 0.088 Uiso 1 1 calc R A . C31 C 0.5067(7) 0.1443(6) 0.4908(4) 0.0652(19) Uani 1 1 d . A . H31 H 0.5756 0.0887 0.4945 0.078 Uiso 1 1 calc R . . C32 C 0.5030(6) 0.2274(6) 0.4278(4) 0.0529(15) Uani 1 1 d . . . H32 H 0.5703 0.2276 0.3898 0.063 Uiso 1 1 calc R A . C33 C 0.3654(5) 0.5402(5) 0.3748(3) 0.0405(12) Uani 1 1 d . A . C34 C 0.3846(6) 0.5428(6) 0.4436(3) 0.0545(16) Uani 1 1 d . . . H34 H 0.4079 0.4776 0.4762 0.065 Uiso 1 1 calc R A . C35 C 0.3697(7) 0.6403(7) 0.4641(4) 0.0654(19) Uani 1 1 d . A . H35 H 0.3869 0.6406 0.5096 0.079 Uiso 1 1 calc R . . C36 C 0.3306(7) 0.7366(7) 0.4197(4) 0.071(2) Uani 1 1 d . . . H36 H 0.3189 0.8025 0.4350 0.085 Uiso 1 1 calc R A . C37 C 0.3081(8) 0.7359(7) 0.3514(5) 0.075(2) Uani 1 1 d . A . H37 H 0.2797 0.8017 0.3210 0.090 Uiso 1 1 calc R . . C38 C 0.3274(6) 0.6392(6) 0.3282(4) 0.0591(17) Uani 1 1 d . . . H38 H 0.3152 0.6394 0.2811 0.071 Uiso 1 1 calc R A . C1 C 0.8386(5) 0.0906(6) 0.2524(3) 0.071(3) Uiso 0.639(7) 1 d PG A 1 C2 C 0.7701(5) 0.0756(6) 0.2097(3) 0.067(3) Uiso 0.639(7) 1 d PG A 1 C3 C 0.8235(5) 0.0973(5) 0.1332(3) 0.063(3) Uiso 0.639(7) 1 d PG A 1 C4 C 0.9250(5) 0.1256(5) 0.1285(3) 0.052(2) Uiso 0.639(7) 1 d PG A 1 C5 C 0.9344(5) 0.1215(5) 0.2022(3) 0.063(3) Uiso 0.639(7) 1 d PG A 1 C6 C 0.8139(8) 0.0761(9) 0.3363(5) 0.119(6) Uiso 0.639(7) 1 d PG A 1 H6A H 0.7407 0.1270 0.3541 0.178 Uiso 0.639(7) 1 calc PR A 1 H6B H 0.8756 0.0894 0.3514 0.178 Uiso 0.639(7) 1 calc PR A 1 H6C H 0.8095 0.0027 0.3575 0.178 Uiso 0.639(7) 1 calc PR A 1 C7 C 0.6599(8) 0.0424(9) 0.2403(5) 0.119(6) Uiso 0.639(7) 1 d PG A 1 H7A H 0.6198 0.0697 0.2869 0.178 Uiso 0.639(7) 1 calc PR A 1 H7B H 0.6779 -0.0360 0.2497 0.178 Uiso 0.639(7) 1 calc PR A 1 H7C H 0.6107 0.0720 0.2042 0.178 Uiso 0.639(7) 1 calc PR A 1 C8 C 0.7800(8) 0.0912(9) 0.0682(4) 0.097(5) Uiso 0.639(7) 1 d PG A 1 H8A H 0.7950 0.0159 0.0643 0.146 Uiso 0.639(7) 1 calc PR A 1 H8B H 0.8197 0.1279 0.0223 0.146 Uiso 0.639(7) 1 calc PR A 1 H8C H 0.6973 0.1258 0.0759 0.146 Uiso 0.639(7) 1 calc PR A 1 C9 C 1.0084(7) 0.1550(8) 0.0577(4) 0.084(4) Uiso 0.639(7) 1 d PG A 1 H9A H 1.0558 0.1926 0.0682 0.127 Uiso 0.639(7) 1 calc PR A 1 H9B H 0.9655 0.2018 0.0206 0.127 Uiso 0.639(7) 1 calc PR A 1 H9C H 1.0578 0.0897 0.0385 0.127 Uiso 0.639(7) 1 calc PR A 1 C10 C 1.0293(8) 0.1457(9) 0.2234(5) 0.118(6) Uiso 0.639(7) 1 d PG A 1 H10A H 1.0832 0.0784 0.2404 0.177 Uiso 0.639(7) 1 calc PR A 1 H10B H 0.9962 0.1885 0.2634 0.177 Uiso 0.639(7) 1 calc PR A 1 H10C H 1.0702 0.1861 0.1801 0.177 Uiso 0.639(7) 1 calc PR A 1 C1A C 0.9014(7) 0.1073(8) 0.2388(4) 0.067(2) Uiso 0.361(7) 1 d PG A 2 C2A C 0.8061(7) 0.0748(8) 0.2340(4) 0.067(2) Uiso 0.361(7) 1 d PG A 2 C3A C 0.8076(7) 0.0855(8) 0.1568(4) 0.067(2) Uiso 0.361(7) 1 d PG A 2 C4A C 0.9037(7) 0.1247(8) 0.1138(4) 0.067(2) Uiso 