# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2147 data_mm9719 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H26 Co Mo O7 P' _chemical_formula_weight 732.39 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 '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' '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.502(2) _cell_length_b 21.848(3) _cell_length_c 10.2900(10) _cell_angle_alpha 91.850(10) _cell_angle_beta 108.330(10) _cell_angle_gamma 71.290(10) _cell_volume 3124.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _exptl_crystal_description ? _exptl_crystal_colour 'v dark' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method ? _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method ' omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -2.6% _diffrn_reflns_number 11453 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.1403 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 25.02 _reflns_number_total 11008 _reflns_number_observed 6667 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 37 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+10.6492P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10971 _refine_ls_number_parameters 797 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1353 _refine_ls_R_factor_obs 0.0531 _refine_ls_wR_factor_all 0.1596 _refine_ls_wR_factor_obs 0.1095 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.047 _refine_ls_restrained_S_all 1.163 _refine_ls_restrained_S_obs 1.047 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.21576(5) 0.07363(3) 0.24574(6) 0.0180(2) Uani 1 d . . Co1 Co 0.22014(7) 0.12152(5) 0.01080(10) 0.0194(2) Uani 1 d . . P1 P 0.35031(14) 0.11249(9) 0.3306(2) 0.0198(4) Uani 1 d . . C5 C 0.2675(6) 0.0091(4) 0.1296(8) 0.028(2) Uani 1 d . . O5 O 0.2953(4) -0.0377(3) 0.0747(6) 0.0380(15) Uani 1 d . . O6 O 0.3864(5) 0.1353(3) -0.0437(6) 0.043(2) Uani 1 d . . C6 C 0.3237(6) 0.1281(4) -0.0189(8) 0.029(2) Uani 1 d . . O7 O 0.1564(5) 0.0706(3) -0.2545(6) 0.045(2) Uani 1 d . . C7 C 0.1814(6) 0.0885(4) -0.1486(8) 0.026(2) Uani 1 d . . O9 O -0.0627(4) 0.1486(3) -0.0066(6) 0.0334(14) Uani 1 d . . C9 C -0.1457(7) 0.1328(6) -0.0886(10) 0.059(3) Uani 1 d . . H9A H -0.2041(7) 0.1684(15) -0.0914(58) 0.088 Uiso 1 calc R . H9B H -0.1465(27) 0.0931(19) -0.0482(40) 0.088 Uiso 1 calc R . H9C H -0.1429(26) 0.1262(33) -0.1821(21) 0.088 Uiso 1 calc R . O8 O 0.0282(4) 0.0593(3) -0.0781(6) 0.0377(15) Uani 1 d . . C8 C 0.0218(6) 0.1078(4) -0.0155(8) 0.027(2) Uani 1 d . . C4 C 0.1034(5) 0.1300(4) 0.0655(7) 0.022(2) Uani 1 d . . C3 C 0.1010(5) 0.1940(3) 0.0300(7) 0.017(2) Uani 1 d . . O10 O -0.0109(4) 0.2245(3) -0.1999(5) 0.040(2) Uani 1 d . . C10 C 0.0189(6) 0.2374(4) -0.0842(8) 0.027(2) Uani 1 d . . O11 O -0.0199(4) 0.2940(3) -0.0344(5) 0.0305(13) Uani 1 d . . C11 C -0.1005(6) 0.3408(4) -0.1360(9) 0.044(2) Uani 1 d . . H11A H -0.1235(28) 0.3806(11) -0.0927(17) 0.066 Uiso 1 calc R . H11B H -0.1526(18) 0.3225(12) -0.1727(44) 0.066 Uiso 1 calc R . H11C H -0.0795(13) 0.3506(22) -0.2109(32) 0.066 Uiso 1 calc R . C1 C 0.2454(5) 0.1554(3) 0.2062(7) 0.017(2) Uani 1 d . . C2 C 0.1856(5) 0.2085(3) 0.1041(7) 0.017(2) Uani 1 d . . C71 C 0.2085(5) 0.2668(3) 0.0761(7) 0.021(2) Uani 1 d . . C72 C 0.1901(6) 0.2899(4) -0.0584(8) 0.027(2) Uani 1 d . . H72 H 0.1614(6) 0.2685(4) -0.1331(8) 0.032 Uiso 1 calc R . C73 C 0.2131(7) 0.3435(4) -0.0845(9) 0.042(2) Uani 1 d . . H73 H 0.2031(7) 0.3572(4) -0.1763(9) 0.051 Uiso 1 calc R . C74 C 0.2503(7) 0.3769(4) 0.0219(10) 0.048(3) Uani 1 d . . H74 H 0.2630(7) 0.4149(4) 0.0036(10) 0.057 Uiso 1 calc R . C75 C 0.2693(8) 0.3550(4) 0.1549(10) 0.055(3) Uani 1 d . . H75 H 0.2958(8) 0.3777(4) 0.2288(10) 0.066 Uiso 1 calc R . C76 C 0.2494(6) 0.2992(4) 0.1817(9) 0.035(2) Uani 1 d . . H76 H 0.2644(6) 0.2837(4) 0.2741(9) 0.042 Uiso 1 calc R . C81 C 0.1785(7) 0.0788(4) 0.4489(8) 0.037(2) Uani 1 d . . H81 H 0.1816(7) 0.1133(4) 0.5147(8) 0.044 Uiso 1 calc R . C82 C 0.2507(6) 0.0183(4) 0.4596(8) 0.030(2) Uani 1 d . . H82 H 0.3150(6) 0.0037(4) 0.5326(8) 0.036 Uiso 1 calc R . C83 C 0.2153(6) -0.0195(4) 0.3588(8) 0.033(2) Uani 1 d . . H83 H 0.2492(6) -0.0657(4) 0.3471(8) 0.040 Uiso 1 calc R . C84 C 0.1185(6) 0.0184(4) 0.2808(8) 0.030(2) Uani 1 d . . H84 H 0.0721(6) 0.0028(4) 0.2078(8) 0.036 Uiso 1 calc R . C85 C 0.0972(6) 0.0783(4) 0.3379(8) 0.030(2) Uani 1 d . . H85 H 0.0325(6) 0.1125(4) 0.3128(8) 0.036 Uiso 1 calc R . C51 C 0.3716(5) 0.1533(4) 0.4878(7) 0.022(2) Uani 1 d . . C52 C 0.2980(6) 0.2038(4) 0.5103(8) 0.031(2) Uani 1 d . . H52 H 0.2366(6) 0.2182(4) 0.4418(8) 0.037 Uiso 1 calc R . C53 C 0.3141(7) 0.2336(4) 0.6331(9) 0.038(2) Uani 1 d . . H53 H 0.2636(7) 0.2684(4) 0.6486(9) 0.046 Uiso 1 calc R . C54 C 0.4027(7) 0.2127(4) 0.7319(8) 0.035(2) Uani 1 d . . H54 H 0.4136(7) 0.2339(4) 0.8147(8) 0.042 Uiso 1 calc R . C55 C 0.4748(7) 0.1626(5) 0.7135(8) 0.042(2) Uani 1 d . . H55 H 0.5350(7) 0.1477(5) 0.7845(8) 0.051 Uiso 1 calc R . C56 C 0.4611(6) 0.1331(4) 0.5919(8) 0.031(2) Uani 1 d . . H56 H 0.5127(6) 0.0988(4) 0.5784(8) 0.037 Uiso 1 calc R . C61 C 0.4606(5) 0.0929(4) 0.2853(7) 0.023(2) Uani 1 d . . C62 C 0.5070(6) 0.1385(4) 0.2910(9) 0.033(2) Uani 1 d . . H62 H 0.4851(6) 0.1793(4) 0.3264(9) 0.040 Uiso 1 calc R . C63 C 0.5856(7) 0.1238(5) 0.2445(10) 0.046(2) Uani 1 d . . H63 H 0.6176(7) 0.1547(5) 0.2484(10) 0.055 Uiso 1 calc R . C64 C 0.6184(7) 0.0644(5) 0.1920(9) 0.050(3) Uani 1 d . . H64 H 0.6711(7) 0.0552(5) 0.1578(9) 0.060 Uiso 1 calc R . C65 C 0.5731(6) 0.0190(4) 0.1905(9) 0.043(2) Uani 1 d . . H65 H 0.5965(6) -0.0220(4) 0.1571(9) 0.051 Uiso 1 calc R . C66 C 0.4936(6) 0.0320(4) 0.2369(8) 0.033(2) Uani 1 d . . H66 H 0.4631(6) 0.0005(4) 0.2356(8) 0.040 Uiso 1 calc R . Mo1' Mo 0.89956(5) 0.34320(3) 0.37827(6) 0.0186(2) Uani 1 d . . Co1' Co 0.72316(7) 0.43134(5) 0.34111(10) 0.0212(2) Uani 1 d . . P1' P 0.79972(14) 0.27808(9) 0.2819(2) 0.0199(4) Uani 1 d . . C5' C 0.8484(5) 0.4056(4) 0.2170(8) 0.026(2) Uani 1 d . . O5' O 0.8338(4) 0.4385(3) 0.1210(6) 0.0390(15) Uani 1 d . . O6' O 0.5461(4) 0.4440(3) 0.1151(7) 0.050(2) Uani 1 d . . C6' C 0.6160(6) 0.4361(4) 0.2040(8) 0.027(2) Uani 1 d . . O7' O 0.6902(5) 0.5670(3) 0.2755(7) 0.059(2) Uani 1 d . . C7' C 0.7080(6) 0.5139(4) 0.3044(9) 0.033(2) Uani 1 d . . O9' O 0.9460(4) 0.4475(3) 0.6913(5) 0.0332(14) Uani 1 d . . C9' C 0.9957(7) 0.4916(4) 0.7568(9) 0.044(2) Uani 1 d . . H9'A H 1.0373(33) 0.4735(14) 0.8498(23) 0.066 Uiso 1 calc R . H9'B H 0.9486(7) 0.5333(10) 0.7618(54) 0.066 Uiso 1 calc R . H9'C H 1.0349(33) 0.4979(22) 0.7034(34) 0.066 Uiso 1 calc R . O8' O 0.8868(4) 0.5114(3) 0.4958(6) 0.0349(14) Uani 1 d . . C8' C 0.8902(6) 0.4646(4) 0.5590(8) 0.026(2) Uani 1 d . . C4' C 0.8415(5) 0.4163(4) 0.5060(7) 0.023(2) Uani 1 d . . C3' C 0.7645(5) 0.4131(3) 0.5528(7) 0.022(2) Uani 1 d . . O10' O 0.7395(5) 0.5120(3) 0.6643(6) 0.044(2) Uani 1 d . . C10' C 0.7294(5) 0.4598(4) 0.6482(7) 0.025(2) Uani 1 d . . O11' O 0.6877(4) 0.4352(3) 0.7203(5) 0.0315(13) Uani 1 d . . C11' C 0.6491(6) 0.4778(4) 0.8161(8) 0.037(2) Uani 1 d . . H11D H 0.6133(34) 0.4577(13) 0.8544(44) 0.055 Uiso 1 calc R . H11E H 0.6061(32) 0.5196(10) 0.7674(15) 0.055 Uiso 1 calc R . H11F H 0.7023(7) 0.4845(22) 0.8906(32) 0.055 Uiso 1 calc R . C1' C 0.7786(5) 0.3313(3) 0.4036(7) 0.021(2) Uani 1 d . . C2' C 0.7239(5) 0.3652(3) 0.4879(7) 0.015(2) Uani 1 d . . C71' C 0.6412(6) 0.3471(4) 0.5004(7) 0.028(2) Uani 1 d . . C72' C 0.5515(6) 0.3929(5) 0.4845(8) 0.037(2) Uani 1 d . . H72' H 0.5419(6) 0.4374(5) 0.4669(8) 0.045 Uiso 1 calc R . C73' C 0.4763(7) 0.3743(5) 0.4940(9) 0.047(3) Uani 1 d . . H73' H 0.4155(7) 0.4059(5) 0.4845(9) 0.056 Uiso 1 calc R . C74' C 0.4903(7) 0.3087(6) 0.5175(9) 0.051(3) Uani 1 d . . H74' H 0.4386(7) 0.2955(6) 0.5225(9) 0.061 Uiso 1 calc R . C75' C 0.5800(7) 0.2624(5) 0.5338(9) 0.045(2) Uani 1 d . . H75' H 0.5906(7) 0.2176(5) 0.5502(9) 0.054 Uiso 1 calc R . C76' C 0.6520(6) 0.2838(4) 0.5252(8) 0.031(2) Uani 1 d . . H76' H 0.7135(6) 0.2525(4) 0.5375(8) 0.037 Uiso 1 calc R . C81' C 1.0388(6) 0.2572(4) 0.4894(10) 0.037(2) Uani 1 d . . H81' H 1.0418(6) 0.2170(4) 0.5371(10) 0.045 Uiso 1 calc R . C82' C 1.0375(6) 0.2643(4) 0.3523(9) 0.038(2) Uani 1 d . . H82' H 1.0369(6) 0.2300(4) 0.2856(9) 0.046 Uiso 1 calc R . C83' C 1.0480(6) 0.3237(4) 0.3305(9) 0.030(2) Uani 1 d . . H83' H 1.0550(6) 0.3395(4) 0.2455(9) 0.036 Uiso 1 calc R . C84' C 1.0506(5) 0.3564(4) 0.4510(9) 0.032(2) Uani 1 d . . H84' H 1.0629(5) 0.3987(4) 0.4676(9) 0.039 Uiso 1 calc R . C85' C 1.0462(5) 0.3154(4) 0.5506(9) 0.035(2) Uani 1 d . . H85' H 1.0564(5) 0.3232(4) 0.6498(9) 0.042 Uiso 1 calc R . C51' C 0.8336(5) 0.1932(3) 0.3401(7) 0.019(2) Uani 1 d . . C52' C 0.8786(6) 0.1721(4) 0.4792(8) 0.028(2) Uani 1 d . . H52' H 0.8898(6) 0.2024(4) 0.5453(8) 0.034 Uiso 1 calc R . C53' C 0.9066(6) 0.1072(4) 0.5201(9) 0.029(2) Uani 1 d . . H53' H 0.9359(6) 0.0932(4) 0.6149(9) 0.034 Uiso 1 calc R . C54' C 0.8921(6) 0.0618(4) 0.4233(9) 0.031(2) Uani 1 d . . H54' H 0.9103(6) 0.0173(4) 0.4520(9) 0.037 Uiso 1 calc R . C55' C 0.8511(6) 0.0827(4) 0.2854(9) 0.032(2) Uani 1 d . . H55' H 0.8430(6) 0.0522(4) 0.2185(9) 0.039 Uiso 1 calc R . C56' C 0.8217(5) 0.1482(3) 0.2446(8) 0.025(2) Uani 1 d . . H56' H 0.7930(5) 0.1622(3) 0.1498(8) 0.030 Uiso 1 calc R . C61' C 0.6981(5) 0.2917(4) 0.1249(7) 0.022(2) Uani 1 d . . C62' C 0.6139(6) 0.2870(4) 0.1286(8) 0.035(2) Uani 1 d . . H62' H 0.6092(6) 0.2747(4) 0.2131(8) 0.041 Uiso 1 calc R . C63' C 0.5345(7) 0.2998(4) 0.0106(9) 0.041(2) Uani 1 d . . H63' H 0.4755(7) 0.2971(4) 0.0147(9) 0.050 Uiso 1 calc R . C64' C 0.5419(7) 0.3166(5) -0.1131(9) 0.050(3) Uani 1 d . . H64' H 0.4881(7) 0.3251(5) -0.1945(9) 0.060 Uiso 1 calc R . C65' C 0.6283(7) 0.3210(5) -0.1175(8) 0.045(2) Uani 1 d . . H65' H 0.6333(7) 0.3326(5) -0.2023(8) 0.054 Uiso 1 calc R . C66' C 0.7067(6) 0.3087(4) -0.0006(8) 0.031(2) Uani 1 d . . H66' H 0.7658(6) 0.3115(4) -0.0042(8) 0.037 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0202(4) 0.0215(4) 0.0150(3) -0.0010(3) 0.0054(3) -0.0104(3) Co1 0.0249(6) 0.0205(5) 0.0166(5) -0.0040(4) 0.0079(4) -0.0112(5) P1 0.0204(11) 0.0227(10) 0.0183(10) -0.0009(8) 0.0055(8) -0.0104(9) C5 0.030(5) 0.029(5) 0.028(4) -0.005(4) 0.011(4) -0.012(4) O5 0.052(4) 0.025(3) 0.036(3) -0.007(3) 0.017(3) -0.009(3) O6 0.044(4) 0.062(4) 0.038(4) 0.000(3) 0.026(3) -0.023(4) C6 0.042(5) 0.031(5) 0.018(4) -0.005(3) 0.008(4) -0.019(4) O7 0.065(5) 0.055(4) 0.025(3) -0.018(3) 0.014(3) -0.035(4) C7 0.030(5) 0.022(4) 0.031(5) -0.007(3) 0.014(4) -0.011(4) O9 0.026(3) 0.045(4) 0.033(3) -0.008(3) 0.006(3) -0.019(3) C9 0.033(6) 0.106(9) 0.042(6) -0.037(6) 0.005(5) -0.037(6) O8 0.040(4) 0.043(4) 0.031(3) -0.013(3) 0.005(3) -0.023(3) C8 0.031(5) 0.039(5) 0.018(4) 0.003(4) 0.001(4) -0.025(4) C4 0.023(4) 0.027(4) 0.020(4) 0.002(3) 0.006(3) -0.014(4) C3 0.014(4) 0.019(4) 0.012(3) -0.005(3) 0.005(3) 0.003(3) O10 0.043(4) 0.045(4) 0.021(3) 0.004(3) -0.003(3) -0.012(3) C10 0.033(5) 0.030(5) 0.017(4) 0.000(3) 0.003(4) -0.016(4) O11 0.026(3) 0.030(3) 0.022(3) 0.006(2) 0.001(2) 0.001(3) C11 0.034(5) 0.052(6) 0.033(5) 0.008(4) 0.014(4) 0.007(5) C1 0.023(4) 0.014(4) 0.020(4) -0.011(3) 0.013(3) -0.009(3) C2 0.014(4) 0.024(4) 0.014(4) -0.008(3) 0.006(3) -0.004(3) C71 0.021(4) 0.020(4) 0.018(4) 0.000(3) -0.001(3) -0.007(3) C72 0.033(5) 0.025(4) 0.022(4) -0.008(3) 0.008(4) -0.011(4) C73 0.066(7) 0.033(5) 0.033(5) 0.006(4) 0.014(5) -0.023(5) C74 0.072(7) 0.033(5) 0.051(6) 0.001(4) 0.020(6) -0.033(5) C75 0.080(8) 0.035(5) 0.047(6) -0.009(5) 0.003(6) -0.035(6) C76 0.041(5) 0.032(5) 0.028(5) 0.000(4) -0.001(4) -0.017(4) C81 0.058(6) 0.053(6) 0.022(4) -0.014(4) 0.025(4) -0.036(5) C82 0.025(5) 0.044(5) 0.019(4) 0.016(4) -0.001(4) -0.016(4) C83 0.044(6) 0.026(4) 0.030(5) 0.008(4) 0.013(4) -0.012(4) C84 0.039(5) 0.041(5) 0.026(4) -0.001(4) 0.015(4) -0.027(4) C85 0.029(5) 0.037(5) 0.030(5) -0.002(4) 0.024(4) -0.003(4) C51 0.024(4) 0.037(5) 0.014(4) -0.007(3) 0.012(3) -0.018(4) C52 0.028(5) 0.049(5) 0.019(4) -0.007(4) 0.008(4) -0.019(4) C53 0.041(6) 0.047(6) 0.036(5) -0.014(4) 0.018(5) -0.023(5) C54 0.052(6) 0.043(5) 0.022(4) -0.016(4) 0.017(4) -0.030(5) C55 0.046(6) 0.061(6) 0.021(4) 0.002(4) 0.001(4) -0.028(5) C56 0.037(5) 0.027(4) 0.025(4) -0.001(3) 0.004(4) -0.010(4) C61 0.017(4) 0.026(4) 0.024(4) 0.000(3) 0.005(3) -0.007(3) C62 0.029(5) 0.032(5) 0.041(5) 0.001(4) 0.009(4) -0.014(4) C63 0.038(6) 0.058(6) 0.060(6) -0.007(5) 0.024(5) -0.032(5) C64 0.029(5) 0.087(8) 0.039(6) -0.017(5) 0.021(5) -0.018(6) C65 0.031(5) 0.039(5) 0.049(6) -0.024(5) 0.014(5) -0.002(4) C66 0.025(5) 0.029(5) 0.036(5) -0.004(4) 0.008(4) 0.002(4) Mo1' 0.0185(4) 0.0174(3) 0.0207(3) -0.0008(3) 0.0057(3) -0.0076(3) Co1' 0.0207(6) 0.0190(5) 0.0210(5) 0.0030(4) 0.0035(5) -0.0053(5) P1' 0.0214(11) 0.0204(10) 0.0199(10) -0.0026(8) 0.0063(8) -0.0100(9) C5' 0.020(4) 0.030(4) 0.027(4) 0.001(4) 