0.361(7) 1 d PG A 2 C5A C 0.9618(7) 0.1381(8) 0.1646(4) 0.067(2) Uiso 0.361(7) 1 d PG A 2 C6A C 0.9330(11) 0.1089(13) 0.3104(6) 0.067(2) Uiso 0.361(7) 1 d PG A 2 H6A1 H 0.9806 0.0377 0.3276 0.100 Uiso 0.361(7) 1 calc PR A 2 H6A2 H 0.8628 0.1280 0.3485 0.100 Uiso 0.361(7) 1 calc PR A 2 H6A3 H 0.9759 0.1619 0.3009 0.100 Uiso 0.361(7) 1 calc PR A 2 C7A C 0.7186(11) 0.0358(12) 0.2995(6) 0.067(2) Uiso 0.361(7) 1 d PG A 2 H7A1 H 0.6450 0.0537 0.2851 0.100 Uiso 0.361(7) 1 calc PR A 2 H7A2 H 0.7083 0.0706 0.3416 0.100 Uiso 0.361(7) 1 calc PR A 2 H7A3 H 0.7463 -0.0422 0.3138 0.100 Uiso 0.361(7) 1 calc PR A 2 C8A C 0.7219(11) 0.0599(13) 0.1257(6) 0.067(2) Uiso 0.361(7) 1 d PG A 2 H8A1 H 0.6784 0.0167 0.1650 0.100 Uiso 0.361(7) 1 calc PR A 2 H8A2 H 0.7634 0.0196 0.0849 0.100 Uiso 0.361(7) 1 calc PR A 2 H8A3 H 0.6690 0.1268 0.1073 0.100 Uiso 0.361(7) 1 calc PR A 2 C9A C 0.9383(11) 0.1479(13) 0.0292(6) 0.067(2) Uiso 0.361(7) 1 d PG A 2 H9A1 H 1.0108 0.0956 0.0120 0.100 Uiso 0.361(7) 1 calc PR A 2 H9A2 H 0.9482 0.2204 0.0132 0.100 Uiso 0.361(7) 1 calc PR A 2 H9A3 H 0.8783 0.1427 0.0080 0.100 Uiso 0.361(7) 1 calc PR A 2 C10A C 1.0688(11) 0.1781(12) 0.1433(6) 0.067(2) Uiso 0.361(7) 1 d PG A 2 H10D H 1.0728 0.2078 0.1845 0.100 Uiso 0.361(7) 1 calc PR A 2 H10E H 1.0650 0.2340 0.0991 0.100 Uiso 0.361(7) 1 calc PR A 2 H10F H 1.1373 0.1183 0.1326 0.100 Uiso 0.361(7) 1 calc PR A 2 C39 C 0.3558(19) -0.0524(15) 0.1233(11) 0.105(6) Uiso 0.50 1 d PD . . H39A H 0.4019 -0.0553 0.1586 0.126 Uiso 0.50 1 calc PR . . H39B H 0.2770 -0.0527 0.1515 0.126 Uiso 0.50 1 calc PR . . Cl1 Cl 0.415(2) -0.1559(19) 0.0784(13) 0.423(13) Uiso 0.50 1 d PD . . Cl2 Cl 0.3530(12) 0.0701(11) 0.0514(8) 0.248(5) Uiso 0.50 1 d PD . . C40 C -0.023(2) 0.3133(19) 0.5305(17) 0.084(8) Uiso 0.319(3) 1 d PD A 1 H40A H -0.0744 0.3053 0.5804 0.101 Uiso 0.319(3) 1 calc PR A 1 H40B H -0.0779 0.3405 0.4969 0.101 Uiso 0.319(3) 1 calc PR A 1 Cl3 Cl 0.006(4) 0.184(2) 0.522(2) 0.45(2) Uiso 0.319(3) 1 d PD A 1 Cl4 Cl -0.0166(17) 0.4378(15) 0.5336(10) 0.215(7) Uiso 0.319(3) 1 d PD . 1 C40A C 0.013(4) 0.243(3) 0.486(3) 0.096(16) Uiso 0.181(3) 1 d PD A 2 H40C H 0.0093 0.2075 0.5388 0.116 Uiso 0.181(3) 1 calc PR A 2 H40D H 0.0932 0.2167 0.4590 0.116 Uiso 0.181(3) 1 calc PR A 2 Cl3A Cl -0.076(3) 0.201(3) 0.4504(17) 0.200(11) Uiso 0.181(3) 1 d PD A 2 Cl4A Cl -0.013(3) 0.381(3) 0.484(2) 0.248(16) Uiso 0.181(3) 1 d PD 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 0.0390(3) 0.0367(3) 0.0359(2) -0.0037(2) -0.0053(2) -0.0057(2) Mo2 0.0383(3) 0.0429(3) 0.0295(2) -0.00473(19) -0.00536(19) -0.0146(2) Cu1 0.0370(4) 0.0461(5) 0.0337(3) -0.0060(3) -0.0042(3) -0.0115(3) Cu2 0.0494(4) 0.0556(5) 0.0318(3) -0.0051(3) -0.0124(3) -0.0091(4) S1 0.0471(8) 0.0481(10) 0.0474(8) -0.0141(7) -0.0091(6) -0.0142(7) S2 