0.006(4) -0.010(4) O5' 0.041(4) 0.041(4) 0.031(3) 0.012(3) 0.008(3) -0.011(3) O6' 0.031(4) 0.050(4) 0.046(4) 0.004(3) -0.011(3) -0.005(3) C6' 0.026(5) 0.022(4) 0.028(4) 0.003(3) 0.006(4) -0.002(4) O7' 0.055(5) 0.019(3) 0.082(5) 0.022(3) 0.002(4) -0.002(3) C7' 0.027(5) 0.025(5) 0.037(5) 0.006(4) 0.007(4) 0.002(4) O9' 0.042(4) 0.030(3) 0.025(3) 0.001(2) -0.002(3) -0.021(3) C9' 0.062(7) 0.041(5) 0.029(5) -0.006(4) 0.000(5) -0.032(5) O8' 0.042(4) 0.027(3) 0.037(3) -0.001(3) 0.004(3) -0.022(3) C8' 0.025(4) 0.033(5) 0.025(4) -0.008(4) 0.010(4) -0.013(4) C4' 0.024(4) 0.025(4) 0.021(4) -0.002(3) 0.005(3) -0.011(4) C3' 0.020(4) 0.023(4) 0.017(4) 0.005(3) -0.004(3) -0.008(3) O10' 0.060(5) 0.028(3) 0.053(4) -0.016(3) 0.028(4) -0.020(3) C10' 0.021(4) 0.027(5) 0.021(4) -0.005(3) 0.009(3) 0.002(4) O11' 0.036(3) 0.035(3) 0.030(3) -0.008(3) 0.017(3) -0.014(3) C11' 0.040(5) 0.040(5) 0.025(4) -0.014(4) 0.021(4) 0.004(4) C1' 0.020(4) 0.023(4) 0.021(4) 0.002(3) -0.002(3) -0.015(3) C2' 0.021(4) 0.010(3) 0.010(3) 0.001(3) 0.005(3) 0.001(3) C71' 0.024(5) 0.044(5) 0.017(4) 0.002(4) 0.003(3) -0.015(4) C72' 0.028(5) 0.054(6) 0.026(5) 0.011(4) 0.000(4) -0.016(5) C73' 0.026(5) 0.075(8) 0.033(5) 0.006(5) 0.003(4) -0.015(5) C74' 0.050(7) 0.088(8) 0.033(5) -0.003(5) 0.018(5) -0.042(6) C75' 0.064(7) 0.055(6) 0.042(6) -0.019(5) 0.030(5) -0.042(6) C76' 0.033(5) 0.031(5) 0.039(5) -0.006(4) 0.018(4) -0.018(4) C81' 0.025(5) 0.024(5) 0.058(6) 0.015(4) 0.010(4) -0.005(4) C82' 0.022(5) 0.045(6) 0.047(6) -0.014(4) 0.006(4) -0.017(4) C83' 0.027(5) 0.028(5) 0.037(5) -0.003(4) 0.021(4) -0.003(4) C84' 0.018(4) 0.031(5) 0.050(5) 0.000(4) 0.003(4) -0.017(4) C85' 0.010(4) 0.051(6) 0.035(5) 0.011(4) 0.001(4) -0.002(4) C51' 0.019(4) 0.020(4) 0.019(4) 0.001(3) 0.007(3) -0.005(3) C52' 0.031(5) 0.029(4) 0.028(4) 0.000(3) 0.010(4) -0.012(4) C53' 0.025(5) 0.027(4) 0.039(5) 0.001(4) 0.017(4) -0.006(4) C54' 0.032(5) 0.022(4) 0.043(5) -0.003(4) 0.020(4) -0.005(4) C55' 0.032(5) 0.015(4) 0.046(5) -0.005(4) 0.011(4) -0.004(4) C56' 0.021(4) 0.022(4) 0.027(4) 0.000(3) 0.003(3) -0.005(3) C61' 0.022(4) 0.023(4) 0.020(4) 0.002(3) 0.004(3) -0.008(3) C62' 0.043(6) 0.039(5) 0.023(4) -0.002(4) 0.008(4) -0.017(4) C63' 0.037(5) 0.053(6) 0.035(5) -0.013(4) 0.002(4) -0.026(5) C64' 0.053(7) 0.054(6) 0.032(5) -0.004(4) -0.010(5) -0.027(5) C65' 0.060(7) 0.067(7) 0.013(4) -0.003(4) 0.008(4) -0.031(6) C66' 0.033(5) 0.037(5) 0.026(4) -0.008(4) 0.012(4) -0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C5 1.956(8) . ? Mo1 C1 2.063(7) . ? Mo1 C4 2.175(7) . ? Mo1 C85 2.293(7) . ? Mo1 C84 2.324(8) . ? Mo1 C81 2.328(7) . ? Mo1 C82 2.366(7) . ? Mo1 C83 2.380(8) . ? Mo1 P1 2.403(2) . ? Mo1 Co1 2.6936(12) . ? Co1 C6 1.774(9) . ? Co1 C7 1.776(8) . ? Co1 C4 2.011(7) . ? Co1 C3 2.071(7) . ? Co1 C1 2.082(7) . ? Co1 C2 2.092(7) . ? P1 C1 1.719(7) . ? P1 C51 1.812(7) . ? P1 C61 1.827(8) . ? C5 O5 1.176(9) . ? O6 C6 1.138(9) . ? O7 C7 1.137(9) . ? O9 C8 1.356(10) . ? O9 C9 1.439(10) . ? O8 C8 1.215(9) . ? C8 C4 1.495(10) . ? C4 C3 1.443(10) . ? C3 C2 1.423(10) . ? C3 C10 1.503(10) . ? O10 C10 1.195(9) . ? C10 O11 1.352(9) . ? O11 C11 1.458(9) . ? C1 C2 1.444(10) . ? C2 C71 1.487(10) . ? C71 C76 1.374(10) . ? C71 C72 1.399(10) . ? C72 C73 1.385(11) . ? C73 C74 1.372(12) . ? C74 C75 1.373(13) . ? C75 C76 1.404(12) . ? C81 C82 1.411(12) . ? C81 C85 1.413(12) . ? C82 C83 1.393(11) . ? C83 C84 1.439(11) . ? C84 C85 1.401(11) . ? C51 C52 1.384(11) . ? C51 C56 1.403(11) . ? C52 C53 1.392(11) . ? C53 C54 1.371(12) . ? C54 C55 1.348(12) . ? C55 C56 1.376(11) . ? C61 C62 1.396(11) . ? C61 C66 1.400(10) . ? C62 C63 1.387(12) . ? C63 C64 1.392(13) . ? C64 C65 1.384(13) . ? C65 C66 1.402(12) . ? Mo1' C5' 1.966(8) . ? Mo1' C1' 2.067(7) . ? Mo1' C4' 2.186(7) . ? Mo1' C85' 2.308(8) . ? Mo1' C84' 2.333(8) . ? Mo1' C81' 2.341(8) . ? Mo1' C82' 2.362(9) . ? Mo1' P1' 2.400(2) . ? Mo1' C83' 2.406(8) . ? Mo1' Co1' 2.7100(13) . ? Co1' C7' 1.781(8) . ? Co1' C6' 1.785(8) . ? Co1' C4' 2.011(8) . ? Co1' C3' 2.081(7) . ? Co1' C1' 2.114(7) . ? Co1' C2' 2.118(7) . ? P1' C1' 1.716(8) . ? P1' C61' 1.819(7) . ? P1' C51' 1.823(7) . ? C5' O5' 1.160(9) . ? O6' C6' 1.143(9) . ? O7' C7' 1.127(9) . ? O9' C8' 1.352(9) . ? O9' C9' 1.445(9) . ? O8' C8' 1.207(9) . ? C8' C4' 1.482(10) . ? C4' C3' 1.442(10) . ? C3' C2' 1.432(10) . ? C3' C10' 1.488(10) . ? O10' C10' 1.199(9) . ? C10' O11' 1.344(9) . ? O11' C11' 1.466(8) . ? C1' C2' 1.428(10) . ? C2' C71' 1.501(10) . ? C71' C76' 1.361(11) . ? C71' C72' 1.391(11) . ? C72' C73' 1.383(12) . ? C73' C74' 1.397(14) . ? C74' C75' 1.395(13) . ? C75' C76' 1.368(11) . ? C81' C82' 1.417(12) . ? C81' C85' 1.423(12) . ? C82' C83' 1.392(11) . ? C83' C84' 1.408(11) . ? C84' C85' 1.415(11) . ? C51' C56' 1.381(10) . ? C51' C52' 1.398(10) . ? C52' C53' 1.380(10) . ? C53' C54' 1.402(11) . ? C54' C55' 1.384(11) . ? C55' C56' 1.390(10) . ? C61' C62' 1.354(11) . ? C61' C66' 1.411(10) . ? C62' C63' 1.389(11) . ? C63' C64' 1.384(12) . ? C64' C65' 1.388(13) . ? C65' C66' 1.374(11) . ? 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 C5 Mo1 C1 105.6(3) . . ? C5 Mo1 C4 90.5(3) . . ? C1 Mo1 C4 70.4(3) . . ? C5 Mo1 C85 128.3(3) . . ? C1 Mo1 C85 122.0(3) . . ? C4 Mo1 C85 87.7(3) . . ? C5 Mo1 C84 93.3(3) . . ? C1 Mo1 C84 154.2(3) . . ? C4 Mo1 C84 92.5(3) . . ? C85 Mo1 C84 35.3(3) . . ? C5 Mo1 C81 139.7(3) . . ? C1 Mo1 C81 111.0(3) . . ? C4 Mo1 C81 116.9(3) . . ? C85 Mo1 C81 35.6(3) . . ? C84 Mo1 C81 58.9(3) . . ? C5 Mo1 C82 106.9(3) . . ? C1 Mo1 C82 128.9(3) . . ? C4 Mo1 C82 145.9(3) . . ? C85 Mo1 C82 58.5(3) . . ? C84 Mo1 C82 58.3(3) . . ? C81 Mo1 C82 35.0(3) . . ? C5 Mo1 C83 82.2(3) . . ? C1 Mo1 C83 162.3(3) . . ? C4 Mo1 C83 126.1(3) . . ? C85 Mo1 C83 58.6(3) . . ? C84 Mo1 C83 35.6(3) . . ? C81 Mo1 C83 58.0(3) . . ? C82 Mo1 C83 34.1(3) . . ? C5 Mo1 P1 98.0(2) . . ? C1 Mo1 P1 44.5(2) . . ? C4 Mo1 P1 114.2(2) . . ? C85 Mo1 P1 129.4(2) . . ? C84 Mo1 P1 150.7(2) . . ? C81 Mo1 P1 96.6(2) . . ? C82 Mo1 P1 92.5(2) . . ? C83 Mo1 P1 119.6(2) . . ? C5 Mo1 Co1 64.4(2) . . ? C1 Mo1 Co1 49.8(2) . . ? C4 Mo1 Co1 47.3(2) . . ? C85 Mo1 Co1 135.0(2) . . ? C84 Mo1 Co1 130.1(2) . . ? C81 Mo1 Co1 155.6(2) . . ? C82 Mo1 Co1 166.4(2) . . ? C83 Mo1 Co1 144.5(2) . . ? P1 Mo1 Co1 78.94(5) . . ? C6 Co1 C7 93.5(4) . . ? C6 Co1 C4 168.5(3) . . ? C7 Co1 C4 96.3(3) . . ? C6 Co1 C3 129.3(3) . . ? C7 Co1 C3 106.8(3) . . ? C4 Co1 C3 41.4(3) . . ? C6 Co1 C1 97.2(3) . . ? C7 Co1 C1 169.1(3) . . ? C4 Co1 C1 73.3(3) . . ? C3 Co1 C1 67.6(3) . . ? C6 Co1 C2 96.9(3) . . ? C7 Co1 C2 139.9(3) . . ? C4 Co1 C2 71.6(3) . . ? C3 Co1 C2 40.0(3) . . ? C1 Co1 C2 40.5(3) . . ? C6 Co1 Mo1 125.7(3) . . ? C7 Co1 Mo1 121.9(3) . . ? C4 Co1 Mo1 52.7(2) . . ? C3 Co1 Mo1 81.5(2) . . ? C1 Co1 Mo1 49.2(2) . . ? C2 Co1 Mo1 81.6(2) . . ? C1 P1 C51 112.5(3) . . ? C1 P1 C61 116.5(3) . . ? C51 P1 C61 106.0(3) . . ? C1 P1 Mo1 57.2(2) . . ? C51 P1 Mo1 122.2(2) . . ? C61 P1 Mo1 130.2(3) . . ? O5 C5 Mo1 167.2(7) . . ? O6 C6 Co1 175.8(8) . . ? O7 C7 Co1 175.8(7) . . ? C8 O9 C9 114.0(6) . . ? O8 C8 O9 123.4(7) . . ? O8 C8 C4 126.1(8) . . ? O9 C8 C4 110.5(7) . . ? C3 C4 C8 118.0(6) . . ? C3 C4 Co1 71.5(4) . . ? C8 C4 Co1 124.4(5) . . ? C3 C4 Mo1 119.5(5) . . ? C8 C4 Mo1 122.2(5) . . ? Co1 C4 Mo1 80.0(3) . . ? C2 C3 C4 113.9(6) . . ? C2 C3 C10 124.7(6) . . ? C4 C3 C10 121.3(6) . . ? C2 C3 Co1 70.8(4) . . ? C4 C3 Co1 67.1(4) . . ? C10 C3 Co1 126.8(5) . . ? O10 C10 O11 124.2(7) . . ? O10 C10 C3 126.7(7) . . ? O11 C10 C3 109.1(6) . . ? C10 O11 C11 114.4(6) . . ? C2 C1 P1 153.7(6) . . ? C2 C1 Mo1 127.8(5) . . ? P1 C1 Mo1 78.3(3) . . ? C2 C1 Co1 70.1(4) . . ? P1 C1 Co1 117.1(3) . . ? Mo1 C1 Co1 81.0(2) . . ? C3 C2 C1 107.4(6) . . ? C3 C2 C71 125.5(6) . . ? C1 C2 C71 127.1(6) . . ? C3 C2 Co1 69.2(4) . . ? C1 C2 Co1 69.4(4) . . ? C71 C2 Co1 124.8(5) . . ? C76 C71 C72 118.0(7) . . ? C76 C71 C2 121.0(7) . . ? C72 C71 C2 121.0(6) . . ? C73 C72 C71 121.0(7) . . ? C74 C73 C72 120.2(8) . . ? C73 C74 C75 119.7(8) . . ? C74 C75 C76 120.1(8) . . ? C71 C76 C75 120.8(8) . . ? C82 C81 C85 107.4(7) . . ? C82 C81 Mo1 74.0(4) . . ? C85 C81 Mo1 70.9(4) . . ? C83 C82 C81 109.0(7) . . ? C83 C82 Mo1 73.5(4) . . ? C81 C82 Mo1 71.0(4) . . ? C82 C83 C84 107.5(7) . . ? C82 C83 Mo1 72.4(4) . . ? C84 C83 Mo1 70.1(4) . . ? C85 C84 C83 107.4(7) . . ? C85 C84 Mo1 71.1(4) . . ? C83 C84 Mo1 74.3(5) . . ? C84 C85 C81 108.7(8) . . ? C84 C85 Mo1 73.5(4) . . ? C81 C85 Mo1 73.5(5) . . ? C52 C51 C56 118.3(7) . . ? C52 C51 P1 120.3(6) . . ? C56 C51 P1 121.4(6) . . ? C51 C52 C53 120.0(8) . . ? C54 C53 C52 119.9(8) . . ? C55 C54 C53 121.1(8) . . ? C54 C55 C56 120.0(8) . . ? C55 C56 C51 120.7(8) . . ? C62 C61 C66 121.0(8) . . ? C62 C61 P1 121.0(6) . . ? C66 C61 P1 117.8(6) . . ? C63 C62 C61 119.2(8) . . ? C62 C63 C64 121.0(9) . . ? C65 C64 C63 119.1(8) . . ? C64 C65 C66 121.6(8) . . ? C61 C66 C65 118.0(8) . . ? C5' Mo1' C1' 104.2(3) . . ? C5' Mo1' C4' 92.7(3) . . ? C1' Mo1' C4' 69.6(3) . . ? C5' Mo1' C85' 129.8(3) . . ? C1' Mo1' C85' 122.8(3) . . ? C4' Mo1' C85' 88.3(3) . . ? C5' Mo1' C84' 94.5(3) . . ? C1' Mo1' C84' 155.4(3) . . ? C4' Mo1' C84' 94.0(3) . . ? C85' Mo1' C84' 35.5(3) . . ? C5' Mo1' C81' 139.3(3) . . ? C1' Mo1' C81' 111.6(3) . . ? C4' Mo1' C81' 117.2(3) . . ? C85' Mo1' C81' 35.6(3) . . ? C84' Mo1' C81' 58.7(3) . . ? C5' Mo1' C82' 105.7(3) . . ? C1' Mo1' C82' 129.2(3) . . ? C4' Mo1' C82' 146.6(3) . . ? C85' Mo1' C82' 58.5(3) . . ? C84' Mo1' C82' 57.7(3) . . ? C81' Mo1' C82' 35.1(3) . . ? C5' Mo1' P1' 95.7(2) . . ? C1' Mo1' P1' 44.4(2) . . ? C4' Mo1' P1' 113.5(2) . . ? C85' Mo1' P1' 129.4(2) . . ? C84' Mo1' P1' 150.0(2) . . ? C81' Mo1' P1' 96.4(2) . . ? C82' Mo1' P1' 92.4(2) . . ? C5' Mo1' C83' 82.7(3) . . ? C1' Mo1' C83' 162.6(3) . . ? C4' Mo1' C83' 126.7(3) . . ? C85' Mo1' C83' 58.0(3) . . ? C84' Mo1' C83' 34.5(3) . . ? C81' Mo1' C83' 57.6(3) . . ? C82' Mo1' C83' 33.9(3) . . ? P1' Mo1' C83' 119.7(2) . . ? C5' Mo1' Co1' 64.0(2) . . ? C1' Mo1' Co1' 50.4(2) . . ? C4' Mo1' Co1' 47.0(2) . . ? C85' Mo1' Co1' 135.3(2) . . ? C84' Mo1' Co1' 129.9(2) . . ? C81' Mo1' Co1' 156.7(2) . . ? C82' Mo1' Co1' 165.9(2) . . ? P1' Mo1' Co1' 79.64(6) . . ? C83' Mo1' Co1' 143.7(2) . . ? C7' Co1' C6' 91.4(4) . . ? C7' Co1' C4' 95.4(3) . . ? C6' Co1' C4' 172.7(3) . . ? C7' Co1' C3' 108.7(3) . . ? C6' Co1' C3' 133.4(3) . . ? C4' Co1' C3' 41.2(3) . . ? C7' Co1' C1' 165.3(3) . . ? C6' Co1' C1' 101.5(3) . . ? C4' Co1' C1' 72.1(3) . . ? C3' Co1' C1' 67.2(3) . . ? C7' Co1' C2' 144.2(3) . . ? C6' Co1' C2' 102.3(3) . . ? C4' Co1' C2' 70.5(3) . . ? C3' Co1' C2' 39.9(3) . . ? C1' Co1' C2' 39.5(3) . . ? C7' Co1' Mo1' 117.5(3) . . ? C6' Co1' Mo1' 126.0(3) . . ? C4' Co1' Mo1' 52.7(2) . . ? C3' Co1' Mo1' 81.9(2) . . ? C1' Co1' Mo1' 48.9(2) . . ? C2' Co1' Mo1' 80.7(2) . . ? C1' P1' C61' 114.2(3) . . ? C1' P1' C51' 114.2(3) . . ? C61' P1' C51' 105.8(3) . . ? C1' P1' Mo1' 57.5(2) . . ? C61' P1' Mo1' 130.6(2) . . ? C51' P1' Mo1' 122.3(2) . . ? O5' C5' Mo1' 168.5(7) . . ? O6' C6' Co1' 174.9(7) . . ? O7' C7' Co1' 174.0(8) . . ? C8' O9' C9' 115.8(6) . . ? O8' C8' O9' 122.5(7) . . ? O8' C8' C4' 127.2(7) . . ? O9' C8' C4' 110.2(6) . . ? C3' C4' C8' 119.7(7) . . ? C3' C4' Co1' 72.0(4) . . ? C8' C4' Co1' 125.6(5) . . ? C3' C4' Mo1' 120.8(5) . . ? C8' C4' Mo1' 119.1(5) . . ? Co1' C4' Mo1' 80.3(3) . . ? C2' C3' C4' 112.1(6) . . ? C2' C3' C10' 126.5(7) . . ? C4' C3' C10' 121.2(7) . . ? C2' C3' Co1' 71.5(4) . . ? C4' C3' Co1' 66.8(4) . . ? C10' C3' Co1' 125.1(5) . . ? O10' C10' O11' 123.2(7) . . ? O10' C10' C3' 125.2(7) . . ? O11' C10' C3' 111.5(7) . . ? C10' O11' C11' 115.9(6) . . ? C2' C1' P1' 153.4(6) . . ? C2' C1' Mo1' 128.3(5) . . ? P1' C1' Mo1' 78.1(3) . . ? C2' C1' Co1' 70.4(4) . . ? P1' C1' Co1' 117.5(4) . . ? Mo1' C1' Co1' 80.8(3) . . ? C1' C2' C3' 108.5(6) . . ? C1' C2' C71' 120.9(6) . . ? C3' C2' C71' 130.6(6) . . ? C1' C2' Co1' 70.1(4) . . ? C3' C2' Co1' 68.6(4) . . ? C71' C2' Co1' 128.5(5) . . ? C76' C71' C72' 117.9(8) . . ? C76' C71' C2' 119.9(7) . . ? C72' C71' C2' 122.2(7) . . ? C73' C72' C71' 120.7(9) . . ? C72' C73' C74' 119.5(9) . . ? C75' C74' C73' 120.2(9) . . ? C76' C75' C74' 117.7(9) . . ? C71' C76' C75' 124.1(9) . . ? C82' C81' C85' 106.9(7) . . ? C82' C81' Mo1' 73.3(5) . . ? C85' C81' Mo1' 70.9(4) . . ? C83' C82' C81' 109.1(8) . . ? C83' C82' Mo1' 74.8(5) . . ? C81' C82' Mo1' 71.7(5) . . ? C82' C83' C84' 107.9(7) . . ? C82' C83' Mo1' 71.3(5) . . ? C84' C83' Mo1' 69.9(4) . . ? C83' C84' C85' 108.3(7) . . ? C83' C84' Mo1' 75.6(5) . . ? C85' C84' Mo1' 71.3(4) . . ? C84' C85' C81' 107.6(8) . . ? C84' C85' Mo1' 73.2(4) . . ? C81' C85' Mo1' 73.4(5) . . ? C56' C51' C52' 119.3(7) . . ? C56' C51' P1' 119.5(5) . . ? C52' C51' P1' 121.0(6) . . ? C53' C52' C51' 119.9(7) . . ? C52' C53' C54' 120.6(8) . . ? C55' C54' C53' 119.1(7) . . ? C54' C55' C56' 120.1(8) . . ? C51' C56' C55' 120.9(7) . . ? C62' C61' C66' 120.1(7) . . ? C62' C61' P1' 