0.0424(7) 0.0403(9) 0.0356(6) -0.0046(6) -0.0061(6) -0.0083(6) S3 0.0435(8) 0.0489(9) 0.0309(6) 0.0014(6) -0.0094(6) -0.0123(7) S4 0.0415(7) 0.0477(9) 0.0327(6) -0.0063(6) -0.0001(6) -0.0104(6) P1 0.0376(7) 0.0398(9) 0.0276(6) -0.0033(5) -0.0066(5) -0.0125(6) P2 0.124(2) 0.0547(17) 0.201(3) -0.0526(19) -0.106(2) 0.0249(15) P3 0.154(3) 0.0541(17) 0.163(3) 0.0259(18) -0.106(2) -0.0426(19) F1 0.315(14) 0.177(10) 0.220(10) -0.133(8) -0.090(9) 0.001(9) F2 0.297(12) 0.111(7) 0.254(10) -0.072(7) -0.176(9) 0.028(7) F3 0.148(7) 0.130(8) 0.443(18) -0.101(9) -0.148(9) 0.021(6) F4 0.218(9) 0.071(5) 0.207(8) -0.011(5) -0.068(7) -0.004(5) F5 0.147(6) 0.081(5) 0.372(13) -0.060(6) -0.157(8) 0.021(4) F6 0.181(8) 0.057(4) 0.264(10) -0.030(5) -0.087(7) 0.023(4) F7 0.374(15) 0.123(8) 0.169(8) 0.015(6) -0.144(9) -0.037(9) F8 0.463(18) 0.120(7) 0.151(7) 0.043(6) -0.162(9) -0.124(10) F9 0.193(8) 0.114(7) 0.310(12) -0.055(7) -0.122(8) -0.051(6) F10 0.188(8) 0.074(5) 0.236(9) 0.005(5) -0.064(7) -0.019(5) F11 0.209(9) 0.095(6) 0.375(14) 0.058(7) -0.178(9) -0.078(6) F12 0.169(7) 0.080(5) 0.235(9) -0.016(5) -0.062(6) -0.026(5) N1 0.057(3) 0.042(3) 0.039(2) 0.001(2) -0.020(2) -0.017(2) N2 0.055(3) 0.045(3) 0.037(2) -0.006(2) -0.020(2) -0.005(2) C11 0.080(5) 0.088(6) 0.049(3) -0.023(4) -0.001(4) -0.052(5) C12 0.052(4) 0.080(6) 0.113(7) -0.060(5) -0.001(4) -0.026(4) C13 0.106(6) 0.065(5) 0.064(4) 0.012(4) -0.037(4) -0.054(5) C14 0.053(4) 0.083(6) 0.065(4) -0.023(4) 0.003(3) -0.040(4) C15 0.055(4) 0.076(6) 0.077(5) -0.015(4) -0.026(4) -0.027(4) C16 0.115(4) 0.121(4) 0.119(4) -0.036(3) -0.022(3) -0.060(3) C17 0.115(4) 0.121(4) 0.119(4) -0.036(3) -0.022(3) -0.060(3) C18 0.115(4) 0.121(4) 0.119(4) -0.036(3) -0.022(3) -0.060(3) C19 0.115(4) 0.121(4) 0.119(4) -0.036(3) -0.022(3) -0.060(3) C20 0.115(4) 0.121(4) 0.119(4) -0.036(3) -0.022(3) -0.060(3) C21 0.040(3) 0.063(4) 0.033(3) -0.013(3) -0.004(2) -0.010(3) C22 0.040(3) 0.037(3) 0.036(3) -0.005(2) -0.015(2) -0.006(2) C23 0.061(4) 0.034(3) 0.045(3) -0.004(2) -0.025(3) -0.006(3) C24 0.062(4) 0.040(4) 0.044(3) -0.010(3) -0.021(3) -0.007(3) C25 0.053(3) 0.043(4) 0.039(3) -0.009(2) -0.016(3) -0.010(3) C26 0.044(3) 0.045(4) 0.033(2) -0.007(2) -0.011(2) -0.011(3) C27 0.055(3) 0.046(4) 0.037(3) -0.004(2) -0.016(3) -0.023(3) C28 0.054(4) 0.065(5) 0.042(3) -0.003(3) -0.003(3) -0.012(3) C29 0.080(5) 0.084(6) 0.048(4) 0.010(4) -0.005(4) -0.037(5) C30 0.116(7) 0.058(5) 0.050(4) 0.013(3) -0.020(4) -0.044(5) C31 0.089(5) 0.042(4) 0.060(4) 0.010(3) -0.026(4) -0.017(4) C32 0.057(4) 0.049(4) 0.053(3) 0.002(3) -0.013(3) -0.022(3) C33 0.043(3) 0.037(3) 0.038(3) -0.006(2) -0.004(2) -0.010(2) C34 0.064(4) 0.054(4) 0.048(3) -0.008(3) -0.014(3) -0.018(3) C35 0.081(5) 0.061(5) 0.066(4) -0.030(4) -0.019(4) -0.019(4) C36 0.088(6) 0.049(5) 