120.2(6) . . ? C66' C61' P1' 119.7(6) . . ? C61' C62' C63' 120.9(8) . . ? C64' C63' C62' 119.6(9) . . ? C63' C64' C65' 119.6(9) . . ? C66' C65' C64' 120.8(8) . . ? C65' C66' C61' 119.0(8) . . ? _refine_diff_density_max 0.588 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.140 data_mm9810 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H30 Co Mo O3 P' _chemical_formula_weight 672.42 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.771(19) _cell_length_b 28.163(12) _cell_length_c 11.014(12) _cell_angle_alpha 90.00 _cell_angle_beta 119.27(5) _cell_angle_gamma 90.00 _cell_volume 2914.5(62) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method ? _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.000 _exptl_absorpt_correction_T_max 0.950 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method 'omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.4 _diffrn_reflns_number 7863 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0855 _diffrn_reflns_limit_h_min -999 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -999 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5102 _reflns_number_observed 3512 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1022P)^2^+6.9089P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5095 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_obs 0.0701 _refine_ls_wR_factor_all 0.2035 _refine_ls_wR_factor_obs 0.1743 _refine_ls_goodness_of_fit_all 1.063 _refine_ls_goodness_of_fit_obs 1.107 _refine_ls_restrained_S_all 1.062 _refine_ls_restrained_S_obs 1.107 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 1.77233(7) 0.09612(2) 0.27485(7) 0.0306(2) Uani 1 d . . Co1 Co 1.88608(11) 0.15502(4) 0.15873(12) 0.0347(3) Uani 1 d . . P1 P 1.5982(2) 0.09267(7) 0.0304(2) 0.0312(5) Uani 1 d . . O5 O 2.0342(6) 0.0408(2) 0.2971(7) 0.050(2) Uani 1 d . . C5 C 1.9381(8) 0.0640(3) 0.2832(9) 0.039(2) Uani 1 d . . O6 O 2.1840(7) 0.1353(3) 0.2620(8) 0.073(2) Uani 1 d . . C6 C 2.0685(9) 0.1438(3) 0.2285(10) 0.047(2) Uani 1 d . . O7 O 1.8469(7) 0.1643(3) -0.1188(7) 0.060(2) Uani 1 d . . C7 C 1.8608(9) 0.1589(3) -0.0094(10) 0.043(2) Uani 1 d . . C81 C 1.6238(10) 0.0415(3) 0.3072(9) 0.042(2) Uani 1 d . . H81 H 1.5580(10) 0.0217(3) 0.2343(9) 0.050 Uiso 1 calc R . C82 C 1.7644(10) 0.0292(3) 0.4018(10) 0.049(2) Uani 1 d . . H82 H 1.8103(10) 0.0001(3) 0.4039(10) 0.059 Uiso 1 calc R . C83 C 1.8261(9) 0.0682(4) 0.4943(9) 0.049(2) Uani 1 d . . H83 H 1.9206(9) 0.0702(4) 0.5697(9) 0.058 Uiso 1 calc R . C84 C 1.7198(10) 0.1033(3) 0.4525(10) 0.049(2) Uani 1 d . . H84 H 1.7311(10) 0.1333(3) 0.4965(10) 0.058 Uiso 1 calc R . C85 C 1.5938(9) 0.0873(3) 0.3353(9) 0.043(2) Uani 1 d . . H85 H 1.5067(9) 0.1041(3) 0.2857(9) 0.051 Uiso 1 calc R . C71 C 1.6175(8) 0.2292(3) 0.0164(9) 0.033(2) Uani 1 d . . C72 C 1.5957(9) 0.2742(3) 0.0536(10) 0.042(2) Uani 1 d . . H72 H 1.6444(9) 0.2835(3) 0.1487(10) 0.050 Uiso 1 calc R . C73 C 1.5032(10) 0.3059(3) -0.0471(11) 0.049(2) Uani 1 d . . H73 H 1.4844(10) 0.3358(3) -0.0200(11) 0.058 Uiso 1 calc R . C74 C 1.4386(9) 0.2938(3) -0.1861(10) 0.048(2) Uani 1 d . . H74 H 1.3771(9) 0.3156(3) -0.2553(10) 0.057 Uiso 1 calc R . C75 C 1.4646(8) 0.2500(3) -0.2228(9) 0.044(2) Uani 1 d . . H75 H 1.4220(8) 0.2420(3) -0.3187(9) 0.053 Uiso 1 calc R . C76 C 1.5503(8) 0.2172(3) -0.1252(9) 0.039(2) Uani 1 d . . H76 H 1.5639(8) 0.1867(3) -0.1534(9) 0.046 Uiso 1 calc R . C51 C 1.4074(8) 0.0951(3) -0.0275(8) 0.033(2) Uani 1 d . . C52 C 1.3231(8) 0.0556(3) -0.0818(9) 0.040(2) Uani 1 d . . H52 H 1.3640(8) 0.0268(3) -0.0909(9) 0.048 Uiso 1 calc R . C53 C 1.1789(9) 0.0572(3) -0.1236(10) 0.049(2) Uani 1 d . . H53 H 1.1214(9) 0.0298(3) -0.1621(10) 0.059 Uiso 1 calc R . C54 C 1.1190(9) 0.0988(3) -0.1089(10) 0.045(2) Uani 1 d . . H54 H 1.0204(9) 0.0999(3) -0.1370(10) 0.054 Uiso 1 calc R . C55 C 1.2022(9) 0.1387(3) -0.0537(10) 0.047(2) Uani 1 d . . H55 H 1.1615(9) 0.1672(3) -0.0433(10) 0.056 Uiso 1 calc R . C56 C 1.3472(8) 0.1367(3) -0.0132(8) 0.038(2) Uani 1 d . . H56 H 1.4048(8) 0.1642(3) 0.0245(8) 0.045 Uiso 1 calc R . C61 C 1.6092(8) 0.0725(3) -0.1201(8) 0.032(2) Uani 1 d . . C62 C 1.7257(9) 0.0460(3) -0.0988(10) 0.042(2) Uani 1 d . . H62 H 1.7997(9) 0.0399(3) -0.0068(10) 0.051 Uiso 1 calc R . C63 C 1.7352(11) 0.0282(3) -0.2121(11) 0.051(2) Uani 1 d . . H63 H 1.8149(11) 0.0096(3) -0.1973(11) 0.062 Uiso 1 calc R . C64 C 1.6289(11) 0.0376(3) -0.3452(11) 0.052(2) Uani 1 d . . H64 H 1.6353(11) 0.0254(3) -0.4224(11) 0.063 Uiso 1 calc R . C65 C 1.5143(11) 0.0644(3) -0.3669(9) 0.048(2) Uani 1 d . . H65 H 1.4415(11) 0.0710(3) -0.4592(9) 0.058 Uiso 1 calc R . C66 C 1.5033(9) 0.0821(3) -0.2550(9) 0.043(2) Uani 1 d . . H66 H 1.4233(9) 0.1007(3) -0.2707(9) 0.051 Uiso 1 calc R . C1 C 1.6819(8) 0.1436(3) 0.1144(9) 0.035(2) Uani 1 d . . C2 C 1.7052(8) 0.1943(3) 0.1245(8) 0.031(2) Uani 1 d . . C3 C 1.8194(8) 0.2045(3) 0.2583(9) 0.039(2) Uani 1 d . . H3 H 1.8483(8) 0.2363(3) 0.2877(9) 0.047 Uiso 1 calc R . C4 C 1.8889(8) 0.1656(3) 0.3466(9) 0.038(2) Uani 1 d . . C8 C 2.0206(9) 0.1791(3) 0.4870(10) 0.048(2) Uani 1 d . . C9 C 2.1021(11) 0.2223(4) 0.4758(11) 0.065(3) Uani 1 d . . H9A H 2.1345(60) 0.2155(9) 0.4085(51) 0.078 Uiso 1 calc R . H9B H 2.1846(41) 0.2289(15) 0.5671(18) 0.078 Uiso 1 calc R . H9C H 2.0391(23) 0.2501(6) 0.4447(66) 0.078 Uiso 1 calc R . C10 C 1.9672(11) 0.1928(4) 0.5899(10) 0.066(3) Uani 1 d . . H10A H 2.0471(17) 0.2048(22) 0.6764(28) 0.079 Uiso 1 calc R . H10B H 1.9265(62) 0.1648(7) 0.6101(52) 0.079 Uiso 1 calc R . H10C H 1.8942(50) 0.2176(17) 0.5482(29) 0.079 Uiso 1 calc R . C11 C 2.1285(9) 0.1386(3) 0.5528(9) 0.051(2) Uani 1 d . . H11A H 2.1729(45) 0.1320(14) 0.4953(33) 0.061 Uiso 1 calc R . H11B H 2.0796(14) 0.1101(7) 0.5586(56) 0.061 Uiso 1 calc R . H11C H 2.2019(35) 0.1479(9) 0.6464(25) 0.061 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0261(4) 0.0295(4) 0.0331(4) 0.0024(3) 0.0121(3) 0.0016(3) Co1 0.0258(6) 0.0340(6) 0.0418(7) 0.0025(5) 0.0144(5) 0.0000(4) P1 0.0259(10) 0.0294(10) 0.0362(11) -0.0011(9) 0.0136(9) 0.0005(8) O5 0.042(3) 0.043(3) 0.067(4) 0.002(3) 0.027(3) 0.009(3) C5 0.026(4) 0.028(4) 0.047(5) 0.010(4) 0.006(4) 0.002(3) O6 0.035(4) 0.094(6) 0.087(6) 0.009(5) 0.028(4) 0.001(4) C6 0.036(5) 0.056(6) 0.046(5) 0.017(4) 0.016(4) 0.004(4) O7 0.053(4) 0.080(5) 0.055(4) 0.018(4) 0.032(4) 0.015(4) C7 0.035(5) 0.046(5) 0.052(6) 0.013(4) 0.024(4) 0.009(4) C81 0.053(5) 0.044(5) 0.039(5) 0.004(4) 0.031(4) -0.002(4) C82 0.061(6) 0.039(5) 0.060(6) 0.032(4) 0.040(5) 0.013(4) C83 0.040(5) 0.071(6) 0.022(4) 0.010(4) 0.006(4) 0.001(5) C84 0.058(6) 0.048(5) 0.055(6) 0.006(4) 0.040(5) 0.001(4) C85 0.038(5) 0.044(5) 0.050(5) -0.006(4) 0.024(4) -0.005(4) C71 0.023(4) 0.032(4) 0.041(5) 0.002(3) 0.014(4) 0.000(3) C72 0.036(4) 0.035(4) 0.050(5) 0.002(4) 0.018(4) 0.004(4) C73 0.048(5) 0.033(4) 0.067(7) 0.006(4) 0.029(5) 0.008(4) C74 0.044(5) 0.047(5) 0.053(6) 0.020(4) 0.025(5) 0.020(4) C75 0.031(4) 0.054(5) 0.031(5) 0.005(4) 0.002(4) 0.004(4) C76 0.034(4) 0.038(4) 0.042(5) -0.002(4) 0.017(4) 0.000(4) C51 0.024(4) 0.037(4) 0.032(4) 0.007(4) 0.010(3) 0.000(3) C52 0.028(4) 0.040(5) 0.051(5) 0.001(4) 0.018(4) 0.001(4) C53 0.037(5) 0.045(5) 0.052(6) -0.004(4) 0.012(4) -0.013(4) C54 0.027(4) 0.055(6) 0.048(5) 0.004(4) 0.014(4) 0.002(4) C55 0.034(4) 0.045(5) 0.059(6) -0.005(4) 0.022(4) 0.005(4) C56 0.028(4) 0.039(4) 0.038(5) -0.004(4) 0.010(4) -0.002(4) C61 0.031(4) 0.031(4) 0.035(4) -0.003(3) 0.016(4) -0.007(3) C62 0.039(5) 0.039(5) 0.052(5) -0.003(4) 0.024(4) 0.002(4) C63 0.056(6) 0.043(5) 0.071(7) -0.003(5) 0.043(6) 0.005(4) C64 0.070(7) 0.044(5) 0.061(6) -0.012(5) 0.046(6) -0.021(5) C65 0.064(6) 0.050(5) 0.032(5) -0.004(4) 0.025(5) -0.021(5) C66 0.043(5) 0.038(5) 0.047(5) 0.000(4) 0.022(4) -0.007(4) C1 0.027(4) 0.029(4) 0.049(5) -0.007(4) 0.018(4) -0.002(3) C2 0.030(4) 0.028(4) 0.038(4) 0.003(3) 0.018(4) 0.004(3) C3 0.029(4) 0.035(4) 0.046(5) 0.000(4) 0.012(4) -0.005(3) C4 0.024(4) 0.041(5) 0.044(5) 0.004(4) 0.013(4) 0.000(3) C8 0.032(5) 0.048(5) 0.045(5) -0.005(4) 0.003(4) -0.002(4) C9 0.049(6) 0.057(6) 0.058(6) -0.011(5) 0.002(5) -0.023(5) C10 0.047(6) 0.079(8) 0.048(6) -0.010(5) 0.006(5) 0.006(5) C11 0.038(5) 0.061(6) 0.036(5) 0.002(4) 0.003(4) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C5 1.963(9) . ? Mo1 C1 2.043(9) . ? Mo1 C4 2.250(8) . ? Mo1 C84 2.296(9) . ? Mo1 C83 2.330(9) . ? Mo1 C85 2.335(9) . ? Mo1 C81 2.368(9) . ? Mo1 C82 2.373(8) . ? Mo1 P1 2.416(4) . ? Mo1 Co1 2.724(2) . ? Co1 C7 1.739(10) . ? Co1 C6 1.753(9) . ? Co1 C1 2.032(8) . ? Co1 C4 2.076(9) . ? Co1 C3 2.106(9) . ? Co1 C2 2.109(8) . ? P1 C1 1.705(8) . ? P1 C61 1.810(8) . ? P1 C51 1.832(8) . ? O5 C5 1.169(10) . ? O6 C6 1.138(10) . ? O7 C7 1.149(11) . ? C81 C82 1.399(13) . ? C81 C85 1.400(12) . ? C81 H81 0.95 . ? C82 C83 1.424(13) . ? C82 H82 0.95 . ? C83 C84 1.408(13) . ? C83 H83 0.95 . ? C84 C85 1.414(13) . ? C84 H84 0.95 . ? C85 H85 0.95 . ? C71 C72 1.386(11) . ? C71 C76 1.403(12) . ? C71 C2 1.474(10) . ? C72 C73 1.393(12) . ? C72 H72 0.95 . ? C73 C74 1.378(14) . ? C73 H73 0.95 . ? C74 C75 1.369(13) . ? C74 H74 0.95 . ? C75 C76 1.375(12) . ? C75 H75 0.95 . ? C76 H76 0.95 . ? C51 C52 1.376(11) . ? C51 C56 1.385(11) . ? C52 C53 1.388(12) . ? C52 H52 0.95 . ? C53 C54 1.386(13) . ? C53 H53 0.95 . ? C54 C55 1.378(12) . ? C54 H54 0.95 . ? C55 C56 1.399(11) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C61 C62 1.379(11) . ? C61 C66 1.387(12) . ? C62 C63 1.394(13) . ? C62 H62 0.95 . ? C63 C64 1.375(14) . ? C63 H63 0.95 . ? C64 C65 1.365(14) . ? C64 H64 0.95 . ? C65 C66 1.387(12) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? C1 C2 1.446(10) . ? C2 C3 1.412(11) . ? C3 C4 1.413(11) . ? C3 H3 0.95 . ? C4 C8 1.550(12) . ? C8 C11 1.535(12) . ? C8 C9 1.540(13) . ? C8 C10 1.549(14) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? 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 C5 Mo1 C1 112.4(3) . . ? C5 Mo1 C4 92.6(3) . . ? C1 Mo1 C4 71.5(3) . . ? C5 Mo1 C84 126.7(4) . . ? C1 Mo1 C84 117.8(3) . . ? C4 Mo1 C84 87.2(3) . . ? C5 Mo1 C83 92.1(3) . . ? C1 Mo1 C83 152.8(3) . . ? C4 Mo1 C83 96.7(3) . . ? C84 Mo1 C83 35.4(3) . . ? C5 Mo1 C85 142.6(3) . . ? C1 Mo1 C85 101.8(3) . . ? C4 Mo1 C85 112.9(3) . . ? C84 Mo1 C85 35.5(3) . . ? C83 Mo1 C85 59.3(3) . . ? C5 Mo1 C81 111.0(3) . . ? C1 Mo1 C81 118.9(3) . . ? C4 Mo1 C81 144.5(3) . . ? C84 Mo1 C81 57.5(3) . . ? C83 Mo1 C81 57.9(3) . . ? C85 Mo1 C81 34.6(3) . . ? C5 Mo1 C82 84.2(3) . . ? C1 Mo1 C82 152.9(3) . . ? C4 Mo1 C82 131.2(3) . . ? C84 Mo1 C82 58.2(3) . . ? C83 Mo1 C82 35.2(3) . . ? C85 Mo1 C82 58.4(3) . . ? C81 Mo1 C82 34.3(3) . . ? C5 Mo1 P1 103.1(3) . . ? C1 Mo1 P1 44.0(2) . . ? C4 Mo1 P1 115.0(2) . . ? C84 Mo1 P1 124.9(3) . . ? C83 Mo1 P1 143.7(2) . . ? C85 Mo1 P1 90.8(3) . . ? C81 Mo1 P1 85.9(2) . . ? C82 Mo1 P1 113.1(3) . . ? C5 Mo1 Co1 72.3(2) . . ? C1 Mo1 Co1 47.9(2) . . ? C4 Mo1 Co1 48.2(2) . . ? C84 Mo1 Co1 134.5(2) . . ? C83 Mo1 Co1 138.8(2) . . ? C85 Mo1 Co1 145.2(2) . . ? C81 Mo1 Co1 163.3(2) . . ? C82 Mo1 Co1 156.1(2) . . ? P1 Mo1 Co1 77.50(11) . . ? C7 Co1 C6 92.1(4) . . ? C7 Co1 C1 99.6(4) . . ? C6 Co1 C1 157.8(4) . . ? C7 Co1 C4 166.2(4) . . ? C6 Co1 C4 97.0(4) . . ? C1 Co1 C4 75.5(3) . . ? C7 Co1 C3 126.7(4) . . ? C6 Co1 C3 119.0(4) . . ? C1 Co1 C3 68.0(3) . . ? C4 Co1 C3 39.5(3) . . ? C7 Co1 C2 97.3(3) . . ? C6 Co1 C2 155.8(4) . . ? C1 Co1 C2 40.8(3) . . ? C4 Co1 C2 70.4(3) . . ? C3 Co1 C2 39.2(3) . . ? C7 Co1 Mo1 131.8(3) . . ? C6 Co1 Mo1 110.5(3) . . ? C1 Co1 Mo1 48.2(2) . . ? C4 Co1 Mo1 53.9(2) . . ? C3 Co1 Mo1 79.2(2) . . ? C2 Co1 Mo1 79.4(2) . . ? C1 P1 C61 120.4(4) . . ? C1 P1 C51 111.3(4) . . ? C61 P1 C51 104.9(4) . . ? C1 P1 Mo1 56.3(3) . . ? C61 P1 Mo1 132.1(3) . . ? C51 P1 Mo1 120.9(3) . . ? O5 C5 Mo1 172.1(7) . . ? O6 C6 Co1 173.7(9) . . ? O7 C7 Co1 175.8(9) . . ? C82 C81 C85 110.3(8) . . ? C82 C81 Mo1 73.0(5) . . ? C85 C81 Mo1 71.4(5) . . ? C82 C81 H81 124.8(6) . . ? C85 C81 H81 124.8(5) . . ? Mo1 C81 H81 122.3(2) . . ? C81 C82 C83 107.3(8) . . ? C81 C82 Mo1 72.6(5) . . ? C83 C82 Mo1 70.7(5) . . ? C81 C82 H82 126.4(6) . . ? C83 C82 H82 126.4(5) . . ? Mo1 C82 H82 122.0(2) . . ? C84 C83 C82 106.8(8) . . ? C84 C83 Mo1 71.0(5) . . ? C82 C83 Mo1 74.1(5) . . ? C84 C83 H83 126.6(6) . . ? C82 C83 H83 126.6(5) . . ? Mo1 C83 H83 120.2(2) . . ? C83 C84 C85 109.8(9) . . ? C83 C84 Mo1 73.6(5) . . ? C85 C84 Mo1 73.7(5) . . ? C83 C84 H84 125.1(6) . . ? C85 C84 H84 125.1(5) . . ? Mo1 C84 H84 119.3(2) . . ? C81 C85 C84 105.9(8) . . ? C81 C85 Mo1 74.0(5) . . ? C84 C85 Mo1 70.7(5) . . ? C81 C85 H85 127.0(5) . . ? C84 C85 H85 127.0(5) . . ? Mo1 C85 H85 120.2(2) . . ? C72 C71 C76 118.6(7) . . ? C72 C71 C2 120.3(8) . . ? C76 C71 C2 121.1(7) . . ? C71 C72 C73 120.6(9) . . ? C71 C72 H72 119.7(5) . . ? C73 C72 H72 119.7(6) . . ? C74 C73 C72 120.2(9) . . ? C74 C73 H73 119.9(5) . . ? C72 C73 H73 119.9(6) . . ? C75 C74 C73 119.0(8) . . ? C75 C74 H74 120.5(5) . . ? C73 C74 H74 120.5(5) . . ? C74 C75 C76 122.0(8) . . ? C74 C75 H75 119.0(5) . . ? C76 C75 H75 119.0(5) . . ? C75 C76 C71 119.4(8) . . ? C75 C76 H76 120.3(5) . . ? C71 C76 H76 120.3(5) . . ? C52 C51 C56 119.3(7) . . ? C52 C51 P1 120.7(6) . . ? C56 C51 P1 120.0(6) . . ? C51 C52 C53 120.7(8) . . ? C51 C52 H52 119.6(5) . . ? C53 C52 H52 119.6(5) . . ? C54 C53 C52 119.9(8) . . ? C54 C53 H53 120.1(5) . . ? C52 C53 H53 120.1(5) . . ? C55 C54 C53 120.0(8) . . ? C55 C54 H54 120.0(5) . . ? C53 C54 H54 120.0(5) . . ? C54 C55 C56 119.5(8) . . ? C54 C55 H55 120.2(5) . . ? C56 C55 H55 120.2(5) . . ? C51 C56 C55 120.5(8) . . ? C51 C56 H56 119.7(5) . . ? C55 C56 H56 119.7(5) . . ? C62 C61 C66 119.4(8) . . ? C62 C61 P1 118.4(6) . . ? C66 C61 P1 122.2(6) . . ? C61 C62 C63 120.1(9) . . ? C61 C62 H62 119.9(5) . . ? C63 C62 H62 119.9(6) . . ? C64 C63 C62 119.9(9) . . ? C64 C63 H63 120.1(6) . . ? C62 C63 H63 120.1(6) . . ? C65 C64 C63 120.2(9) . . ? C65 C64 H64 119.9(6) . . ? C63 C64 H64 119.9(6) . . ? C64 C65 C66 120.4(9) . . ? C64 C65 H65 119.8(6) . . ? C66 C65 H65 119.8(6) . . ? C61 C66 C65 120.0(9) . . ? C61 C66 H66 120.0(5) . . ? C65 C66 H66 120.0(6) . . ? C2 C1 P1 154.0(7) . . ? C2 C1 Co1 72.4(4) . . ? P1 C1 Co1 119.1(4) . . ? C2 C1 Mo1 126.1(6) . . ? P1 C1 Mo1 79.7(3) . . ? Co1 C1 Mo1 83.9(3) . . ? C3 C2 C1 108.1(7) . . ? C3 C2 C71 126.5(7) . . ? C1 C2 C71 125.3(7) . . ? C3 C2 Co1 70.3(5) . . ? C1 C2 Co1 66.7(4) . . ? C71 C2 Co1 131.7(6) . . ? C2 C3 C4 117.3(7) . . ? C2 C3 Co1 70.5(5) . . ? C4 C3 Co1 69.1(5) . . ? C2 C3 H3 121.3(5) . . ? C4 C3 H3 121.3(5) . . ? Co1 C3 H3 131.5(2) . . ? C3 C4 C8 114.5(7) . . ? C3 C4 Co1 71.4(5) . . ? C8 C4 Co1 126.2(6) . . ? C3 C4 Mo1 114.6(6) . . ? C8 C4 Mo1 130.2(6) . . ? Co1 C4 Mo1 77.9(3) . . ? C11 C8 C9 107.2(8) . . ? C11 C8 C10 107.8(8) . . ? C9 C8 C10 107.0(8) . . ? C11 C8 C4 113.6(7) . . ? C9 C8 C4 113.1(8) . . ? C10 C8 C4 107.8(7) . . ? C8 C9 H9A 109.5(6) . . ? C8 C9 H9B 109.5(5) . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5(5) . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5(5) . . ? C8 C10 H10B 109.5(6) . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5(5) . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5(6) . . ? C8 C11 H11B 109.5(5) . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5(5) . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Mo1 Co1 C7 85.7(5) . . . . ? C1 Mo1 Co1 C7 -60.1(5) . . . . ? C4 Mo1 Co1 C7 -163.7(5) . . . . ? C84 Mo1 Co1 C7 -149.8(5) . . . . ? C83 Mo1 Co1 C7 157.9(5) . . . . ? C85 Mo1 Co1 C7 -95.6(5) . . . . ? C81 Mo1 Co1 C7 -18.6(8) . . . . ? C82 Mo1 Co1 C7 96.9(7) . . . . ? P1 Mo1 Co1 C7 -22.6(4) . . . . ? C5 Mo1 Co1 C6 -27.0(4) . . . . ? C1 Mo1 Co1 C6 -172.8(5) . . . . ? C4 Mo1 Co1 C6 83.6(4) . . . . ? C84 Mo1 Co1 C6 97.5(5) . . . . ? C83 Mo1 Co1 C6 45.2(5) . . . . ? C85 Mo1 Co1 C6 151.7(5) . . . . ? C81 Mo1 Co1 C6 -131.3(8) . . . . ? C82 Mo1 Co1 C6 -15.8(7) . . . . ? P1 Mo1 Co1 C6 -135.3(4) . . . . ? C5 Mo1 Co1 C1 145.9(4) . . . . ? C1 Mo1 Co1 C1 0.0 . . . . ? C4 Mo1 Co1 C1 -103.6(4) . . . . ? C84 Mo1 Co1 C1 -89.7(5) . . . . ? C83 Mo1 Co1 C1 -142.0(5) . . . . ? C85 Mo1 Co1 C1 -35.5(5) . . . . ? C81 Mo1 Co1 C1 41.6(8) . . . . ? C82 Mo1 Co1 C1 157.0(7) . . . . ? P1 Mo1 Co1 C1 37.5(3) . . . . ? C5 Mo1 Co1 C4 -110.5(4) . . . . ? C1 Mo1 Co1 C4 103.6(4) . . . . ? C4 Mo1 Co1 C4 0.0 . . . . ? C84 Mo1 Co1 C4 13.9(4) . . . . ? C83 Mo1 Co1 C4 -38.4(5) . . . . ? C85 Mo1 Co1 C4 68.1(5) . . . . ? C81 Mo1 Co1 C4 145.2(8) . . . . ? C82 Mo1 Co1 C4 -99.4(7) . . . . ? P1 Mo1 Co1 C4 141.1(3) . . . . ? C5 Mo1 Co1 C3 -144.1(3) . . . . ? C1 Mo1 Co1 C3 70.1(4) . . . . ? C4 Mo1 Co1 C3 -33.5(3) . . . . ? C84 Mo1 Co1 C3 -19.6(4) . . . . ? C83 Mo1 Co1 C3 -71.9(4) . . . . ? C85 Mo1 Co1 C3 34.6(4) . . . . ? C81 Mo1 Co1 C3 111.6(8) . . . . ? C82 Mo1 Co1 C3 -132.9(7) . . . . ? P1 Mo1 Co1 C3 107.6(2) . . . . ? C5 Mo1 Co1 C2 176.0(3) . . . . ? C1 Mo1 Co1 C2 30.2(4) . . . . ? C4 Mo1 Co1 C2 -73.4(3) . . . . ? C84 Mo1 Co1 C2 -59.5(4) . . . . ? C83 Mo1 Co1 C2 -111.8(4) . . . . ? C85 Mo1 Co1 C2 -5.3(4) . . . . ? C81 Mo1 Co1 C2 71.7(8) . . . . ? C82 Mo1 Co1 C2 -172.8(7) . . . . ? P1 Mo1 Co1 C2 67.7(2) . . . . ? C5 Mo1 P1 C1 -108.8(4) . . . . ? C1 Mo1 P1 C1 0.000(1) . . . . ? C4 Mo1 P1 C1 -9.5(4) . . . . ? C84 Mo1 P1 C1 95.5(4) . . . . ? C83 Mo1 P1 C1 138.8(5) . . . . ? C85 Mo1 P1 C1 106.3(4) . . . . ? C81 Mo1 P1 C1 140.6(4) . . . . ? C82 Mo1 P1 C1 162.0(4) . . . . ? Co1 Mo1 P1 C1 -40.6(3) . . . . ? C5 Mo1 P1 C61 -6.2(4) . . . . ? C1 Mo1 P1 C61 102.6(5) . . . . ? C4 Mo1 P1 C61 93.1(4) . . . . ? C84 Mo1 P1 C61 -161.9(4) . . . . ? C83 Mo1 P1 C61 -118.6(5) . . . . ? C85 Mo1 P1 C61 -151.1(4) . . . . ? C81 Mo1 P1 C61 -116.8(4) . . . . ? C82 Mo1 P1 C61 -95.4(4) . . . . ? Co1 Mo1 P1 C61 62.0(4) . . . . ? C5 Mo1 P1 C51 155.0(4) . . . . ? C1 Mo1 P1 C51 -96.2(4) . . . . ? C4 Mo1 P1 C51 -105.8(4) . . . . ? C84 Mo1 P1 C51 -0.7(4) . . . . ? C83 Mo1 P1 C51 42.6(5) . . . . ? C85 Mo1 P1 C51 10.0(4) . . . . ? C81 Mo1 P1 C51 44.3(4) . . . . ? C82 Mo1 P1 C51 65.7(4) . . . . ? Co1 Mo1 P1 C51 -136.8(3) . . . . ? C1 Mo1 C5 O5 -159.5(52) . . . . ? C4 Mo1 C5 O5 129.4(53) . . . . ? C84 Mo1 C5 O5 40.9(54) . . . . ? C83 Mo1 C5 O5 32.7(53) . . . . ? C85 Mo1 C5 O5 -5.0(56) . . . . ? C81 Mo1 C5 O5 -23.6(54) . . . . ? C82 Mo1 C5 O5 -1.7(53) . . . . ? P1 Mo1 C5 O5 -114.1(53) . . . . ? Co1 Mo1 C5 O5 173.8(54) . . . . ? C7 Co1 C6 O6 -20.9(79) . . . . ? C1 Co1 C6 O6 101.3(77) . . . . ? C4 Co1 C6 O6 169.5(78) . . . . ? C3 Co1 C6 O6 -155.7(78) . . . . ? C2 Co1 C6 O6 -134.0(76) . . . . ? Mo1 Co1 C6 O6 115.6(78) . . . . ? C6 Co1 C7 O7 -83.0(106) . . . . ? C1 Co1 C7 O7 115.9(106) . . . . ? C4 Co1 C7 O7 48.1(114) . . . . ? C3 Co1 C7 O7 46.2(107) . . . . ? C2 Co1 C7 O7 74.6(106) . . . . ? Mo1 Co1 C7 O7 156.9(104) . . . . ? C5 Mo1 C81 C82 41.0(6) . . . . ? C1 Mo1 C81 C82 173.7(5) . . . . ? C4 Mo1 C81 C82 -87.6(7) . . . . ? C84 Mo1 C81 C82 -79.9(6) . . . . ? C83 Mo1 C81 C82 -37.7(6) . . . . ? C85 Mo1 C81 C82 -119.1(8) . . . . ? C82 Mo1 C81 C82 0.000(2) . . . . ? P1 Mo1 C81 C82 143.5(6) . . . . ? Co1 Mo1 C81 C82 139.5(7) . . . . ? C5 Mo1 C81 C85 160.1(5) . . . . ? C1 Mo1 C81 C85 -67.2(6) . . . . ? C4 Mo1 C81 C85 31.4(8) . . . . ? C84 Mo1 C81 C85 39.1(5) . . . . ? C83 Mo1 C81 C85 81.3(6) . . . . ? C85 Mo1 C81 C85 0.000(1) . . . . ? C82 Mo1 C81 C85 119.1(8) . . . . ? P1 Mo1 C81 C85 -97.5(5) . . . . ? Co1 Mo1 C81 C85 -101.4(8) . . . . ? C85 C81 C82 C83 0.6(10) . . . . ? Mo1 C81 C82 C83 62.6(6) . . . . ? C85 C81 C82 Mo1 -62.1(6) . . . . ? Mo1 C81 C82 Mo1 0.0 . . . . ? C5 Mo1 C82 C81 -142.0(6) . . . . ? C1 Mo1 C82 C81 -12.1(10) . . . . ? C4 Mo1 C82 C81 129.5(6) . . . . ? C84 Mo1 C82 C81 77.7(6) . . . . ? C83 Mo1 C82 C81 116.0(8) . . . . ? C85 Mo1 C82 C81 35.7(5) . . . . ? C81 Mo1 C82 C81 0.0 . . . . ? P1 Mo1 C82 C81 -40.2(6) . . . . ? Co1 Mo1 C82 C81 -152.7(5) . . . . ? C5 Mo1 C82 C83 102.0(6) . . . . ? C1 Mo1 C82 C83 -128.1(8) . . . . ? C4 Mo1 C82 C83 13.5(7) . . . . ? C84 Mo1 C82 C83 -38.3(5) . . . . ? C83 Mo1 C82 C83 0.000(3) . . . . ? C85 Mo1 C82 C83 -80.4(6) . . . . ? C81 Mo1 C82 C83 -116.0(8) . . . . ? P1 Mo1 C82 C83 -156.2(5) . . . . ? Co1 Mo1 C82 C83 91.3(8) . . . . ? C81 C82 C83 C84 0.0(10) . . . . ? Mo1 C82 C83 C84 63.9(6) . . . . ? C81 C82 C83 Mo1 -63.9(6) . . . . ? Mo1 C82 C83 Mo1 0.000(1) . . . . ? C5 Mo1 C83 C84 168.5(6) . . . . ? C1 Mo1 C83 C84 13.7(10) . . . . ? C4 Mo1 C83 C84 75.6(6) . . . . ? C84 Mo1 C83 C84 0.000(4) . . . . ? C85 Mo1 C83 C84 -37.0(5) . . . . ? C81 Mo1 C83 C84 -77.8(6) . . . . ? C82 Mo1 C83 C84 -114.6(8) . . . . ? P1 Mo1 C83 C84 -75.8(7) . . . . ? Co1 Mo1 C83 C84 103.4(6) . . . . ? C5 Mo1 C83 C82 -76.9(6) . . . . ? C1 Mo1 C83 C82 128.3(7) . . . . ? C4 Mo1 C83 C82 -169.8(5) . . . . ? C84 Mo1 C83 C82 114.6(8) . . . . ? C85 Mo1 C83 C82 77.5(6) . . . . ? C81 Mo1 C83 C82 36.7(5) . . . . ? C82 Mo1 C83 C82 0.000(1) . . . . ? P1 Mo1 C83 C82 38.8(7) . . . . ? Co1 Mo1 C83 C82 -142.1(4) . . . . ? C82 C83 C84 C85 -0.6(10) . . . . ? Mo1 C83 C84 C85 65.4(6) . . . . ? C82 C83 C84 Mo1 -66.0(6) . . . . ? Mo1 C83 C84 Mo1 0.000(2) . . . . ? C5 Mo1 C84 C83 -14.3(7) . . . . ? C1 Mo1 C84 C83 -172.9(5) . . . . ? C4 Mo1 C84 C83 -105.6(6) . . . . ? C83 Mo1 C84 C83 0.000(5) . . . . ? C85 Mo1 C84 C83 117.0(8) . . . . ? C81 Mo1 C84 C83 78.9(6) . . . . ? C82 Mo1 C84 C83 38.1(5) . . . . ? P1 Mo1 C84 C83 135.6(5) . . . . ? Co1 Mo1 C84 C83 -115.9(5) . . . . ? C5 Mo1 C84 C85 -131.3(5) . . . . ? C1 Mo1 C84 C85 70.1(6) . . . . ? C4 Mo1 C84 C85 137.5(5) . . . . ? C83 Mo1 C84 C85 -117.0(8) . . . . ? C85 Mo1 C84 C85 0.000(1) . . . . ? C81 Mo1 C84 C85 -38.1(5) . . . . ? C82 Mo1 C84 C85 -78.8(6) . . . . ? P1 Mo1 C84 C85 18.7(6) . . . . ? Co1 Mo1 C84 C85 127.1(5) . . . . ? C82 C81 C85 C84 -0.9(10) . . . . ? Mo1 C81 C85 C84 -64.0(6) . . . . ? C82 C81 C85 Mo1 63.1(6) . . . . ? Mo1 C81 C85 Mo1 0.0 . . . . ? C83 C84 C85 C81 0.9(10) . . . . ? Mo1 C84 C85 C81 66.2(6) . . . . ? C83 C84 C85 Mo1 -65.3(6) . . . . ? Mo1 C84 C85 Mo1 0.0 . . . . ? C5 Mo1 C85 C81 -31.5(8) . . . . ? C1 Mo1 C85 C81 124.4(5) . . . . ? C4 Mo1 C85 C81 -160.8(5) . . . . ? C84 Mo1 C85 C81 -113.7(8) . . . . ? C83 Mo1 C85 C81 -76.8(6) . . . . ? C81 Mo1 C85 C81 0.000(1) . . . . ? C82 Mo1 C85 C81 -35.4(5) . . . . ? P1 Mo1 C85 C81 81.5(5) . . . . ? Co1 Mo1 C85 C81 150.5(4) . . . . ? C5 Mo1 C85 C84 82.2(7) . . . . ? C1 Mo1 C85 C84 -121.8(5) . . . . ? C4 Mo1 C85 C84 -47.1(6) . . . . ? C84 Mo1 C85 C84 0.000(2) . . . . ? C83 Mo1 C85 C84 36.9(5) . . . . ? C81 Mo1 C85 C84 113.7(8) . . . . ? C82 Mo1 C85 C84 78.3(6) . . . . ? P1 Mo1 C85 C84 -164.8(5) . . . . ? Co1 Mo1 C85 C84 -95.8(6) . . . . ? C76 C71 C72 C73 3.4(12) . . . . ? C2 C71 C72 C73 -174.4(8) . . . . ? C71 C72 C73 C74 -4.0(14) . . . . ? C72 C73 C74 C75 1.5(14) . . . . ? C73 C74 C75 C76 1.6(14) . . . . ? C74 C75 C76 C71 -2.1(13) . . . . ? C72 C71 C76 C75 -0.4(12) . . . . ? C2 C71 C76 C75 177.3(8) . . . . ? C1 P1 C51 C52 -171.8(7) . . . . ? C61 P1 C51 C52 56.4(8) . . . . ? Mo1 P1 C51 C52 -109.2(7) . . . . ? C1 P1 C51 C56 6.4(8) . . . . ? C61 P1 C51 C56 -125.4(7) . . . . ? Mo1 P1 C51 C56 69.0(7) . . . . ? C56 C51 C52 C53 0.7(13) . . . . ? P1 C51 C52 C53 178.9(7) . . . . ? C51 C52 C53 C54 -0.8(14) . . . . ? C52 C53 C54 C55 0.4(15) . . . . ? C53 C54 C55 C56 0.2(14) . . . . ? C52 C51 C56 C55 -0.1(13) . . . . ? P1 C51 C56 C55 -178.4(7) . . . . ? C54 C55 C56 C51 -0.3(14) . . . . ? C1 P1 C61 C62 84.4(7) . . . . ? C51 P1 C61 C62 -149.3(6) . . . . ? Mo1 P1 C61 C62 14.1(8) . . . . ? C1 P1 C61 C66 -96.9(7) . . . . ? C51 P1 C61 C66 29.4(8) . . . . ? Mo1 P1 C61 C66 -167.3(5) . . . . ? C66 C61 C62 C63 -1.4(12) . . . . ? P1 C61 C62 C63 177.3(7) . . . . ? C61 C62 C63 C64 0.9(13) . . . . ? C62 C63 C64 C65 0.1(14) . . . . ? C63 C64 C65 C66 -0.5(13) . . . . ? C62 C61 C66 C65 1.0(12) . . . . ? P1 C61 C66 C65 -177.7(6) . . . . ? C64 C65 C66 C61 0.0(13) . . . . ? C61 P1 C1 C2 64.7(15) . . . . ? C51 P1 C1 C2 -58.6(16) . . . . ? Mo1 P1 C1 C2 -172.4(16) . . . . ? C61 P1 C1 Co1 -45.9(6) . . . . ? C51 P1 C1 Co1 -169.2(4) . . . . ? Mo1 P1 C1 Co1 77.0(4) . . . . ? C61 P1 C1 Mo1 -122.9(4) . . . . ? C51 P1 C1 Mo1 113.8(3) . . . . ? Mo1 P1 C1 Mo1 0.0 . . . . ? C7 Co1 C1 C2 -90.1(5) . . . . ? C6 Co1 C1 C2 149.0(10) . . . . ? C4 Co1 C1 C2 76.7(5) . . . . ? C3 Co1 C1 C2 35.8(5) . . . . ? C2 Co1 C1 C2 0.0 . . . . ? Mo1 Co1 C1 C2 130.9(6) . . . . ? C7 Co1 C1 P1 64.4(6) . . . . ? C6 Co1 C1 P1 -56.5(13) . . . . ? C4 Co1 C1 P1 -128.8(6) . . . . ? C3 Co1 C1 P1 -169.8(6) . . . . ? C2 Co1 C1 P1 154.5(8) . . . . ? Mo1 Co1 C1 P1 -74.6(4) . . . . ? C7 Co1 C1 Mo1 139.0(3) . . . . ? C6 Co1 C1 Mo1 18.1(12) . . . . ? C4 Co1 C1 Mo1 -54.2(3) . . . . ? C3 Co1 C1 Mo1 -95.2(4) . . . . ? C2 Co1 C1 Mo1 -130.9(6) . . . . ? Mo1 Co1 C1 Mo1 0.0 . . . . ? C5 Mo1 C1 C2 -98.4(7) . . . . ? C4 Mo1 C1 C2 -13.2(6) . . . . ? C84 Mo1 C1 C2 63.2(8) . . . . ? C83 Mo1 C1 C2 54.3(11) . . . . ? C85 Mo1 C1 C2 97.2(7) . . . . ? C81 Mo1 C1 C2 129.5(6) . . . . ? C82 Mo1 C1 C2 137.3(7) . . . . ? P1 Mo1 C1 C2 175.9(9) . . . . ? Co1 Mo1 C1 C2 -63.0(6) . . . . ? C5 Mo1 C1 P1 85.8(4) . . . . ? C4 Mo1 C1 P1 170.9(4) . . . . ? C84 Mo1 C1 P1 -112.7(4) . . . . ? C83 Mo1 C1 P1 -121.6(6) . . . . ? C85 Mo1 C1 P1 -78.7(3) . . . . ? C81 Mo1 C1 P1 -46.4(4) . . . . ? C82 Mo1 C1 P1 -38.6(8) . . . . ? P1 Mo1 C1 P1 0.0 . . . . ? Co1 Mo1 C1 P1 121.1(4) . . . . ? C5 Mo1 C1 Co1 -35.3(4) . . . . ? C4 Mo1 C1 Co1 49.8(3) . . . . ? C84 Mo1 C1 Co1 126.2(3) . . . . ? C83 Mo1 C1 Co1 117.3(6) . . . . ? C85 Mo1 C1 Co1 160.2(3) . . . . ? C81 Mo1 C1 Co1 -167.4(3) . . . . ? C82 Mo1 C1 Co1 -159.7(6) . . . . ? P1 Mo1 C1 Co1 -121.1(4) . . . . ? Co1 Mo1 C1 Co1 0.0 . . . . ? P1 C1 C2 C3 -179.1(12) . . . . ? Co1 C1 C2 C3 -58.2(6) . . . . ? Mo1 C1 C2 C3 10.2(10) . . . . ? P1 C1 C2 C71 4.8(20) . . . . ? Co1 C1 C2 C71 125.7(8) . . . . ? Mo1 C1 C2 C71 -166.0(6) . . . . ? P1 C1 C2 Co1 -120.9(15) . . . . ? Co1 C1 C2 Co1 0.0 . . . . ? Mo1 C1 C2 Co1 68.4(5) . . . . ? C72 C71 C2 C3 -29.1(12) . . . . ? C76 C71 C2 C3 153.2(8) . . . . ? C72 C71 C2 C1 146.4(8) . . . . ? C76 C71 C2 C1 -31.3(12) . . . . ? C72 C71 C2 Co1 -124.6(8) . . . . ? C76 C71 C2 Co1 57.7(10) . . . . ? C7 Co1 C2 C3 -142.8(5) . . . . ? C6 Co1 C2 C3 -30.8(11) . . . . ? C1 Co1 C2 C3 120.9(7) . . . . ? C4 Co1 C2 C3 30.6(5) . . . . ? C3 Co1 C2 C3 0.000(2) . . . . ? Mo1 Co1 C2 C3 85.9(4) . . . . ? C7 Co1 C2 C1 96.2(5) . . . . ? C6 Co1 C2 C1 -151.7(9) . . . . ? C1 Co1 C2 C1 0.0 . . . . ? C4 Co1 C2 C1 -90.3(5) . . . . ? C3 Co1 C2 C1 -120.9(7) . . . . ? Mo1 Co1 C2 C1 -35.0(4) . . . . ? C7 Co1 C2 C71 -21.1(8) . . . . ? C6 Co1 C2 C71 91.0(11) . . . . ? C1 Co1 C2 C71 -117.3(9) . . . . ? C4 Co1 C2 C71 152.4(8) . . . . ? C3 Co1 C2 C71 121.8(9) . . . . ? Mo1 Co1 C2 C71 -152.3(7) . . . . ? C1 C2 C3 C4 3.4(11) . . . . ? C71 C2 C3 C4 179.5(8) . . . . ? Co1 C2 C3 C4 -52.6(7) . . . . ? C1 C2 C3 Co1 56.0(5) . . . . ? C71 C2 C3 Co1 -127.9(8) . . . . ? Co1 C2 C3 Co1 0.0 . . . . ? C7 Co1 C3 C2 48.4(6) . . . . ? C6 Co1 C3 C2 166.1(5) . . . . ? C1 Co1 C3 C2 -37.2(5) . . . . ? C4 Co1 C3 C2 -130.9(7) . . . . ? C2 Co1 C3 C2 0.000(1) . . . . ? Mo1 Co1 C3 C2 -86.4(4) . . . . ? C7 Co1 C3 C4 179.3(5) . . . . ? C6 Co1 C3 C4 -62.9(6) . . . . ? C1 Co1 C3 C4 93.7(5) . . . . ? C4 Co1 C3 C4 0.000(3) . . . . ? C2 Co1 C3 C4 130.9(7) . . . . ? Mo1 Co1 C3 C4 44.6(4) . . . . ? C2 C3 C4 C8 175.4(8) . . . . ? Co1 C3 C4 C8 122.1(7) . . . . ? C2 C3 C4 Co1 53.3(7) . . . . ? Co1 C3 C4 Co1 0.000(1) . . . . ? C2 C3 C4 Mo1 -13.3(10) . . . . ? Co1 C3 C4 Mo1 -66.6(5) . . . . ? C7 Co1 C4 C3 -2.4(17) . . . . ? C6 Co1 C4 C3 128.3(5) . . . . ? C1 Co1 C4 C3 -72.9(5) . . . . ? C3 Co1 C4 C3 0.000(3) . . . . ? C2 Co1 C4 C3 -30.4(4) . . . . ? Mo1 Co1 C4 C3 -121.4(5) . . . . ? C7 Co1 C4 C8 -109.6(16) . . . . ? C6 Co1 C4 C8 21.1(8) . . . . ? C1 Co1 C4 C8 179.9(8) . . . . ? C3 Co1 C4 C8 -107.2(9) . . . . ? C2 Co1 C4 C8 -137.6(8) . . . . ? Mo1 Co1 C4 C8 131.4(8) . . . . ? C7 Co1 C4 Mo1 119.0(15) . . . . ? C6 Co1 C4 Mo1 -110.3(3) . . . . ? C1 Co1 C4 Mo1 48.5(3) . . . . ? C3 Co1 C4 Mo1 121.4(5) . . . . ? C2 Co1 C4 Mo1 91.0(3) . . . . ? Mo1 Co1 C4 Mo1 0.0 . . . . ? C5 Mo1 C4 C3 126.1(7) . . . . ? C1 Mo1 C4 C3 13.3(6) . . . . ? C84 Mo1 C4 C3 -107.3(7) . . . . ? C83 Mo1 C4 C3 -141.5(7) . . . . ? C85 Mo1 C4 C3 -82.1(7) . . . . ? C81 Mo1 C4 C3 -100.8(8) . . . . ? C82 Mo1 C4 C3 -149.3(6) . . . . ? P1 Mo1 C4 C3 20.3(7) . . . . ? Co1 Mo1 C4 C3 62.8(6) . . . . ? C5 Mo1 C4 C8 -64.3(8) . . . . ? C1 Mo1 C4 C8 -177.0(9) . . . . ? C84 Mo1 C4 C8 62.3(8) . . . . ? C83 Mo1 C4 C8 28.1(8) . . . . ? C85 Mo1 C4 C8 87.6(8) . . . . ? C81 Mo1 C4 C8 68.8(10) . . . . ? C82 Mo1 C4 C8 20.3(10) . . . . ? P1 Mo1 C4 C8 -170.1(7) . . . . ? Co1 Mo1 C4 C8 -127.6(9) . . . . ? C5 Mo1 C4 Co1 63.2(3) . . . . ? C1 Mo1 C4 Co1 -49.5(3) . . . . ? C84 Mo1 C4 Co1 -170.1(3) . . . . ? C83 Mo1 C4 Co1 155.7(3) . . . . ? C85 Mo1 C4 Co1 -144.9(3) . . . . ? C81 Mo1 C4 Co1 -163.6(4) . . . . ? C82 Mo1 C4 Co1 147.9(3) . . . . ? P1 Mo1 C4 Co1 -42.5(3) . . . . ? Co1 Mo1 C4 Co1 0.0 . . . . ? C3 C4 C8 C11 -155.7(8) . . . . ? Co1 C4 C8 C11 -71.5(10) . . . . ? Mo1 C4 C8 C11 34.7(12) . . . . ? C3 C4 C8 C9 -33.2(12) . . . . ? Co1 C4 C8 C9 51.0(11) . . . . ? Mo1 C4 C8 C9 157.2(7) . . . . ? C3 C4 C8 C10 84.9(10) . . . . ? Co1 C4 C8 C10 169.1(7) . . . . ? Mo1 C4 C8 C10 -84.8(9) . . . . ? _refine_diff_density_max 2.075 _refine_diff_density_min -1.747 _refine_diff_density_rms 0.144 data_mm9804 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H34 Co Mo O4 P' _chemical_formula_weight 668.43 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 '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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.989(4) _cell_length_b 12.810(7) _cell_length_c 21.045(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.80(2) _cell_angle_gamma 90.00 _cell_volume 2888.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _exptl_crystal_description ? _exptl_crystal_colour 'v dark' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method ? _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.965 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method 'omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.6% _diffrn_reflns_number 6969 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6629 _reflns_number_observed 5319 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+1.0229P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6629 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_obs 0.0387 _refine_ls_wR_factor_all 0.1019 _refine_ls_wR_factor_obs 0.0932 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_obs 1.077 _refine_ls_restrained_S_all 1.050 _refine_ls_restrained_S_obs 1.077 _refine_ls_shift/esd_max 0.218 _refine_ls_shift/esd_mean 0.008 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.48915(2) 0.20220(2) 0.703912(12) 0.01941(8) Uani 1 d . . Co1 Co 0.39574(4) 0.19444(3) 0.57487(2) 0.01803(10) Uani 1 d . . P1 P 0.23245(7) 0.14239(6) 0.68072(3) 0.0178(2) Uani 1 d . . O5 O 0.6904(2) 0.0321(2) 0.69460(14) 0.0459(7) Uani 1 d . . C5 C 0.6151(3) 0.0947(3) 0.6940(2) 0.0301(7) Uani 1 d . . O6 O 0.4708(3) -0.0203(2) 0.57207(13) 0.0460(7) Uani 1 d . . C6 C 0.4434(3) 0.0658(3) 0.5762(2) 0.0303(7) Uani 1 d . . O7 O 0.3275(2) 0.1892(2) 0.43381(11) 0.0425(7) Uani 1 d . . C7 C 0.3521(3) 0.1926(2) 0.4897(2) 0.0263(7) Uani 1 d . . O1 O 0.3473(2) 0.0783(2) 0.71342(10) 0.0217(4) Uani 1 d . . C9 C 0.7474(4) 0.2456(4) 0.6209(3) 0.0610(14) Uani 1 d . . H9A H 0.8211(13) 0.2660(13) 0.6049(15) 0.092 Uiso 1 calc R . H9B H 0.7133(12) 0.1805(8) 0.5998(14) 0.092 Uiso 1 calc R . H9C H 0.7711(24) 0.2351(19) 0.6682(3) 0.092 Uiso 1 calc R . C10 C 0.7021(4) 0.4316(3) 0.6385(2) 0.0550(12) Uani 1 d . . H10A H 0.7767(17) 0.4518(14) 0.6233(12) 0.082 Uiso 1 calc R . H10B H 0.7241(27) 0.4211(8) 0.6858(3) 0.082 Uiso 1 calc R . H10C H 0.6393(11) 0.4870(7) 0.6279(12) 0.082 Uiso 1 calc R . C11 C 0.6288(4) 0.3487(4) 0.5310(2) 0.0523(11) Uani 1 d . . H11A H 0.7084(6) 0.3667(24) 0.5200(3) 0.078 Uiso 1 calc R . H11B H 0.5692(22) 0.4058(16) 0.5179(3) 0.078 Uiso 1 calc R . H11C H 0.5958(28) 0.2847(8) 0.5079(2) 0.078 Uiso 1 calc R . C8 C 0.6495(3) 0.3309(3) 0.6054(2) 0.0290(7) Uani 1 d . . C4 C 0.5257(3) 0.3007(2) 0.62545(15) 0.0212(6) Uani 1 d . . C3 C 0.4187(3) 0.3544(2) 0.59263(14) 0.0206(6) Uani 1 d . . H3 H 0.4248(3) 0.4022(2) 0.55587(14) 0.025 Uiso 1 calc R . C2 C 0.2963(3) 0.3220(2) 0.60082(14) 0.0187(6) Uani 1 d . . C12 C 0.1784(3) 0.3783(2) 0.56399(14) 0.0213(6) Uani 1 d . . C13 C 0.1778(3) 0.4861(2) 0.5961(2) 0.0320(7) Uani 1 d . . H13A H 0.1807(23) 0.4773(2) 0.6427(3) 0.048 Uiso 1 calc R . H13B H 0.1015(11) 0.5237(8) 0.5755(8) 0.048 Uiso 1 calc R . H13C H 0.2508(12) 0.5261(7) 0.5905(10) 0.048 Uiso 1 calc R . C14 C 0.0602(3) 0.3186(2) 0.5687(2) 0.0265(7) Uani 1 d . . H14A H 0.0539(11) 0.3148(15) 0.6144(2) 0.040 Uiso 1 calc R . H14B H 0.0640(10) 0.2478(6) 0.5516(10) 0.040 Uiso 1 calc R . H14C H -0.0130(3) 0.3548(10) 0.5432(9) 0.040 Uiso 1 calc R . C15 C 0.1774(3) 0.3942(3) 0.4918(2) 0.0311(7) Uani 1 d . . H15A H 0.1667(23) 0.3267(4) 0.4694(3) 0.047 Uiso 1 calc R . H15B H 0.2566(10) 0.4256(18) 0.4875(2) 0.047 Uiso 1 calc R . H15C H 0.1083(14) 0.4406(15) 0.4721(3) 0.047 Uiso 1 calc R . C1 C 0.3071(2) 0.2403(2) 0.64597(13) 0.0172(5) Uani 1 d . . C81 C 0.5627(3) 0.3498(3) 0.7636(2) 0.0377(8) Uani 1 d . . H81 H 0.5745(3) 0.4127(3) 0.7418(2) 0.045 Uiso 1 calc R . C82 C 0.6505(4) 0.2703(4) 0.7810(2) 0.0487(11) Uani 1 d . . H82 H 0.7328(4) 0.2697(4) 0.7737(2) 0.058 Uiso 1 calc R . C83 C 0.5948(4) 0.1904(3) 0.8116(2) 0.0500(11) Uani 1 d . . H83 H 0.6328(4) 0.1265(3) 0.8283(2) 0.060 Uiso 1 calc R . C84 C 0.4729(4) 0.2231(3) 0.8127(2) 0.0377(8) Uani 1 d . . H84 H 0.4138(4) 0.1850(3) 0.8302(2) 0.045 Uiso 1 calc R . C85 C 0.4544(3) 0.3211(3) 0.7836(2) 0.0306(7) Uani 1 d . . H85 H 0.3804(3) 0.3617(3) 0.7782(2) 0.037 Uiso 1 calc R . C51 C 0.1511(3) 0.1935(2) 0.73971(14) 0.0212(6) Uani 1 d . . C52 C 0.1057(3) 0.1240(3) 0.7801(2) 0.0307(7) Uani 1 d . . H52 H 0.1182(3) 0.0510(3) 0.7763(2) 0.037 Uiso 1 calc R . C53 C 0.0426(4) 0.1610(3) 0.8256(2) 0.0405(9) Uani 1 d . . H53 H 0.0137(4) 0.1134(3) 0.8535(2) 0.049 Uiso 1 calc R . C54 C 0.0215(3) 0.2663(3) 0.8306(2) 0.0373(8) Uani 1 d . . H54 H -0.0237(3) 0.2909(3) 0.8612(2) 0.045 Uiso 1 calc R . C55 C 0.0662(3) 0.3367(3) 0.7910(2) 0.0314(7) Uani 1 d . . H55 H 0.0525(3) 0.4094(3) 0.7946(2) 0.038 Uiso 1 calc R . C56 C 0.1311(3) 0.2996(2) 0.7462(2) 0.0252(6) Uani 1 d . . H56 H 0.1624(3) 0.3477(2) 0.7194(2) 0.030 Uiso 1 calc R . C61 C 0.1220(3) 0.0551(2) 0.63086(14) 0.0209(6) Uani 1 d . . C62 C -0.0062(3) 0.0662(2) 0.62416(15) 0.0248(6) Uani 1 d . . H62 H -0.0380(3) 0.1228(2) 0.64471(15) 0.030 Uiso 1 calc R . C63 C -0.0876(3) -0.0051(3) 0.5876(2) 0.0313(7) Uani 1 d . . H63 H -0.1750(3) 0.0027(3) 0.5831(2) 0.038 Uiso 1 calc R . C64 C -0.0417(3) -0.0873(3) 0.5578(2) 0.0329(7) Uani 1 d . . H64 H -0.0977(3) -0.1356(3) 0.5324(2) 0.039 Uiso 1 calc R . C65 C 0.0858(3) -0.0999(3) 0.5647(2) 0.0313(7) Uani 1 d . . H65 H 0.1171(3) -0.1571(3) 0.5444(2) 0.038 Uiso 1 calc R . C66 C 0.1671(3) -0.0293(2) 0.60116(15) 0.0257(6) Uani 1 d . . H66 H 0.2545(3) -0.0383(2) 0.60607(15) 0.031 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01713(13) 0.02092(13) 0.01928(13) -0.00038(10) 0.00209(9) 0.00345(10) Co1 0.0179(2) 0.0183(2) 0.0191(2) 0.00047(15) 0.00662(15) 0.00118(15) P1 0.0197(3) 0.0157(3) 0.0194(3) 0.0004(3) 0.0072(3) 0.0017(3) O5 0.0378(15) 0.0400(15) 0.063(2) 0.0128(13) 0.0176(13) 0.0213(12) C5 0.026(2) 0.031(2) 0.033(2) 0.0031(14) 0.0073(13) 0.0041(14) O6 0.074(2) 0.0252(13) 0.045(2) 0.0016(11) 0.0261(14) 0.0152(13) C6 0.039(2) 0.029(2) 0.027(2) 0.0019(13) 0.0163(14) 0.0056(14) O7 0.0403(15) 0.067(2) 0.0207(12) -0.0008(12) 0.0077(10) 0.0097(13) C7 0.025(2) 0.027(2) 0.029(2) 0.0002(13) 0.0111(13) 0.0023(13) O1 0.0216(10) 0.0204(10) 0.0240(10) 0.0046(8) 0.0070(8) 0.0032(8) C9 0.034(2) 0.056(3) 0.105(4) 0.034(3) 0.039(2) 0.015(2) C10 0.048(2) 0.054(3) 0.072(3) -0.019(2) 0.034(2) -0.028(2) C11 0.031(2) 0.081(3) 0.051(2) 0.003(2) 0.024(2) -0.012(2) C8 0.0181(14) 0.026(2) 0.045(2) 0.0020(14) 0.0111(13) -0.0002(12) C4 0.0169(13) 0.0199(14) 0.0271(15) 0.0005(12) 0.0058(11) 0.0006(11) C3 0.0201(14) 0.0163(13) 0.0258(15) 0.0005(11) 0.0056(11) -0.0028(11) C2 0.0149(13) 0.0170(13) 0.0244(14) -0.0003(11) 0.0050(11) 0.0001(10) C12 0.0152(13) 0.0201(14) 0.029(2) 0.0046(12) 0.0048(11) 0.0032(11) C13 0.029(2) 0.020(2) 0.044(2) 0.0007(14) 0.0034(14) 0.0057(13) C14 0.0178(14) 0.029(2) 0.032(2) 0.0052(13) 0.0033(12) 0.0010(12) C15 0.026(2) 0.036(2) 0.031(2) 0.0132(14) 0.0046(13) 0.0077(14) C1 0.0151(12) 0.0170(13) 0.0201(13) -0.0012(11) 0.0053(10) 0.0021(10) C81 0.039(2) 0.039(2) 0.035(2) -0.014(2) 0.008(2) -0.012(2) C82 0.027(2) 0.073(3) 0.041(2) -0.019(2) -0.004(2) -0.007(2) C83 0.062(3) 0.055(3) 0.023(2) -0.001(2) -0.012(2) 0.024(2) C84 0.053(2) 0.040(2) 0.021(2) -0.0040(14) 0.009(2) -0.004(2) C85 0.034(2) 0.033(2) 0.025(2) -0.0115(13) 0.0071(13) -0.0019(14) C51 0.0214(14) 0.0243(15) 0.0197(13) -0.0013(11) 0.0086(11) 0.0010(12) C52 0.042(2) 0.027(2) 0.027(2) 0.0005(13) 0.0164(14) -0.0030(14) C53 0.052(2) 0.042(2) 0.037(2) -0.003(2) 0.028(2) -0.014(2) C54 0.039(2) 0.042(2) 0.038(2) -0.013(2) 0.024(2) -0.003(2) C55 0.029(2) 0.027(2) 0.041(2) -0.0107(14) 0.0133(15) 0.0004(14) C56 0.025(2) 0.0228(15) 0.029(2) -0.0015(13) 0.0107(13) -0.0019(12) C61 0.0241(15) 0.0168(13) 0.0229(14) 0.0025(11) 0.0075(12) 0.0002(11) C62 0.0244(15) 0.0236(15) 0.028(2) -0.0011(12) 0.0081(12) 0.0003(12) C63 0.025(2) 0.032(2) 0.038(2) 0.0009(15) 0.0091(14) -0.0054(14) C64 0.040(2) 0.029(2) 0.030(2) -0.0050(14) 0.0077(14) -0.0126(15) C65 0.041(2) 0.026(2) 0.029(2) -0.0082(13) 0.0125(14) -0.0032(14) C66 0.031(2) 0.024(2) 0.0248(15) 0.0006(12) 0.0116(13) 0.0023(13) _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 C5 1.996(3) . ? Mo1 C1 2.155(3) . ? Mo1 C4 2.185(3) . ? Mo1 O1 2.264(2) . ? Mo1 C82 2.294(4) . ? Mo1 C83 2.310(3) . ? Mo1 C81 2.314(4) . ? Mo1 C84 2.350(3) . ? Mo1 C85 2.358(3) . ? Mo1 Co1 2.6839(7) . ? Mo1 P1 2.8588(13) . ? Co1 C6 1.728(3) . ? Co1 C7 1.751(3) . ? Co1 C1 2.044(3) . ? Co1 C4 2.086(3) . ? Co1 C3 2.088(3) . ? Co1 C2 2.104(3) . ? P1 O1 1.535(2) . ? P1 C1 1.745(3) . ? P1 C61 1.806(3) . ? P1 C51 1.806(3) . ? O5 C5 1.149(4) . ? O6 C6 1.152(4) . ? O7 C7 1.147(4) . ? C9 C8 1.518(5) . ? C10 C8 1.519(5) . ? C11 C8 1.548(5) . ? C8 C4 1.560(4) . ? C4 C3 1.405(4) . ? C3 C2 1.454(4) . ? C2 C1 1.401(4) . ? C2 C12 1.534(4) . ? C12 C14 1.530(4) . ? C12 C15 1.531(4) . ? C12 C13 1.538(4) . ? C81 C82 1.395(6) . ? C81 C85 1.397(5) . ? C82 C83 1.417(6) . ? C83 C84 1.408(6) . ? C84 C85 1.392(5) . ? C51 C56 