0.074(5) -0.025(4) -0.018(4) -0.008(4) C37 0.094(6) 0.046(5) 0.083(5) -0.010(4) -0.033(5) -0.006(4) C38 0.073(5) 0.044(4) 0.051(3) -0.008(3) -0.012(3) -0.004(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 2.2406(17) . ? Mo1 S4 2.3308(17) . ? Mo1 S3 2.3412(16) . ? Mo1 C5 2.350(7) . ? Mo1 C4 2.380(6) . ? Mo1 C1 2.381(7) . ? Mo1 C3A 2.405(10) . ? Mo1 C2A 2.408(10) . ? Mo1 C4A 2.416(10) . ? Mo1 C1A 2.421(10) . ? Mo1 C5A 2.427(9) . ? Mo1 C3 2.430(6) . ? Mo2 S2 2.2376(17) . ? Mo2 C15 2.330(6) . ? Mo2 S4 2.3336(17) . ? Mo2 S3 2.3336(17) . ? Mo2 C11 2.349(6) . ? Mo2 C14 2.365(6) . ? Mo2 C13 2.369(7) . ? Mo2 C12 2.392(7) . ? Mo2 Cu2 2.7726(10) . ? Mo2 Cu1 2.7924(11) . ? Cu1 P1 2.2261(17) . ? Cu1 S3 2.2701(17) . ? Cu1 S1 2.3574(17) . ? Cu1 S2 2.4019(18) . ? Cu1 Cu2 3.0112(13) . ? Cu2 N2 1.950(4) 2_665 ? Cu2 S4 2.2676(17) . ? Cu2 S1 2.3532(19) . ? Cu2 S2 2.3859(18) . ? P1 C33 1.816(6) . ? P1 C27 1.830(6) . ? P1 C21 1.879(6) . ? P2 F1 1.505(8) . ? P2 F3 1.516(9) . ? P2 F4 1.545(8) . ? P2 F6 1.556(9) . ? P2 F5 1.561(8) . ? P2 F2 1.607(9) . ? P3 F11 1.516(8) . ? P3 F8 1.520(8) . ? P3 F9 1.542(8) . ? P3 F12 1.560(9) . ? P3 F7 1.571(9) . ? P3 F10 1.586(9) . ? N1 C22 1.372(7) . ? N1 C21 1.429(7) . ? N1 H1 0.8700 . ? N2 C25 1.348(7) . ? N2 C24 1.353(8) . ? N2 Cu2 1.950(4) 2_665 ? C11 C15 1.386(11) . ? C11 C12 1.448(12) . ? C11 C16 1.503(11) . ? C12 C13 1.405(11) . ? C12 C17 1.455(13) . ? C13 C14 1.412(12) . ? C13 C18 1.485(13) . ? C14 C15 1.377(10) . ? C14 C19 1.525(12) . ? C15 C20 1.536(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 C26 1.392(8) . ? C22 C23 1.421(8) . ? C23 C24 1.361(8) . ? C23 H23 0.9400 . ? C24 H24 0.9400 . ? C25 C26 1.374(7) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? C27 C32 1.365(9) . ? C27 C28 1.388(8) . ? C28 C29 1.415(10) . ? C28 H28 0.9400 . ? C29 C30 1.371(12) . ? C29 H29 0.9400 . ? C30 C31 1.354(11) . ? C30 H30 0.9400 . ? C31 C32 1.407(9) . ? C31 H31 0.9400 . ? C32 H32 0.9400 . ? C33 C34 1.391(8) . ? C33 C38 1.407(9) . ? C34 C35 1.378(9) . ? C34 H34 0.9400 . ? C35 C36 1.366(11) . ? C35 H35 0.9400 . ? C36 C37 1.392(11) . ? C36 H36 0.9400 . ? C37 C38 1.378(10) . ? C37 H37 0.9400 . ? C38 H38 0.9400 . ? C1 C5 1.410(3) . ? C1 C2 1.410(3) . ? C1 C6 1.498(4) . ? C2 C3 1.410(3) . ? C2 C7 1.499(4) . ? C3 C4 1.410(3) . ? C3 C8 1.499(4) . ? C4 C5 1.410(3) . ? C4 C9 1.499(4) . ? C5 C10 1.498(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C1A C5A 1.421(4) . ? C1A C2A 1.422(4) . ? C1A C6A 1.512(5) . ? C2A C3A 1.421(4) . ? C2A C7A 1.511(5) . ? C3A C4A 1.422(4) . ? C3A C8A 1.512(5) . ? C4A C5A 1.423(4) . ? C4A C9A 1.511(5) . ? C5A C10A 1.512(5) . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C6A H6A3 0.9700 . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C7A H7A3 0.9700 . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C8A H8A3 0.9700 . ? C9A H9A1 0.9700 . ? C9A H9A2 0.9700 . ? C9A H9A3 0.9700 . ? C10A H10D 0.9700 . ? C10A H10E 0.9700 . ? C10A H10F 0.9700 . ? C39 Cl1 1.642(17) . ? C39 Cl2 1.839(15) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 Cl3 1.666(18) . ? C40 Cl4 1.694(17) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? Cl4 Cl4 1.90(3) 2_566 ? C40A Cl4A 1.73(2) . ? C40A Cl3A 1.75(2) . ? C40A H40C 0.9800 . ? C40A H40D 0.9800 . ? 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 106.19(6) . . ? S1 Mo1 S3 105.87(6) . . ? S4 Mo1 S3 100.35(6) . . ? S1 Mo1 C5 140.32(15) . . ? S4 Mo1 C5 99.85(14) . . ? S3 Mo1 C5 98.11(14) . . ? S1 Mo1 C4 116.87(13) . . ? S4 Mo1 C4 87.39(14) . . ? S3 Mo1 C4 132.44(13) . . ? C5 Mo1 C4 34.69(11) . . ? S1 Mo1 C1 115.00(15) . . ? S4 Mo1 C1 134.32(14) . . ? S3 Mo1 C1 87.00(15) . . ? C5 Mo1 C1 34.67(11) . . ? C4 Mo1 C1 57.26(17) . . ? S1 Mo1 C3A 85.3(2) . . ? S4 Mo1 C3A 120.45(19) . . ? S3 Mo1 C3A 133.1(2) . . ? C5 Mo1 C3A 55.5(2) . . ? C4 Mo1 C3A 39.8(2) . . ? C1 Mo1 C3A 48.4(2) . . ? S1 Mo1 C2A 100.0(2) . . ? S4 Mo1 C2A 141.5(2) . . ? S3 Mo1 C2A 98.9(2) . . ? C5 Mo1 C2A 44.4(2) . . ? C4 Mo1 C2A 55.4(2) . . ? C1 Mo1 C2A 16.9(2) . . ? C3A Mo1 C2A 34.36(15) . . ? S1 Mo1 C4A 106.6(2) . . ? S4 Mo1 C4A 88.4(2) . . ? S3 Mo1 C4A 142.4(2) . . ? C5 Mo1 C4A 44.2(2) . . ? C4 Mo1 C4A 10.5(2) . . ? C1 Mo1 C4A 62.2(2) . . ? C3A Mo1 C4A 34.31(15) . . ? C2A Mo1 C4A 57.0(2) . . ? S1 Mo1 C1A 134.2(2) . . ? S4 Mo1 C1A 114.63(19) . . ? S3 Mo1 C1A 86.7(2) . . ? C5 Mo1 C1A 17.1(2) . . ? C4 Mo1 C1A 48.7(2) . . ? C1 Mo1 C1A 20.1(2) . . ? C3A Mo1 C1A 56.9(2) . . ? C2A Mo1 C1A 34.25(15) . . ? C4A Mo1 C1A 56.8(2) . . ? S1 Mo1 C5A 140.0(2) . . ? S4 Mo1 C5A 85.3(2) . . ? S3 Mo1 C5A 109.5(2) . . ? C5 Mo1 C5A 17.0(2) . . ? C4 Mo1 C5A 23.7(2) . . ? C1 Mo1 C5A 50.4(2) . . ? C3A Mo1 C5A 56.9(2) . . ? C2A Mo1 C5A 56.8(2) . . ? C4A Mo1 C5A 34.17(15) . . ? C1A Mo1 C5A 34.10(15) . . ? S1 Mo1 C3 85.78(14) . . ? S4 Mo1 C3 110.17(13) . . ? S3 Mo1 C3 142.88(14) . . ? C5 Mo1 C3 56.99(17) . . ? C4 Mo1 C3 34.07(10) . . ? C1 Mo1 C3 56.60(16) . . ? C3A Mo1 C3 10.6(2) . . ? C2A Mo1 C3 43.9(2) . . ? C4A Mo1 C3 26.5(2) . . ? C1A Mo1 C3 61.9(2) . . ? C5A Mo1 C3 54.6(2) . . ? S2 Mo2 C15 142.6(2) . . ? S2 Mo2 S4 106.18(6) . . ? C15 Mo2 S4 102.4(2) . . ? S2 Mo2 S3 106.04(6) . . ? C15 Mo2 S3 91.8(2) . . ? S4 Mo2 S3 100.49(6) . . ? S2 Mo2 C11 112.5(2) . . ? C15 Mo2 C11 34.4(3) . . ? S4 Mo2 C11 136.7(2) . . ? S3 Mo2 C11 87.1(2) . . ? S2 Mo2 C14 126.8(2) . . ? C15 Mo2 C14 34.1(3) . . ? S4 Mo2 C14 84.07(18) . . ? S3 Mo2 C14 123.6(2) . . ? C11 Mo2 C14 57.5(2) . . ? S2 Mo2 C13 93.0(2) . . ? C15 Mo2 C13 57.3(3) . . ? S4 Mo2 C13 102.2(2) . . ? S3 Mo2 C13 144.81(18) . . ? C11 Mo2 C13 58.1(3) . . ? C14 Mo2 C13 34.7(3) . . ? S2 Mo2 