1.388(4) . ? C51 C52 1.397(4) . ? C52 C53 1.385(5) . ? C53 C54 1.377(5) . ? C54 C55 1.389(5) . ? C55 C56 1.386(4) . ? C61 C62 1.392(4) . ? C61 C66 1.393(4) . ? C62 C63 1.386(4) . ? C63 C64 1.377(5) . ? C64 C65 1.386(5) . ? C65 C66 1.379(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Mo1 C1 132.44(12) . . ? C5 Mo1 C4 94.08(13) . . ? C1 Mo1 C4 75.22(11) . . ? C5 Mo1 O1 91.86(12) . . ? C1 Mo1 O1 68.76(9) . . ? C4 Mo1 O1 135.81(9) . . ? C5 Mo1 C82 83.77(15) . . ? C1 Mo1 C82 142.12(14) . . ? C4 Mo1 C82 94.15(15) . . ? O1 Mo1 C82 130.03(13) . . ? C5 Mo1 C83 81.28(14) . . ? C1 Mo1 C83 140.48(14) . . ? C4 Mo1 C83 129.96(15) . . ? O1 Mo1 C83 94.23(14) . . ? C82 Mo1 C83 35.8(2) . . ? C5 Mo1 C81 117.00(14) . . ? C1 Mo1 C81 106.91(12) . . ? C4 Mo1 C81 80.67(13) . . ? O1 Mo1 C81 133.57(11) . . ? C82 Mo1 C81 35.25(15) . . ? C83 Mo1 C81 58.81(15) . . ? C5 Mo1 C84 112.63(14) . . ? C1 Mo1 C84 105.31(12) . . ? C4 Mo1 C84 137.45(12) . . ? O1 Mo1 C84 77.96(11) . . ? C82 Mo1 C84 58.75(15) . . ? C83 Mo1 C84 35.17(14) . . ? C81 Mo1 C84 58.07(13) . . ? C5 Mo1 C85 138.22(13) . . ? C1 Mo1 C85 88.84(11) . . ? C4 Mo1 C85 104.50(12) . . ? O1 Mo1 C85 99.60(10) . . ? C82 Mo1 C85 58.21(14) . . ? C83 Mo1 C85 58.03(13) . . ? C81 Mo1 C85 34.77(12) . . ? C84 Mo1 C85 34.39(12) . . ? C5 Mo1 Co1 89.25(10) . . ? C1 Mo1 Co1 48.47(7) . . ? C4 Mo1 Co1 49.44(8) . . ? O1 Mo1 Co1 86.96(5) . . ? C82 Mo1 Co1 142.40(12) . . ? C83 Mo1 Co1 170.48(11) . . ? C81 Mo1 Co1 126.06(10) . . ? C84 Mo1 Co1 153.52(10) . . ? C85 Mo1 Co1 131.10(9) . . ? C5 Mo1 P1 118.55(10) . . ? C1 Mo1 P1 37.54(8) . . ? C4 Mo1 P1 111.44(8) . . ? O1 Mo1 P1 32.29(5) . . ? C82 Mo1 P1 143.26(11) . . ? C83 Mo1 P1 114.35(13) . . ? C81 Mo1 P1 121.62(9) . . ? C84 Mo1 P1 84.94(10) . . ? C85 Mo1 P1 89.15(9) . . ? Co1 Mo1 P1 71.07(3) . . ? C6 Co1 C7 90.97(15) . . ? C6 Co1 C1 117.00(13) . . ? C7 Co1 C1 133.40(13) . . ? C6 Co1 C4 116.29(15) . . ? C7 Co1 C4 122.19(13) . . ? C1 Co1 C4 79.78(11) . . ? C6 Co1 C3 155.35(15) . . ? C7 Co1 C3 101.05(13) . . ? C1 Co1 C3 69.24(11) . . ? C4 Co1 C3 39.34(11) . . ? C6 Co1 C2 155.47(13) . . ? C7 Co1 C2 103.67(13) . . ? C1 Co1 C2 39.46(11) . . ? C4 Co1 C2 72.38(11) . . ? C3 Co1 C2 40.59(11) . . ? C6 Co1 Mo1 88.40(11) . . ? C7 Co1 Mo1 173.43(10) . . ? C1 Co1 Mo1 52.12(8) . . ? C4 Co1 Mo1 52.72(8) . . ? C3 Co1 Mo1 77.21(8) . . ? C2 Co1 Mo1 79.22(8) . . ? O1 P1 C1 98.94(12) . . ? O1 P1 C61 108.02(13) . . ? C1 P1 C61 121.29(13) . . ? O1 P1 C51 111.66(13) . . ? C1 P1 C51 112.21(14) . . ? C61 P1 C51 104.64(14) . . ? O1 P1 Mo1 51.99(8) . . ? C1 P1 Mo1 48.79(9) . . ? C61 P1 Mo1 140.88(10) . . ? C51 P1 Mo1 113.94(10) . . ? O5 C5 Mo1 173.5(3) . . ? O6 C6 Co1 174.7(3) . . ? O7 C7 Co1 177.4(3) . . ? P1 O1 Mo1 95.72(10) . . ? C9 C8 C10 109.5(3) . . ? C9 C8 C11 105.2(3) . . ? C10 C8 C11 107.2(3) . . ? C9 C8 C4 112.4(3) . . ? C10 C8 C4 110.6(3) . . ? C11 C8 C4 111.7(3) . . ? C3 C4 C8 115.5(3) . . ? C3 C4 Co1 70.4(2) . . ? C8 C4 Co1 124.3(2) . . ? C3 C4 Mo1 112.4(2) . . ? C8 C4 Mo1 131.7(2) . . ? Co1 C4 Mo1 77.83(10) . . ? C4 C3 C2 119.8(3) . . ? C4 C3 Co1 70.2(2) . . ? C2 C3 Co1 70.3(2) . . ? C1 C2 C3 110.6(2) . . ? C1 C2 C12 129.0(2) . . ? C3 C2 C12 120.4(2) . . ? C1 C2 Co1 67.9(2) . . ? C3 C2 Co1 69.1(2) . . ? C12 C2 Co1 131.5(2) . . ? C14 C12 C15 108.1(3) . . ? C14 C12 C2 111.5(2) . . ? C15 C12 C2 112.6(2) . . ? C14 C12 C13 109.5(3) . . ? C15 C12 C13 108.5(3) . . ? C2 C12 C13 106.6(2) . . ? C2 C1 P1 147.5(2) . . ? C2 C1 Co1 72.6(2) . . ? P1 C1 Co1 116.42(15) . . ? C2 C1 Mo1 118.8(2) . . ? P1 C1 Mo1 93.68(12) . . ? Co1 C1 Mo1 79.41(9) . . ? C82 C81 C85 108.3(4) . . ? C82 C81 Mo1 71.6(2) . . ? C85 C81 Mo1 74.4(2) . . ? C81 C82 C83 107.7(4) . . ? C81 C82 Mo1 73.2(2) . . ? C83 C82 Mo1 72.7(2) . . ? C84 C83 C82 107.5(3) . . ? C84 C83 Mo1 73.9(2) . . ? C82 C83 Mo1 71.4(2) . . ? C85 C84 C83 107.9(4) . . ? C85 C84 Mo1 73.1(2) . . ? C83 C84 Mo1 70.9(2) . . ? C84 C85 C81 108.6(3) . . ? C84 C85 Mo1 72.5(2) . . ? C81 C85 Mo1 70.9(2) . . ? C56 C51 C52 118.6(3) . . ? C56 C51 P1 122.4(2) . . ? C52 C51 P1 119.0(2) . . ? C53 C52 C51 120.2(3) . . ? C54 C53 C52 120.6(3) . . ? C53 C54 C55 120.0(3) . . ? C56 C55 C54 119.3(3) . . ? C55 C56 C51 121.3(3) . . ? C62 C61 C66 119.1(3) . . ? C62 C61 P1 122.0(2) . . ? C66 C61 P1 118.8(2) . . ? C63 C62 C61 120.2(3) . . ? C64 C63 C62 120.0(3) . . ? C63 C64 C65 120.4(3) . . ? C66 C65 C64 119.8(3) . . ? C65 C66 C61 120.5(3) . . ? _refine_diff_density_max 0.467 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.090 data_mm9803 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C47 H43 Cl2 Co Mo O7 P2' _chemical_formula_weight 1007.52 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 '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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.676(7) _cell_length_b 18.323(4) _cell_length_c 12.021(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.79(3) _cell_angle_gamma 90.00 _cell_volume 4441.1(28) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'v dark' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method ? _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device AFC5R _diffrn_measurement_method 'omega/2theta scans ' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1% _diffrn_reflns_number 10808 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.1470 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 999 _diffrn_reflns_limit_k_min -999 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 999 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.45 _reflns_number_total 7844 _reflns_number_observed 4528 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 22 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+4.5819P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7822 _refine_ls_number_parameters 535 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1412 _refine_ls_R_factor_obs 0.0569 _refine_ls_wR_factor_all 0.1449 _refine_ls_wR_factor_obs 0.1085 _refine_ls_goodness_of_fit_all 1.014 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 1.092 _refine_ls_restrained_S_obs 1.102 _refine_ls_shift/esd_max 0.111 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.18178(3) -0.04615(3) 0.53742(5) 0.0191(2) Uani 1 d . . Co1 Co 0.17304(4) -0.00313(5) 0.74443(7) 0.0168(2) Uani 1 d . . P1 P 0.18457(8) -0.11883(10) 0.70778(14) 0.0201(4) Uani 1 d . . P2 P 0.21466(8) 0.03949(10) 0.91697(13) 0.0191(4) Uani 1 d . . O1 O 0.0293(2) -0.0819(3) 0.5022(4) 0.0406(13) Uani 1 d . . C1 C 0.0851(4) -0.0669(4) 0.5186(5) 0.027(2) Uani 1 d . . O2 O 0.0324(3) 0.0209(3) 0.7368(4) 0.0422(14) Uani 1 d . . C2 C 0.0881(3) 0.0102(4) 0.7400(5) 0.024(2) Uani 1 d . . C3 C 0.4070(3) -0.0726(4) 0.7557(7) 0.041(2) Uani 1 d . . H3A H 0.4148(3) -0.1229(9) 0.7829(38) 0.061 Uiso 1 calc R . H3B H 0.4275(5) -0.0388(18) 0.8165(29) 0.061 Uiso 1 calc R . H3C H 0.4265(5) -0.0652(26) 0.6893(13) 0.061 Uiso 1 calc R . O3 O 0.3367(2) -0.0590(2) 0.7239(4) 0.0325(12) Uani 1 d . . C4 C 0.3169(3) 0.0106(4) 0.7059(5) 0.0206(15) Uani 1 d . . O4 O 0.3571(2) 0.0600(3) 0.7143(4) 0.0377(13) Uani 1 d . . C5 C 0.2447(3) 0.0188(3) 0.6709(5) 0.0170(14) Uani 1 d . . O5 O 0.1409(2) 0.1768(2) 0.5773(4) 0.0258(11) Uani 1 d . . C6 C 0.2126(3) 0.0878(3) 0.6816(5) 0.0152(14) Uani 1 d . . O6 O 0.1484(2) 0.0678(2) 0.4968(3) 0.0217(10) Uani 1 d . . C7 C 0.1653(3) 0.1101(3) 0.5803(5) 0.0207(15) Uani 1 d . . C8 C 0.0947(4) 0.1988(4) 0.4716(6) 0.039(2) Uani 1 d . . H8A H 0.0792(18) 0.2487(10) 0.4799(15) 0.058 Uiso 1 calc R . H8B H 0.0566(12) 0.1655(16) 0.4564(22) 0.058 Uiso 1 calc R . H8C H 0.1172(8) 0.1969(25) 0.4081(9) 0.058 Uiso 1 calc R . C9 C 0.2406(3) 0.1436(3) 0.7722(5) 0.0187(14) Uani 1 d . . C10 C 0.2440(3) 0.1274(3) 0.8818(5) 0.0184(14) Uani 1 d . . H10 H 0.2616(3) 0.1616(3) 0.9401(5) 0.022 Uiso 1 calc R . C11 C 0.2699(3) 0.2134(3) 0.7420(5) 0.0179(14) Uani 1 d . . C12 C 0.3005(3) 0.2159(4) 0.6484(5) 0.023(2) Uani 1 d . . H12 H 0.2966(3) 0.1758(4) 0.5973(5) 0.028 Uiso 1 calc R . C13 C 0.3362(3) 0.2770(4) 0.6314(6) 0.035(2) Uani 1 d . . H13 H 0.3586(3) 0.2774(4) 0.5705(6) 0.042 Uiso 1 calc R . C14 C 0.3400(4) 0.3373(4) 0.7003(7) 0.039(2) Uani 1 d . . H14 H 0.3648(4) 0.3788(4) 0.6870(7) 0.047 Uiso 1 calc R . C15 C 0.3079(4) 0.3374(4) 0.7881(7) 0.039(2) Uani 1 d . . H15 H 0.3094(4) 0.3793(4) 0.8351(7) 0.047 Uiso 1 calc R . C16 C 0.2728(3) 0.2753(4) 0.8085(6) 0.029(2) Uani 1 d . . H16 H 0.2505(3) 0.2757(4) 0.8696(6) 0.035 Uiso 1 calc R . C17 C 0.2691(4) -0.0465(4) 0.4427(6) 0.034(2) Uani 1 d . . H17 H 0.3074(4) -0.0169(4) 0.4668(6) 0.041 Uiso 1 calc R . C18 C 0.2600(4) -0.1173(4) 0.4828(6) 0.040(2) Uani 1 d . . H18 H 0.2907(4) -0.1439(4) 0.5386(6) 0.048 Uiso 1 calc R . C19 C 0.1961(5) -0.1414(4) 0.4239(6) 0.045(2) Uani 1 d . . H19 H 0.1762(5) -0.1871(4) 0.4334(6) 0.054 Uiso 1 calc R . C20 C 0.1681(4) -0.0852(5) 0.3491(6) 0.040(2) Uani 1 d . . H20 H 0.1258(4) -0.0867(5) 0.2982(6) 0.048 Uiso 1 calc R . C21 C 0.2122(4) -0.0272(4) 0.3618(6) 0.031(2) Uani 1 d . . H21 H 0.2050(4) 0.0179(4) 0.3221(6) 0.037 Uiso 1 calc R . C22 C 0.2552(3) -0.1750(4) 0.7828(6) 0.023(2) Uani 1 d . . C23 C 0.2827(3) -0.1629(4) 0.8965(6) 0.029(2) Uani 1 d . . H23 H 0.2644(3) -0.1263(4) 0.9364(6) 0.035 Uiso 1 calc R . C24 C 0.3363(4) -0.2031(4) 0.9534(7) 0.039(2) Uani 1 d . . H24 H 0.3547(4) -0.1939(4) 1.0318(7) 0.046 Uiso 1 calc R . C25 C 0.3633(4) -0.2567(4) 0.8967(7) 0.036(2) Uani 1 d . . H25 H 0.4009(4) -0.2836(4) 0.9350(7) 0.044 Uiso 1 calc R . C26 C 0.3350(4) -0.2706(4) 0.7844(7) 0.038(2) Uani 1 d . . H26 H 0.3526(4) -0.3083(4) 0.7453(7) 0.045 Uiso 1 calc R . C27 C 0.2813(4) -0.2305(4) 0.7275(6) 0.035(2) Uani 1 d . . H27 H 0.2620(4) -0.2410(4) 0.6498(6) 0.042 Uiso 1 calc R . C28 C 0.1179(3) -0.1859(3) 0.7120(5) 0.0205(15) Uani 1 d . . C29 C 0.0836(4) -0.1834(4) 0.7985(6) 0.032(2) Uani 1 d . . H29 H 0.0923(4) -0.1453(4) 0.8533(6) 0.038 Uiso 1 calc R . C30 C 0.0361(4) -0.2366(4) 0.8061(7) 0.037(2) Uani 1 d . . H30 H 0.0132(4) -0.2347(4) 0.8664(7) 0.045 Uiso 1 calc R . C31 C 0.0225(4) -0.2918(4) 0.7264(7) 0.041(2) Uani 1 d . . H31 H -0.0099(4) -0.3278(4) 0.7312(7) 0.050 Uiso 1 calc R . C32 C 0.0562(4) -0.2943(4) 0.6394(7) 0.044(2) Uani 1 d . . H32 H 0.0473(4) -0.3323(4) 0.5845(7) 0.053 Uiso 1 calc R . C33 C 0.1031(4) -0.2416(4) 0.6317(6) 0.034(2) Uani 1 d . . H33 H 0.1255(4) -0.2436(4) 0.5708(6) 0.041 Uiso 1 calc R . C34 C 0.1582(3) 0.0587(3) 1.0124(5) 0.0209(15) Uani 1 d . . C35 C 0.1631(3) 0.1226(4) 1.0767(6) 0.028(2) Uani 1 d . . H35 H 0.1948(3) 0.1587(4) 1.0693(6) 0.034 Uiso 1 calc R . C36 C 0.1217(4) 0.1336(4) 1.1514(6) 0.034(2) Uani 1 d . . H36 H 0.1244(4) 0.1776(4) 1.1939(6) 0.041 Uiso 1 calc R . C37 C 0.0762(4) 0.0800(4) 1.1643(6) 0.033(2) Uani 1 d . . H37 H 0.0480(4) 0.0873(4) 1.2159(6) 0.040 Uiso 1 calc R . C38 C 0.0721(3) 0.0170(4) 1.1027(6) 0.031(2) Uani 1 d . . H38 H 0.0413(3) -0.0197(4) 1.1120(6) 0.038 Uiso 1 calc R . C39 C 0.1125(3) 0.0064(4) 1.0267(6) 0.032(2) Uani 1 d . . H39 H 0.1089(3) -0.0375(4) 0.9837(6) 0.038 Uiso 1 calc R . C40 C 0.2892(3) 0.0087(3) 1.0208(5) 0.0210(15) Uani 1 d . . C41 C 0.2856(3) -0.0238(3) 1.1244(5) 0.025(2) Uani 1 d . . H41 H 0.2435(3) -0.0314(3) 1.1421(5) 0.031 Uiso 1 calc R . C42 C 0.3426(4) -0.0452(4) 1.2018(6) 0.039(2) Uani 1 d . . H42 H 0.3392(4) -0.0660(4) 1.2727(6) 0.047 Uiso 1 calc R . C43 C 0.4041(4) -0.0365(4) 1.1769(6) 0.037(2) Uani 1 d . . H43 H 0.4432(4) -0.0518(4) 1.2293(6) 0.045 Uiso 1 calc R . C44 C 0.4079(4) -0.0048(4) 1.0734(6) 0.035(2) Uani 1 d . . H44 H 0.4500(4) 0.0018(4) 1.0553(6) 0.042 Uiso 1 calc R . C45 C 0.3514(3) 0.0172(3) 0.9966(4) 0.028(2) Uani 1 d . . H45 H 0.3550(3) 0.0386(3) 0.9263(4) 0.033 Uiso 1 calc R . C46 C 0.4485(3) 0.1922(3) 0.8480(4) 0.054(2) Uani 1 d RD . H46A H 0.4109(3) 0.2262(3) 0.8441(4) 0.065 Uiso 1 calc R . H46B H 0.4317(3) 0.1490(3) 0.8008(4) 0.065 Uiso 1 calc R . Cl1 Cl 0.47670(11) 0.16455(15) 0.9876(2) 0.0631(7) Uani 1 d D . Cl2 Cl 0.50883(12) 0.2348(2) 0.7906(2) 0.0757(8) Uani 1 d D . C47 C 0.5358(9) -0.3884(9) 0.9950(14) 0.138(4) Uiso 1 d D . O7 O 0.5687(8) -0.4385(9) 0.9624(14) 0.138(4) Uiso 0.645(11) d PD 1 O7' O 0.4638(14) -0.4174(16) 0.9768(24) 0.138(4) Uiso 0.355(11) d PD 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 0.0246(3) 0.0177(3) 0.0154(3) -0.0012(3) 0.0053(2) -0.0017(3) Co1 0.0203(5) 0.0146(4) 0.0165(4) -0.0001(4) 0.0059(4) -0.0010(4) P1 0.0233(9) 0.0185(9) 0.0183(8) -0.0015(7) 0.0042(7) -0.0011(8) P2 0.0227(9) 0.0193(9) 0.0161(8) 0.0005(8) 0.0059(7) -0.0022(8) O1 0.030(3) 0.041(3) 0.045(3) 0.007(3) -0.005(3) -0.006(3) C1 0.033(4) 0.026(4) 0.018(3) -0.001(3) -0.002(3) -0.005(3) O2 0.029(3) 0.059(4) 0.042(3) 0.006(3) 0.014(2) 0.011(3) C2 0.027(4) 0.018(4) 0.026(4) 0.000(3) 0.004(3) -0.002(3) C3 0.026(4) 0.048(5) 0.051(5) 0.011(4) 0.014(4) 0.010(4) O3 0.024(3) 0.021(3) 0.052(3) 0.006(2) 0.007(2) 0.004(2) C4 0.024(4) 0.022(4) 0.016(3) 