C12 85.1(2) . . ? C15 Mo2 C12 57.5(3) . . ? S4 Mo2 C12 136.4(2) . . ? S3 Mo2 C12 117.0(2) . . ? C11 Mo2 C12 35.5(3) . . ? C14 Mo2 C12 57.4(3) . . ? C13 Mo2 C12 34.3(3) . . ? S2 Mo2 Cu2 55.65(5) . . ? C15 Mo2 Cu2 152.24(19) . . ? S4 Mo2 Cu2 51.86(4) . . ? S3 Mo2 Cu2 102.24(5) . . ? C11 Mo2 Cu2 166.4(2) . . ? C14 Mo2 Cu2 122.08(18) . . ? C13 Mo2 Cu2 112.93(17) . . ? C12 Mo2 Cu2 131.2(3) . . ? S2 Mo2 Cu1 55.74(4) . . ? C15 Mo2 Cu1 138.90(19) . . ? S4 Mo2 Cu1 102.34(5) . . ? S3 Mo2 Cu1 51.63(5) . . ? C11 Mo2 Cu1 114.99(16) . . ? C14 Mo2 Cu1 172.38(17) . . ? C13 Mo2 Cu1 144.7(2) . . ? C12 Mo2 Cu1 117.93(18) . . ? Cu2 Mo2 Cu1 65.51(3) . . ? S2 Mo2 Mo1 99.39(5) . . ? C15 Mo2 Mo1 117.3(2) . . ? S4 Mo2 Mo1 52.01(5) . . ? S3 Mo2 Mo1 52.28(4) . . ? C11 Mo2 Mo1 134.5(2) . . ? C14 Mo2 Mo1 124.8(2) . . ? C13 Mo2 Mo1 153.6(2) . . ? C12 Mo2 Mo1 169.1(3) . . ? Cu2 Mo2 Mo1 58.33(3) . . ? Cu1 Mo2 Mo1 58.48(3) . . ? P1 Cu1 S3 116.21(6) . . ? P1 Cu1 S1 121.24(6) . . ? S3 Cu1 S1 104.39(7) . . ? P1 Cu1 S2 111.28(7) . . ? S3 Cu1 S2 102.80(6) . . ? S1 Cu1 S2 98.05(6) . . ? P1 Cu1 Mo1 150.47(5) . . ? S3 Cu1 Mo1 54.33(4) . . ? S1 Cu1 Mo1 51.11(5) . . ? S2 Cu1 Mo1 98.25(5) . . ? P1 Cu1 Mo2 139.46(5) . . ? S3 Cu1 Mo2 53.70(4) . . ? S1 Cu1 Mo2 98.55(5) . . ? S2 Cu1 Mo2 50.35(5) . . ? Mo1 Cu1 Mo2 62.12(3) . . ? P1 Cu1 Cu2 146.16(5) . . ? S3 Cu1 Cu2 96.95(5) . . ? S1 Cu1 Cu2 50.20(5) . . ? S2 Cu1 Cu2 50.79(5) . . ? Mo1 Cu1 Cu2 56.67(4) . . ? Mo2 Cu1 Cu2 56.93(3) . . ? N2 Cu2 S4 111.83(16) 2_665 . ? N2 Cu2 S1 122.51(16) 2_665 . ? S4 Cu2 S1 104.58(7) . . ? N2 Cu2 S2 113.51(16) 2_665 . ? S4 Cu2 S2 103.51(6) . . ? S1 Cu2 S2 98.62(6) . . ? N2 Cu2 Mo1 147.26(16) 2_665 . ? S4 Cu2 Mo1 54.33(5) . . ? S1 Cu2 Mo1 51.37(5) . . ? S2 Cu2 Mo1 99.07(5) . . ? N2 Cu2 Mo2 138.15(16) 2_665 . ? S4 Cu2 Mo2 54.04(5) . . ? S1 Cu2 Mo2 99.21(5) . . ? S2 Cu2 Mo2 50.74(4) . . ? Mo1 Cu2 Mo2 62.57(3) . . ? N2 Cu2 Cu1 150.02(15) 2_665 . ? S4 Cu2 Cu1 97.66(5) . . ? S1 Cu2 Cu1 50.33(5) . . ? S2 Cu2 Cu1 51.27(4) . . ? Mo1 Cu2 Cu1 57.16(4) . . ? Mo2 Cu2 Cu1 57.56(3) . . ? Mo1 S1 Cu2 73.51(6) . . ? Mo1 S1 Cu1 73.91(6) . . ? Cu2 S1 Cu1 79.47(6) . . ? Mo2 S2 Cu2 73.62(5) . . ? Mo2 S2 Cu1 73.92(6) . . ? Cu2 S2 Cu1 77.94(6) . . ? Cu1 S3 Mo2 74.67(6) . . ? Cu1 S3 Mo1 73.70(5) . . ? Mo2 S3 Mo1 75.69(5) . . ? Cu2 S4 Mo1 73.45(6) . . ? Cu2 S4 Mo2 74.10(5) . . ? Mo1 S4 Mo2 75.89(5) . . ? C33 P1 C27 105.5(3) . . ? C33 P1 C21 104.7(3) . . ? C27 P1 C21 106.1(3) . . ? C33 P1 Cu1 110.49(18) . . ? C27 P1 Cu1 114.6(2) . . ? C21 P1 Cu1 114.57(17) . . ? F1 P2 F3 94.6(7) . . ? F1 P2 F4 98.0(6) . . ? F3 P2 F4 95.0(6) . . ? F1 P2 F6 86.9(6) . . ? F3 P2 F6 87.0(6) . . ? F4 P2 F6 174.6(6) . . ? F1 P2 F5 89.3(6) . . ? F3 P2 F5 174.9(8) . . ? F4 P2 F5 87.7(5) . . ? F6 P2 F5 89.9(5) . . ? F1 P2 F2 175.8(8) . . ? F3 P2 F2 