0.004(3) 0.005(3) 0.008(3) O4 0.024(3) 0.021(3) 0.066(4) 0.009(3) 0.005(3) -0.006(2) C5 0.024(4) 0.015(3) 0.013(3) 0.006(3) 0.006(3) 0.002(3) O5 0.028(3) 0.020(3) 0.025(2) 0.001(2) -0.002(2) 0.004(2) C6 0.016(3) 0.013(3) 0.018(3) 0.001(3) 0.008(3) -0.002(3) O6 0.025(3) 0.022(3) 0.016(2) 0.001(2) 0.000(2) 0.001(2) C7 0.024(4) 0.014(3) 0.028(4) 0.002(3) 0.014(3) -0.005(3) C8 0.036(4) 0.029(4) 0.047(5) 0.011(4) -0.001(4) 0.006(4) C9 0.016(3) 0.017(3) 0.025(4) -0.002(3) 0.008(3) 0.004(3) C10 0.021(4) 0.015(3) 0.019(3) -0.005(3) 0.002(3) -0.003(3) C11 0.011(3) 0.015(3) 0.023(3) 0.003(3) -0.008(3) -0.004(3) C12 0.016(3) 0.024(4) 0.027(4) 0.006(3) 0.001(3) -0.004(3) C13 0.029(4) 0.036(5) 0.035(4) 0.015(4) -0.001(3) -0.005(4) C14 0.039(5) 0.020(4) 0.050(5) 0.020(4) -0.006(4) -0.014(4) C15 0.047(5) 0.019(4) 0.043(5) 0.004(4) -0.010(4) -0.003(4) C16 0.036(4) 0.021(4) 0.027(4) 0.003(3) 0.000(3) -0.001(3) C17 0.036(4) 0.044(5) 0.027(4) -0.005(4) 0.017(3) -0.001(4) C18 0.059(6) 0.043(5) 0.026(4) 0.005(4) 0.026(4) 0.020(4) C19 0.080(7) 0.035(5) 0.028(4) -0.010(4) 0.027(5) -0.008(5) C20 0.050(5) 0.056(6) 0.017(4) -0.006(4) 0.014(4) -0.009(5) C21 0.050(5) 0.026(4) 0.021(4) 0.005(3) 0.020(3) 0.004(4) C22 0.026(4) 0.018(4) 0.029(4) 0.003(3) 0.011(3) -0.002(3) C23 0.038(4) 0.024(4) 0.024(4) -0.002(3) 0.005(3) -0.002(3) C24 0.038(5) 0.039(5) 0.035(4) 0.008(4) 0.000(4) -0.006(4) C25 0.028(4) 0.032(4) 0.049(5) 0.015(4) 0.008(4) 0.006(4) C26 0.043(5) 0.023(4) 0.050(5) 0.009(4) 0.013(4) 0.014(4) C27 0.051(5) 0.028(4) 0.030(4) 0.002(3) 0.017(4) 0.007(4) C28 0.020(4) 0.015(3) 0.024(3) 0.003(3) 0.001(3) 0.001(3) C29 0.038(4) 0.029(4) 0.031(4) -0.002(3) 0.011(4) -0.001(4) C30 0.032(4) 0.033(5) 0.048(5) 0.007(4) 0.013(4) -0.005(4) C31 0.033(4) 0.027(4) 0.057(5) 0.025(4) -0.006(4) -0.008(4) C32 0.056(6) 0.028(5) 0.044(5) -0.007(4) 0.000(4) -0.010(4) C33 0.045(5) 0.025(4) 0.031(4) -0.002(3) 0.006(4) -0.007(4) C34 0.022(3) 0.024(4) 0.018(3) 0.004(3) 0.008(3) -0.001(3) C35 0.030(4) 0.027(4) 0.032(4) -0.004(3) 0.016(3) -0.004(3) C36 0.035(4) 0.032(4) 0.039(4) -0.001(4) 0.018(4) 0.004(4) C37 0.031(4) 0.041(5) 0.029(4) -0.004(4) 0.011(3) 0.012(4) C38 0.029(4) 0.037(5) 0.032(4) -0.002(4) 0.014(3) -0.010(3) C39 0.038(4) 0.034(4) 0.029(4) -0.009(4) 0.017(3) -0.006(4) C40 0.029(4) 0.014(3) 0.021(3) -0.004(3) 0.008(3) 0.000(3) C41 0.032(4) 0.021(4) 0.027(4) 0.005(3) 0.013(3) 0.004(3) C42 0.055(5) 0.039(5) 0.026(4) 0.005(4) 0.016(4) 0.016(4) C43 0.042(5) 0.035(5) 0.032(4) 0.003(4) 0.003(3) 0.021(4) C44 0.034(4) 0.035(4) 0.036(4) -0.006(4) 0.009(3) 0.002(4) C45 0.035(4) 0.030(4) 0.018(3) 0.000(3) 0.003(3) 0.001(3) C46 0.036(5) 0.057(6) 0.065(6) 0.001(5) -0.001(4) -0.018(4) Cl1 0.0488(14) 0.078(2) 0.0614(15) 0.0216(14) 0.0107(12) 0.0025(13) Cl2 0.0523(15) 0.109(2) 0.070(2) 0.034(2) 0.0209(13) 0.001(2) _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 C1 1.998(7) . ? Mo1 C5 2.181(6) . ? Mo1 O6 2.219(4) . ? Mo1 C19 2.275(7) . ? Mo1 C18 2.283(7) . ? Mo1 C20 2.331(7) . ? Mo1 C17 2.337(7) . ? Mo1 C21 2.359(6) . ? Mo1 P1 2.433(2) . ? Mo1 Co1 2.654(2) . ? Co1 C2 1.762(7) . ? Co1 C5 1.927(6) . ? Co1 C6 2.072(6) . ? Co1 P1 2.189(2) . ? Co1 P2 2.205(2) . ? P1 C22 1.850(7) . ? P1 C28 1.855(6) . ? P2 C10 1.804(6) . ? P2 C34 1.843(6) . ? P2 C40 1.843(7) . ? O1 C1 1.160(8) . ? O2 C2 1.161(7) . ? C3 O3 1.439(8) . ? O3 C4 1.343(8) . ? C4 O4 1.217(8) . ? C4 C5 1.467(8) . ? C5 C6 1.446(8) . ? O5 C7 1.320(7) . ? O5 C8 1.467(8) . ? C6 C7 1.442(9) . ? C6 C9 1.512(8) . ? O6 C7 1.255(7) . ? C9 C10 1.338(9) . ? C9 C11 1.494(8) . ? C11 C16 1.381(9) . ? C11 C12 1.409(8) . ? C12 C13 1.382(9) . ? C13 C14 1.372(10) . ? C14 C15 1.365(11) . ? C15 C16 1.400(10) . ? C17 C21 1.395(10) . ? C17 C18 1.411(10) . ? C18 C19 1.424(11) . ? C19 C20 1.405(11) . ? C20 C21 1.387(10) . ? C22 C23 1.377(9) . ? C22 C27 1.388(9) . ? C23 C24 1.380(10) . ? C24 C25 1.382(10) . ? C25 C26 1.371(10) . ? C26 C27 1.381(10) . ? C28 C29 1.384(9) . ? C28 C33 1.392(9) . ? C29 C30 1.401(10) . ? C30 C31 1.378(10) . ? C31 C32 1.380(11) . ? C32 C33 1.385(10) . ? C34 C39 1.383(9) . ? C34 C35 1.394(9) . ? C35 C36 1.385(9) . ? C36 C37 1.392(10) . ? C37 C38 1.363(10) . ? C38 C39 1.382(9) . ? C40 C45 1.389(8) . ? C40 C41 1.397(9) . ? C41 C42 1.386(10) . ? C42 C43 1.381(10) . ? C43 C44 1.391(10) . ? C44 C45 1.380(9) . ? C46 Cl1 1.727(6) . ? C46 Cl2 1.739(6) . ? C47 O7 1.26(2) . ? C47 O7' 1.55(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 C1 Mo1 C5 127.3(2) . . ? C1 Mo1 O6 84.2(2) . . ? C5 Mo1 O6 75.8(2) . . ? C1 Mo1 C19 92.6(3) . . ? C5 Mo1 C19 136.4(3) . . ? O6 Mo1 C19 131.7(2) . . ? C1 Mo1 C18 127.8(3) . . ? C5 Mo1 C18 100.3(3) . . ? O6 Mo1 C18 132.8(2) . . ? C19 Mo1 C18 36.4(3) . . ? C1 Mo1 C20 85.9(3) . . ? C5 Mo1 C20 143.8(2) . . ? O6 Mo1 C20 96.3(2) . . ? C19 Mo1 C20 35.5(3) . . ? C18 Mo1 C20 59.1(3) . . ? C1 Mo1 C17 143.7(3) . . ? C5 Mo1 C17 87.8(2) . . ? O6 Mo1 C17 97.5(2) . . ? C19 Mo1 C17 59.3(3) . . ? C18 Mo1 C17 35.5(3) . . ? C20 Mo1 C17 57.8(3) . . ? C1 Mo1 C21 112.7(3) . . ? C5 Mo1 C21 110.2(2) . . ? O6 Mo1 C21 78.3(2) . . ? C19 Mo1 C21 58.7(3) . . ? C18 Mo1 C21 58.7(3) . . ? C20 Mo1 C21 34.4(2) . . ? C17 Mo1 C21 34.6(2) . . ? C1 Mo1 P1 80.1(2) . . ? C5 Mo1 P1 77.3(2) . . ? O6 Mo1 P1 130.43(12) . . ? C19 Mo1 P1 95.9(2) . . ? C18 Mo1 P1 92.5(2) . . ? C20 Mo1 P1 128.6(2) . . ? C17 Mo1 P1 122.1(2) . . ? C21 Mo1 P1 150.8(2) . . ? C1 Mo1 Co1 83.6(2) . . ? C5 Mo1 Co1 45.7(2) . . ? O6 Mo1 Co1 81.06(11) . . ? C19 Mo1 Co1 146.6(2) . . ? C18 Mo1 Co1 129.7(2) . . ? C20 Mo1 Co1 169.4(2) . . ? C17 Mo1 Co1 132.6(2) . . ? C21 Mo1 Co1 152.0(2) . . ? P1 Mo1 Co1 50.75(5) . . ? C2 Co1 C5 145.0(3) . . ? C2 Co1 C6 110.5(3) . . ? C5 Co1 C6 42.2(2) . . ? C2 Co1 P1 106.3(2) . . ? C5 Co1 P1 88.9(2) . . ? C6 Co1 P1 129.5(2) . . ? C2 Co1 P2 99.1(2) . . ? C5 Co1 P2 100.2(2) . . ? C6 Co1 P2 87.4(2) . . ? P1 Co1 P2 119.67(7) . . ? C2 Co1 Mo1 106.7(2) . . ? C5 Co1 Mo1 54.1(2) . . ? C6 Co1 Mo1 77.4(2) . . ? P1 Co1 Mo1 59.38(5) . . ? P2 Co1 Mo1 153.33(6) . . ? C22 P1 C28 97.5(3) . . ? C22 P1 Co1 123.4(2) . . ? C28 P1 Co1 121.4(2) . . ? C22 P1 Mo1 125.7(2) . . ? C28 P1 Mo1 120.4(2) . . ? Co1 P1 Mo1 69.88(6) . . ? C10 P2 C34 105.5(3) . . ? C10 P2 C40 99.1(3) . . ? C34 P2 C40 100.7(3) . . ? C10 P2 Co1 100.2(2) . . ? C34 P2 Co1 119.0(2) . . ? C40 P2 Co1 128.5(2) . . ? O1 C1 Mo1 175.7(6) . . ? O2 C2 Co1 178.2(6) . . ? C4 O3 C3 117.4(5) . . ? O4 C4 O3 120.9(6) . . ? O4 C4 C5 125.5(6) . . ? O3 C4 C5 113.5(6) . . ? C6 C5 C4 121.4(6) . . ? C6 C5 Co1 74.3(3) . . ? C4 C5 Co1 133.2(4) . . ? C6 C5 Mo1 109.4(4) . . ? C4 C5 Mo1 124.0(4) . . ? Co1 C5 Mo1 80.2(2) . . ? C7 O5 C8 116.8(5) . . ? C7 C6 C5 114.3(5) . . ? C7 C6 C9 119.8(5) . . ? C5 C6 C9 123.1(5) . . ? C7 C6 Co1 106.6(4) . . ? C5 C6 Co1 63.5(3) . . ? C9 C6 Co1 113.6(4) . . ? C7 O6 Mo1 112.8(4) . . ? O6 C7 O5 120.8(6) . . ? O6 C7 C6 121.2(6) . . ? O5 C7 C6 118.0(6) . . ? C10 C9 C11 119.5(6) . . ? C10 C9 C6 119.2(6) . . ? C11 C9 C6 121.0(5) . . ? C9 C10 P2 118.8(5) . . ? C16 C11 C12 117.8(6) . . ? C16 C11 C9 122.1(6) . . ? C12 C11 C9 119.9(6) . . ? C13 C12 C11 119.6(7) . . ? C14 C13 C12 121.6(7) . . ? C15 C14 C13 119.7(7) . . ? C14 C15 C16 119.6(7) . . ? C11 C16 C15 121.6(7) . . ? C21 C17 C18 108.3(7) . . ? C21 C17 Mo1 73.5(4) . . ? C18 C17 Mo1 70.1(4) . . ? C17 C18 C19 107.2(7) . . ? C17 C18 Mo1 74.3(4) . . ? C19 C18 Mo1 71.5(4) . . ? C20 C19 C18 107.2(7) . . ? C20 C19 Mo1 74.4(4) . . ? C18 C19 Mo1 72.1(4) . . ? C21 C20 C19 108.9(7) . . ? C21 C20 Mo1 73.9(4) . . ? C19 C20 Mo1 70.1(4) . . ? C20 C21 C17 108.4(7) . . ? C20 C21 Mo1 71.7(4) . . ? C17 C21 Mo1 71.9(4) . . ? C23 C22 C27 118.4(7) . . ? C23 C22 P1 120.1(5) . . ? C27 C22 P1 121.6(5) . . ? C22 C23 C24 121.0(7) . . ? C23 C24 C25 120.2(7) . . ? C26 C25 C24 119.2(7) . . ? C25 C26 C27 120.6(7) . . ? C26 C27 C22 120.6(7) . . ? C29 C28 C33 118.3(6) . . ? C29 C28 P1 120.5(5) . . ? C33 C28 P1 121.1(5) . . ? C28 C29 C30 120.6(7) . . ? C31 C30 C29 120.3(7) . . ? C30 C31 C32 119.4(7) . . ? C31 C32 C33 120.5(7) . . ? C32 C33 C28 120.9(7) . . ? C39 C34 C35 118.7(6) . . ? C39 C34 P2 119.3(5) . . ? C35 C34 P2 121.9(5) . . ? C36 C35 C34 120.2(7) . . ? C35 C36 C37 119.9(7) . . ? C38 C37 C36 119.9(7) . . ? C37 C38 C39 120.3(7) . . ? C38 C39 C34 120.9(7) . . ? C45 C40 C41 118.0(6) . . ? C45 C40 P2 119.8(4) . . ? C41 C40 P2 122.2(5) . . ? C42 C41 C40 120.9(7) . . ? C43 C42 C41 120.6(7) . . ? C42 C43 C44 118.7(7) . . ? C45 C44 C43 120.9(7) . . ? C44 C45 C40 120.9(6) . . ? Cl1 C46 Cl2 113.6(3) . . ? _refine_diff_density_max 0.881 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.118 data_mm9809 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33.50 H37.50 Cl Co0.50 Mo0.50 O P1.50' _chemical_formula_weight 615.48 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 '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' 'P' 'P' 0.1023 0.0942 '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' '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.460(5) _cell_length_b 18.534(5) _cell_length_c 11.506(5) _cell_angle_alpha 103.78(3) _cell_angle_beta 91.12(3) _cell_angle_gamma 76.21(3) _cell_volume 3107.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method ? _exptl_crystal_F_000 1282 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Poor crystal, poor data. ; _diffrn_ambient_temperature 180(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 RAXIS-IIC _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19369 _diffrn_reflns_av_R_equivalents 0.1227 _diffrn_reflns_av_sigmaI/netI 0.2132 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.18 _reflns_number_total 10516 _reflns_number_observed 4972 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 34 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1737P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10482 _refine_ls_number_parameters 644 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1962 _refine_ls_R_factor_obs 0.1044 _refine_ls_wR_factor_all 0.3402 _refine_ls_wR_factor_obs 0.2871 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.338 _refine_ls_restrained_S_all 1.086 _refine_ls_restrained_S_obs 1.345 _refine_ls_shift/esd_max -10.615 _refine_ls_shift/esd_mean 0.164 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.03616(7) 0.28095(6) 0.84270(8) 0.0258(3) Uani 1 d . . Co1 Co 0.18056(11) 0.19930(8) 0.72011(13) 0.0261(4) Uani 1 d . . P1 P 0.1153(2) 0.1499(2) 0.8405(3) 0.0275(7) Uani 1 d . . P2 P 0.1123(2) 0.3119(2) 0.6876(3) 0.0282(7) Uani 1 d . . P3 P 0.3202(2) 0.1965(2) 0.7420(3) 0.0295(7) Uani 1 d . . O1 O -0.0464(6) 0.1894(5) 0.6207(8) 0.045(2) Uani 1 d . . C1 C -0.0162(9) 0.2228(7) 0.6998(11) 0.034(3) Uani 1 d . . C2 C 0.1857(9) 0.1364(7) 0.5785(11) 0.038(3) Uani 1 d . . O2 O 0.1965(7) 0.0949(5) 0.4851(7) 0.050(3) Uani 1 d . . C3 C -0.0436(9) 0.4089(7) 0.9134(12) 0.044(4) Uani 1 d . . H3 H -0.0311(9) 0.4493(7) 0.8842(12) 0.052 Uiso 1 calc R . C4 C -0.0069(10) 0.3819(8) 1.0129(12) 0.048(4) Uani 1 d . . H4 H 0.0356(10) 0.4016(8) 1.0637(12) 0.058 Uiso 1 calc R . C5 C -0.0418(9) 0.3234(7) 1.0243(11) 0.040(3) Uani 1 d . . H5 H -0.0267(9) 0.2949(7) 1.0834(11) 0.048 Uiso 1 calc R . C6 C -0.1041(9) 0.3114(8) 0.9350(11) 0.042(3) Uani 1 d . . H6 H -0.1393(9) 0.2749(8) 0.9248(11) 0.051 Uiso 1 calc R . C7 C -0.1041(9) 0.3621(8) 0.8659(11) 0.041(3) Uani 1 d . . H7 H -0.1386(9) 0.3658(8) 0.7974(11) 0.050 Uiso 1 calc R . C8 C 0.0610(9) 0.0696(6) 0.7880(10) 0.031(3) Uani 1 d . . C9 C 0.0015(10) 0.0558(8) 0.8640(13) 0.047(4) Uani 1 d . . H9 H -0.0106(10) 0.0883(8) 0.9422(13) 0.056 Uiso 1 calc R . C10 C -0.0396(11) -0.0019(8) 0.8315(13) 0.055(4) Uani 1 d . . H10 H -0.0784(11) -0.0102(8) 0.8873(13) 0.066 Uiso 1 calc R . C11 C -0.0262(12) -0.0481(8) 0.7194(15) 0.061(5) Uani 1 d . . H11 H -0.0583(12) -0.0867(8) 0.6949(15) 0.073 Uiso 1 calc R . C12 C 0.0356(12) -0.0384(9) 0.6399(13) 0.063(5) Uani 1 d . . H12 H 0.0498(12) -0.0733(9) 0.5639(13) 0.076 Uiso 1 calc R . C13 C 0.0749(12) 0.0209(8) 0.6722(12) 0.055(4) Uani 1 d . . H13 H 0.1125(12) 0.0298(8) 0.6157(12) 0.066 Uiso 1 calc R . C14 C 0.1715(8) 0.1169(7) 0.9680(10) 0.031(3) Uani 1 d . . C15 C 0.2328(10) 0.0479(8) 0.9485(11) 0.045(4) Uani 1 d . . H15 H 0.2453(10) 0.0158(8) 0.8700(11) 0.054 Uiso 1 calc R . C16 C 0.2772(11) 0.0255(8) 1.0481(13) 0.056(4) Uani 1 d . . H16 H 0.3222(11) -0.0208(8) 1.0355(13) 0.067 Uiso 1 calc R . C17 C 0.2569(10) 0.0678(8) 1.1573(12) 0.048(4) Uani 1 d . . H17 H 0.2863(10) 0.0506(8) 1.2225(12) 0.057 Uiso 1 calc R . C18 C 0.1945(10) 0.1358(8) 1.1795(11) 0.043(3) Uani 1 d . . H18 H 0.1813(10) 0.1659(8) 1.2592(11) 0.052 Uiso 1 calc R . C19 C 0.1509(9) 0.1603(8) 1.0857(11) 0.040(3) Uani 1 d . . H19 H 0.1064(9) 0.2070(8) 1.1007(11) 0.048 Uiso 1 calc R . C20 C 0.0502(8) 0.3280(6) 0.5551(10) 0.028(3) Uani 1 d . . C21 C -0.0007(10) 0.3993(8) 0.5567(12) 0.045(4) Uani 1 d . . H21 H -0.0010(10) 