87.7(6) . . ? F4 P2 F2 85.4(5) . . ? F6 P2 F2 89.7(6) . . ? F5 P2 F2 88.2(6) . . ? F11 P3 F8 92.2(6) . . ? F11 P3 F9 177.4(7) . . ? F8 P3 F9 89.2(6) . . ? F11 P3 F12 91.5(5) . . ? F8 P3 F12 94.8(6) . . ? F9 P3 F12 90.6(5) . . ? F11 P3 F7 85.3(6) . . ? F8 P3 F7 176.2(8) . . ? F9 P3 F7 93.2(6) . . ? F12 P3 F7 88.2(5) . . ? F11 P3 F10 89.7(6) . . ? F8 P3 F10 86.5(6) . . ? F9 P3 F10 88.2(5) . . ? F12 P3 F10 178.2(6) . . ? F7 P3 F10 90.6(6) . . ? C22 N1 C21 125.1(5) . . ? C22 N1 H1 117.4 . . ? C21 N1 H1 117.4 . . ? C25 N2 C24 116.5(5) . . ? C25 N2 Cu2 121.2(4) . 2_665 ? C24 N2 Cu2 120.9(4) . 2_665 ? C15 C11 C12 106.7(6) . . ? C15 C11 C16 128.0(9) . . ? C12 C11 C16 124.9(8) . . ? C15 C11 Mo2 72.0(4) . . ? C12 C11 Mo2 73.8(4) . . ? C16 C11 Mo2 124.6(5) . . ? C13 C12 C11 106.8(7) . . ? C13 C12 C17 128.2(10) . . ? C11 C12 C17 124.9(8) . . ? C13 C12 Mo2 72.0(4) . . ? C11 C12 Mo2 70.6(4) . . ? C17 C12 Mo2 126.1(6) . . ? C12 C13 C14 108.3(7) . . ? C12 C13 C18 126.5(10) . . ? C14 C13 C18 124.9(8) . . ? C12 C13 Mo2 73.7(4) . . ? C14 C13 Mo2 72.5(4) . . ? C18 C13 Mo2 124.5(6) . . ? C15 C14 C13 107.7(7) . . ? C15 C14 C19 125.3(9) . . ? C13 C14 C19 126.7(8) . . ? C15 C14 Mo2 71.6(4) . . ? C13 C14 Mo2 72.8(4) . . ? C19 C14 Mo2 125.5(5) . . ? C14 C15 C11 110.4(8) . . ? C14 C15 C20 125.8(8) . . ? C11 C15 C20 123.6(8) . . ? C14 C15 Mo2 74.3(4) . . ? C11 C15 Mo2 73.5(4) . . ? C20 C15 Mo2 123.4(6) . . ? 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 . . ? N1 C21 P1 113.1(4) . . ? N1 C21 H21A 109.0 . . ? P1 C21 H21A 109.0 . . ? N1 C21 H21B 109.0 . . ? P1 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? N1 C22 C26 123.2(5) . . ? N1 C22 C23 119.3(5) . . ? C26 C22 C23 117.4(5) . . ? C24 C23 C22 118.8(6) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? N2 C24 C23 124.1(5) . . ? N2 C24 H24 117.9 . . ? C23 C24 H24 117.9 . . ? N2 C25 C26 123.8(6) . . ? N2 C25 H25 118.1 . . ? C26 C25 H25 118.1 . . ? C25 C26 C22 119.3(5) . . ? C25 C26 H26 120.3 . . ? C22 C26 H26 120.3 . . ? C32 C27 C28 119.5(6) . . ? C32 C27 P1 120.6(5) . . ? C28 C27 P1 119.9(5) . . ? C27 C28 C29 119.4(7) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C30 C29 C28 119.5(7) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C31 C30 C29 121.4(7) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 119.2(7) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C27 C32 C31 121.0(6) . . ? C27 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C34 C33 C38 118.5(6) . . ? C34 C33 P1 122.9(5) . . ? C38 C33 P1 118.4(4) . . ? C35 C34 C33 120.3(7) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C36 C35 C34 121.3(7) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 119.3(7) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C38 C37 C36 120.4(8) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C33 120.2(7) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? C5 C1 C2 108.0 . . ? C5 C1 C6 126.0 . . ? C2 C1 C6 126.0 . . ? C5 C1 Mo1 71.4(2) . . ? C2 C1 Mo1 74.9(2) . . ? C6 C1 Mo1 119.5(2) . . ? C3 C2 C1 108.0 . . ? C3 C2 C7 126.0 . . ? C1 C2 C7 126.0 . . ? C3 C2 Mo1 73.1(2) . . ? C1 C2 Mo1 71.1(2) . . ? C7 C2 Mo1 121.6(2) . . ? C2 C3 C4 108.0 . . ? C2 C3 C8 126.0 . . ? C4 C3 C8 126.0 . . ? C2 C3 Mo1 73.2(2) . . ? C4 C3 Mo1 71.0(2) . . ? C8 C3 Mo1 121.5(2) . . ? C3 C4 C5 108.0 . . ? C3 C4 C9 126.0 . . ? C5 C4 C9 126.0 . . ? C3 C4 Mo1 74.9(2) . . ? C5 C4 Mo1 71.5(2) . . ? C9 C4 Mo1 119.5(2) . . ? C1 C5 C4 108.0 . . ? C1 C5 C10 126.0 . . ? C4 C5 C10 126.0 . . ? C1 C5 Mo1 73.9(2) . . ? C4 C5 Mo1 73.8(2) . . ? C10 C5 Mo1 118.2(2) . . ? C5A C1A C2A 108.1 . . ? C5A C1A C6A 126.0 . . ? C2A C1A C6A 126.0 . . ? C5A C1A Mo1 73.2(3) . . ? C2A C1A Mo1 72.4(3) . . ? C6A C1A Mo1 120.3(3) . . ? C3A C2A C1A 108.0 . . ? C3A C2A C7A 126.0 . . ? C1A C2A C7A 126.0 . . ? C3A C2A Mo1 72.7(3) . . ? C1A C2A Mo1 73.4(3) . . ? C7A C2A Mo1 119.8(3) . . ? C2A C3A C4A 108.0 . . ? C2A C3A C8A 126.0 . . ? C4A C3A C8A 125.9 . . ? C2A C3A Mo1 72.9(3) . . ? C4A C3A Mo1 73.3(3) . . ? C8A C3A Mo1 119.6(3) . . ? C3A C4A C5A 108.0 . . ? C3A C4A C9A 126.1 . . ? C5A C4A C9A 126.0 . . ? C3A C4A Mo1 72.4(3) . . ? C5A C4A Mo1 73.3(3) . . ? C9A C4A Mo1 120.1(3) . . ? C1A C5A C4A 108.0 . . ? C1A C5A C10A 126.0 . . ? C4A C5A C10A 126.0 . . ? C1A C5A Mo1 72.7(3) . . ? C4A C5A Mo1 72.5(3) . . ? C10A C5A Mo1 120.5(3) . . ? C1A C6A H6A1 109.5 . . ? C1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C2A C7A H7A1 109.5 . . ? C2A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C2A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C3A C8A H8A1 109.5 . . ? C3A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C3A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C4A C9A H9A1 109.5 . . ? C4A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C4A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C5A C10A H10D 109.5 . . ? C5A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C5A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? Cl1 C39 Cl2 106.4(14) . . ? Cl1 C39 H39A 110.5 . . ? Cl2 C39 H39A 110.5 . . ? Cl1 C39 H39B 110.5 . . ? Cl2 C39 H39B 110.5 . . ? H39A C39 H39B 108.6 . . ? Cl3 C40 Cl4 166(3) . . ? Cl3 C40 H40A 94.5 . . ? Cl4 C40 H40A 94.5 . . ? Cl3 C40 H40B 94.5 . . ? Cl4 C40 H40B 94.5 . . ? H40A C40 H40B 103.2 . . ? C40 Cl4 Cl4 139(2) . 2_566 ? Cl4A C40A Cl3A 119(3) . . ? Cl4A C40A H40C 107.6 . . ? Cl3A C40A H40C 107.6 . . ? Cl4A C40A H40D 107.6 . . ? Cl3A C40A H40D 107.6 . . ? H40C C40A H40D 107.1 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.651 _refine_diff_density_min -1.357 _refine_diff_density_rms 0.130 #===END