0.4401(8) 0.6249(12) 0.054 Uiso 1 calc R . C22 C -0.0525(11) 0.4137(8) 0.4595(12) 0.053(4) Uani 1 d . . H22 H -0.0875(11) 0.4639(8) 0.4634(12) 0.063 Uiso 1 calc R . C23 C -0.0537(10) 0.3571(8) 0.3599(11) 0.048(4) Uani 1 d . . H23 H -0.0886(10) 0.3669(8) 0.2940(11) 0.057 Uiso 1 calc R . C24 C -0.0011(11) 0.2834(8) 0.3581(11) 0.052(4) Uani 1 d . . H24 H -0.0011(11) 0.2429(8) 0.2895(11) 0.063 Uiso 1 calc R . C25 C 0.0498(10) 0.2680(8) 0.4514(11) 0.044(3) Uani 1 d . . H25 H 0.0848(10) 0.2178(8) 0.4474(11) 0.052 Uiso 1 calc R . C26 C 0.1663(9) 0.3914(7) 0.7111(10) 0.032(3) Uani 1 d . . C27 C 0.2089(9) 0.4050(7) 0.6182(11) 0.038(3) Uani 1 d . . H27 H 0.2100(9) 0.3715(7) 0.5412(11) 0.046 Uiso 1 calc R . C28 C 0.2501(9) 0.4640(7) 0.6297(12) 0.041(3) Uani 1 d . . H28 H 0.2782(9) 0.4716(7) 0.5624(12) 0.049 Uiso 1 calc R . C29 C 0.2496(10) 0.5131(8) 0.7446(13) 0.046(4) Uani 1 d . . H29 H 0.2789(10) 0.5537(8) 0.7552(13) 0.056 Uiso 1 calc R . C30 C 0.2069(10) 0.5027(7) 0.8417(13) 0.049(4) Uani 1 d . . H30 H 0.2055(10) 0.5368(7) 0.9181(13) 0.059 Uiso 1 calc R . C31 C 0.1654(8) 0.4412(7) 0.8266(11) 0.032(3) Uani 1 d . . H31 H 0.1370(8) 0.4330(7) 0.8932(11) 0.038 Uiso 1 calc R . C32 C 0.3663(9) 0.2484(7) 0.6548(11) 0.035(3) Uani 1 d . . C33 C 0.3498(11) 0.2328(8) 0.5292(12) 0.053(4) Uani 1 d . . H33 H 0.3117(11) 0.1999(8) 0.4986(12) 0.064 Uiso 1 calc R . C34 C 0.3862(13) 0.2631(11) 0.4540(15) 0.072(5) Uani 1 d . . H34 H 0.3748(13) 0.2507(11) 0.3711(15) 0.087 Uiso 1 calc R . C35 C 0.4422(14) 0.3139(12) 0.4973(19) 0.080(6) Uani 1 d . . H35 H 0.4712(14) 0.3332(12) 0.4437(19) 0.096 Uiso 1 calc R . C36 C 0.4530(16) 0.3336(12) 0.6162(21) 0.093(7) Uani 1 d . . H36 H 0.4845(16) 0.3715(12) 0.6487(21) 0.112 Uiso 1 calc R . C37 C 0.4176(12) 0.2981(12) 0.6910(15) 0.072(5) Uani 1 d . . H37 H 0.4306(12) 0.3098(12) 0.7735(15) 0.087 Uiso 1 calc R . C38 C 0.4020(9) 0.1046(7) 0.6984(9) 0.037(3) Uani 1 d . . C39 C 0.4897(9) 0.1001(8) 0.6747(10) 0.041(3) Uani 1 d . . H39 H 0.5093(9) 0.1453(8) 0.6773(10) 0.049 Uiso 1 calc R . C40 C 0.5515(11) 0.0273(9) 0.6460(12) 0.055(4) Uani 1 d . . H40 H 0.6128(11) 0.0241(9) 0.6313(12) 0.066 Uiso 1 calc R . C41 C 0.5229(11) -0.0380(10) 0.6394(12) 0.057(5) Uani 1 d . . H41 H 0.5648(11) -0.0862(10) 0.6230(12) 0.068 Uiso 1 calc R . C42 C 0.4342(12) -0.0343(8) 0.6563(12) 0.053(4) Uani 1 d . . H42 H 0.4144(12) -0.0801(8) 0.6463(12) 0.063 Uiso 1 calc R . C43 C 0.3724(10) 0.0369(7) 0.6882(13) 0.049(4) Uani 1 d . . H43 H 0.3114(10) 0.0396(7) 0.7028(13) 0.058 Uiso 1 calc R . C44 C 0.5404(10) 0.1780(11) 0.9581(13) 0.066(5) Uani 1 d . . H44A H 0.5845(36) 0.2042(55) 0.9992(32) 0.099 Uiso 1 calc R . H44B H 0.5189(16) 0.1993(58) 0.8897(52) 0.099 Uiso 1 calc R . H44C H 0.5681(48) 0.1232(11) 0.9296(78) 0.099 Uiso 1 calc R . C45 C 0.4808(12) 0.1270(10) 1.1131(14) 0.066(5) Uani 1 d . . H45A H 0.5427(24) 0.1181(46) 1.1375(88) 0.099 Uiso 1 calc R . H45B H 0.4704(73) 0.0796(21) 1.0620(37) 0.099 Uiso 1 calc R . H45C H 0.4407(53) 0.1433(30) 1.1843(56) 0.099 Uiso 1 calc R . C46 C 0.4541(12) 0.2684(9) 1.1311(13) 0.063(5) Uani 1 d . . H46A H 0.5042(43) 0.2662(20) 1.1848(71) 0.094 Uiso 1 calc R . H46B H 0.3980(38) 0.2827(31) 1.1785(74) 0.094 Uiso 1 calc R . H46C H 0.4545(79) 0.3066(16) 1.0852(14) 0.094 Uiso 1 calc R . C47 C 0.4629(9) 0.1890(8) 1.0440(12) 0.043(3) Uani 1 d . . C48 C 0.3727(9) 0.1838(7) 0.9810(11) 0.040(3) Uani 1 d . . H48A H 0.3806(9) 0.1313(7) 0.9299(11) 0.048 Uiso 1 calc R . H48B H 0.3268(9) 0.1904(7) 1.0440(11) 0.048 Uiso 1 calc R . C49 C 0.3353(8) 0.2412(7) 0.9024(10) 0.033(3) Uani 1 d . . H49 H 0.3752(8) 0.2769(7) 0.9064(10) 0.039 Uiso 1 calc R . C50 C 0.2422(8) 0.2871(6) 0.9444(9) 0.027(3) Uani 1 d . . C51 C 0.1725(8) 0.2716(6) 0.8794(11) 0.032(3) Uani 1 d . . C52 C 0.2344(9) 0.3471(7) 1.0573(10) 0.032(3) Uani 1 d . . C53 C 0.2791(9) 0.4064(7) 1.0685(11) 0.037(3) Uani 1 d . . H53 H 0.3147(9) 0.4077(7) 1.0030(11) 0.044 Uiso 1 calc R . C54 C 0.2717(11) 0.4621(8) 1.1727(13) 0.054(4) Uani 1 d . . H54 H 0.3023(11) 0.5015(8) 1.1788(13) 0.064 Uiso 1 calc R . C55 C 0.2202(11) 0.4616(9) 1.2690(11) 0.055(4) Uani 1 d . . H55 H 0.2152(11) 0.5008(9) 1.3406(11) 0.066 Uiso 1 calc R . C56 C 0.1767(10) 0.4052(8) 1.2616(10) 0.044(4) Uani 1 d . . H56 H 0.1417(10) 0.4051(8) 1.3285(10) 0.053 Uiso 1 calc R . C57 C 0.1826(9) 0.3476(8) 1.1580(10) 0.041(3) Uani 1 d . . H57 H 0.1519(9) 0.3084(8) 1.1544(10) 0.050 Uiso 1 calc R . C58 C 0.7955(15) 0.0979(13) 0.6654(18) 0.096(7) Uani 1 d . . H58A H 0.8078(15) 0.0430(13) 0.6658(18) 0.116 Uiso 1 calc R . H58B H 0.8537(15) 0.1106(13) 0.6593(18) 0.116 Uiso 1 calc R . Cl1 Cl 0.7381(5) 0.1110(4) 0.5422(6) 0.122(2) Uani 1 d . . Cl2 Cl 0.7439(5) 0.1499(5) 0.7969(6) 0.137(3) Uani 1 d . . C59 C 0.6458(18) 0.3448(14) 0.9834(25) 0.140(4) Uiso 1 d D . H59A H 0.6992(44) 0.3338(95) 0.9315(117) 0.211 Uiso 1 calc R . H59B H 0.6283(57) 0.2971(49) 0.9815(181) 0.211 Uiso 1 calc R . H59C H 0.6586(97) 0.3682(53) 1.0656(73) 0.211 Uiso 1 calc R . C60 C 0.5649(19) 0.4035(15) 0.9359(23) 0.140(4) Uiso 1 d D . H60A H 0.5843(19) 0.4154(15) 0.8626(23) 0.168 Uiso 1 calc R . H60B H 0.5129(19) 0.3809(15) 0.9177(23) 0.168 Uiso 1 calc R . C61 C 0.5397(19) 0.4796(14) 1.0427(23) 0.140(4) Uiso 1 d D . H61A H 0.5886(19) 0.5062(14) 1.0613(23) 0.211 Uiso 1 calc R . H61B H 0.5153(19) 0.4716(14) 1.1163(23) 0.211 Uiso 1 calc R . C62 C 0.7201(19) 0.3272(16) 0.6501(21) 0.140(4) Uiso 1 d D . H62A H 0.7484(99) 0.3591(102) 0.7121(28) 0.211 Uiso 1 calc R . H62B H 0.7295(127) 0.2760(19) 0.6650(83) 0.211 Uiso 1 calc R . H62C H 0.6560(32) 0.3505(113) 0.6520(65) 0.211 Uiso 1 calc R . C63 C 0.7632(17) 0.3206(17) 0.5211(20) 0.140(4) Uiso 1 d D . H63A H 0.8077(17) 0.3520(17) 0.5317(20) 0.168 Uiso 1 calc R . H63B H 0.7952(17) 0.2667(17) 0.4876(20) 0.168 Uiso 1 calc R . C64 C 0.6946(14) 0.3467(12) 0.4289(16) 0.140(4) Uiso 1 d D . H64A H 0.6339(14) 0.3534(12) 0.4623(16) 0.168 Uiso 1 calc R 1 H64B H 0.7002(14) 0.3974(12) 0.4207(16) 0.168 Uiso 1 calc R 1 C65 C 0.7037(14) 0.2920(12) 0.3015(16) 0.140(4) Uiso 0.48(2) d PRD 1 H65A H 0.7116(14) 0.3222(12) 0.2439(16) 0.168 Uiso 0.48(2) calc PR 1 H65B H 0.6458(14) 0.2783(12) 0.2855(16) 0.168 Uiso 0.48(2) calc PR 1 C66 C 0.7790(32) 0.2144(21) 0.2685(37) 0.140(4) Uiso 0.48(2) d PD 1 H66A H 0.7575(32) 0.1725(21) 0.2886(37) 0.168 Uiso 0.48(2) calc PR 1 H66B H 0.8328(32) 0.2203(21) 0.3145(37) 0.168 Uiso 0.48(2) calc PR 1 C67 C 0.8062(32) 0.1919(29) 0.1060(42) 0.140(4) Uiso 0.48(2) d PD 1 H67A H 0.7752(241) 0.2349(109) 0.0731(88) 0.211 Uiso 0.48(2) calc PR 1 H67B H 0.7872(300) 0.1457(79) 0.0659(84) 0.211 Uiso 0.48(2) calc PR 1 H67C H 0.8707(93) 0.1833(260) 0.0929(43) 0.211 Uiso 0.48(2) calc PR 1 C68 C 0.7037(14) 0.2920(12) 0.3015(16) 0.140(4) Uiso 0.52(2) d P 2 H68A H 0.7671(28) 0.2649(20) 0.2831(42) 0.168 Uiso 0.52(2) calc PR 2 H68B H 0.6847(28) 0.3226(20) 0.2418(42) 0.168 Uiso 0.52(2) calc PR 2 C69 C 0.6442(28) 0.2291(20) 0.2899(42) 0.140(4) Uiso 0.52(2) d PD 2 H69A H 0.5924(28) 0.2410(20) 0.2397(42) 0.168 Uiso 0.52(2) calc PR 2 H69B H 0.6220(28) 0.2288(20) 0.3699(42) 0.168 Uiso 0.52(2) calc PR 2 C70 C 0.7088(35) 0.1477(19) 0.2286(50) 0.140(4) Uiso 0.52(2) d PD 2 H70A H 0.7108(231) 0.1124(78) 0.2804(189) 0.211 Uiso 0.52(2) calc PR 2 H70B H 0.7689(66) 0.1541(49) 0.2172(360) 0.211 Uiso 0.52(2) calc PR 2 H70C H 0.6862(165) 0.1268(116) 0.1508(177) 0.211 Uiso 0.52(2) calc PR 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 0.0300(6) 0.0229(5) 0.0211(5) 0.0036(4) -0.0018(4) -0.0019(4) Co1 0.0337(10) 0.0206(8) 0.0209(8) 0.0038(6) -0.0014(7) -0.0015(7) P1 0.031(2) 0.0226(14) 0.0266(15) 0.0061(12) -0.0010(13) -0.0012(13) P2 0.035(2) 0.0243(15) 0.0225(14) 0.0050(13) -0.0027(13) -0.0026(13) P3 0.032(2) 0.031(2) 0.0216(14) 0.0056(13) 0.0003(13) -0.0008(13) O1 0.050(6) 0.048(5) 0.035(5) 0.000(4) -0.015(4) -0.017(5) C1 0.040(8) 0.032(6) 0.034(7) 0.012(6) 0.005(6) -0.013(6) C2 0.049(9) 0.029(6) 0.037(7) 0.017(6) -0.001(6) -0.004(6) O2 0.080(8) 0.039(5) 0.023(4) -0.003(4) -0.003(5) -0.009(5) C3 0.043(8) 0.031(7) 0.041(7) -0.009(6) 0.013(6) 0.005(6) C4 0.056(9) 0.037(7) 0.034(7) -0.011(6) -0.007(7) 0.002(7) C5 0.046(8) 0.039(7) 0.024(6) 0.007(6) 0.003(6) 0.009(6) C6 0.047(9) 0.039(7) 0.031(7) -0.002(6) 0.011(6) -0.001(6) C7 0.036(8) 0.047(8) 0.028(6) 0.000(6) -0.005(6) 0.007(6) C8 0.044(8) 0.024(6) 0.023(6) 0.007(5) -0.004(5) -0.005(5) C9 0.049(9) 0.044(8) 0.049(8) 0.011(7) 0.001(7) -0.013(7) C10 0.064(11) 0.056(9) 0.049(8) 0.003(8) 0.011(8) -0.029(8) C11 0.078(12) 0.028(7) 0.076(11) 0.013(8) -0.012(9) -0.013(8) C12 0.086(13) 0.062(10) 0.042(8) -0.015(8) 0.005(8) -0.047(9) C13 0.089(12) 0.046(8) 0.039(8) 0.007(7) 0.011(8) -0.034(8) C14 0.033(7) 0.032(6) 0.026(6) 0.008(5) -0.001(5) -0.003(5) C15 0.055(9) 0.043(8) 0.030(7) 0.012(6) -0.001(6) 0.004(7) C16 0.058(10) 0.045(8) 0.056(9) 0.018(7) 0.001(8) 0.007(7) C17 0.051(9) 0.056(9) 0.041(8) 0.034(7) -0.012(7) -0.002(7) C18 0.050(9) 0.060(9) 0.023(6) 0.012(6) -0.013(6) -0.020(7) C19 0.036(8) 0.049(8) 0.036(7) 0.009(6) -0.003(6) -0.010(6) C20 0.025(6) 0.022(6) 0.027(6) -0.002(5) 0.003(5) 0.002(5) C21 0.058(9) 0.039(7) 0.033(7) 0.009(6) -0.010(6) -0.003(7) C22 0.064(10) 0.042(8) 0.047(8) 0.011(7) -0.021(7) -0.003(7) C23 0.057(10) 0.052(9) 0.027(7) 0.014(6) -0.009(6) 0.002(7) C24 0.073(11) 0.045(8) 0.024(6) 0.003(6) -0.011(7) 0.010(7) C25 0.052(9) 0.041(7) 0.035(7) 0.010(6) -0.008(6) -0.005(7) C26 0.044(8) 0.032(6) 0.031(6) 0.014(5) -0.013(6) -0.022(6) C27 0.048(8) 0.029(6) 0.033(7) 0.000(6) 0.008(6) -0.008(6) C28 0.036(8) 0.040(7) 0.049(8) 0.015(6) 0.002(6) -0.011(6) C29 0.044(9) 0.036(7) 0.067(9) 0.017(7) -0.006(7) -0.019(6) C30 0.068(10) 0.023(6) 0.046(8) -0.002(6) -0.015(7) -0.002(7) C31 0.028(7) 0.035(6) 0.037(7) 0.011(6) -0.006(5) -0.013(5) C32 0.033(7) 0.038(7) 0.037(7) 0.015(6) 0.000(6) -0.009(6) C33 0.070(11) 0.042(8) 0.039(8) 0.008(7) 0.016(7) 0.003(7) C34 0.081(14) 0.098(14) 0.049(10) 0.036(10) 0.017(9) -0.022(11) C35 0.085(15) 0.093(14) 0.084(14) 0.060(12) 0.004(12) -0.023(12) C36 0.113(19) 0.085(14) 0.118(17) 0.061(13) -0.021(15) -0.061(13) C37 0.072(12) 0.117(15) 0.051(9) 0.041(10) -0.009(9) -0.047(12) C38 0.055(9) 0.036(7) 0.013(5) 0.007(5) -0.002(5) 0.002(6) C39 0.036(8) 0.056(8) 0.025(6) 0.003(6) -0.002(5) -0.004(6) C40 0.054(10) 0.062(10) 0.033(7) 0.014(7) -0.012(7) 0.017(8) C41 0.052(10) 0.064(10) 0.035(8) 0.014(7) -0.001(7) 0.025(8) C42 0.080(12) 0.028(7) 0.046(8) 0.015(6) -0.007(8) 0.000(7) C43 0.044(9) 0.036(7) 0.057(9) 0.011(7) 0.010(7) 0.006(6) C44 0.045(10) 0.104(14) 0.047(9) 0.032(9) 0.001(7) -0.001(9) C45 0.061(11) 0.079(11) 0.066(10) 0.043(9) -0.016(8) -0.007(9) C46 0.069(11) 0.079(12) 0.038(8) 0.003(8) -0.013(8) -0.023(9) C47 0.042(8) 0.049(8) 0.040(7) 0.012(6) -0.001(6) -0.011(6) C48 0.040(8) 0.037(7) 0.037(7) 0.007(6) -0.015(6) 0.000(6) C49 0.032(7) 0.034(6) 0.031(6) 0.006(5) -0.009(5) -0.009(5) C50 0.028(7) 0.033(6) 0.022(5) 0.010(5) 0.000(5) -0.010(5) C51 0.037(7) 0.017(5) 0.036(7) -0.004(5) 0.008(6) -0.005(5) C52 0.041(8) 0.029(6) 0.027(6) 0.008(5) -0.009(5) -0.010(6) C53 0.034(7) 0.032(7) 0.038(7) 0.002(6) -0.010(6) -0.003(6) C54 0.059(10) 0.041(8) 0.053(9) -0.008(7) -0.010(8) -0.017(7) C55 0.078(12) 0.058(9) 0.022(7) -0.001(7) -0.014(7) -0.017(9) C56 0.057(9) 0.048(8) 0.021(6) 0.001(6) 0.001(6) -0.005(7) C57 0.044(8) 0.057(8) 0.023(6) 0.009(6) -0.002(6) -0.012(7) C58 0.088(16) 0.101(15) 0.098(15) 0.008(13) -0.023(13) -0.037(13) Cl1 0.146(6) 0.110(5) 0.104(4) 0.021(4) -0.019(4) -0.025(4) Cl2 0.138(6) 0.159(7) 0.091(4) 0.010(4) 0.027(4) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C1 2.010(13) . ? Mo1 C51 2.116(13) . ? Mo1 C5 2.302(12) . ? Mo1 C7 2.305(12) . ? Mo1 C6 2.317(13) . ? Mo1 C4 2.343(12) . ? Mo1 C3 2.352(12) . ? Mo1 P2 2.406(4) . ? Mo1 P1 2.439(3) . ? Mo1 Co1 2.600(2) . ? Co1 C2 1.754(13) . ? Co1 C51 1.982(11) . ? Co1 P3 2.158(4) . ? Co1 P1 2.208(4) . ? Co1 P2 2.218(3) . ? P1 C14 1.845(12) . ? P1 C8 1.853(12) . ? P2 C26 1.824(12) . ? P2 C20 1.832(12) . ? P3 C32 1.804(13) . ? P3 C38 1.828(12) . ? P3 C49 1.869(11) . ? O1 C1 1.133(14) . ? C2 O2 1.151(14) . ? C3 C4 1.41(2) . ? C3 C7 1.44(2) . ? C4 C5 1.35(2) . ? C5 C6 1.41(2) . ? C6 C7 1.37(2) . ? C8 C9 1.39(2) . ? C8 C13 1.41(2) . ? C9 C10 1.35(2) . ? C10 C11 1.36(2) . ? C11 C12 1.41(2) . ? C12 C13 1.35(2) . ? C14 C15 1.37(2) . ? C14 C19 1.40(2) . ? C15 C16 1.42(2) . ? C16 C17 1.31(2) . ? C17 C18 1.36(2) . ? C18 C19 1.37(2) . ? C20 C21 1.36(2) . ? C20 C25 1.42(2) . ? C21 C22 1.40(2) . ? C22 C23 1.36(2) . ? C23 C24 1.41(2) . ? C24 C25 1.36(2) . ? C26 C27 1.37(2) . ? C26 C31 1.42(2) . ? C27 C28 1.37(2) . ? C28 C29 1.41(2) . ? C29 C30 1.38(2) . ? C30 C31 1.41(2) . ? C32 C37 1.34(2) . ? C32 C33 1.43(2) . ? C33 C34 1.33(2) . ? C34 C35 1.43(3) . ? C35 C36 1.35(3) . ? C36 C37 1.39(2) . ? C38 C39 1.37(2) . ? C38 C43 1.41(2) . ? C39 C40 1.42(2) . ? C40 C41 1.37(2) . ? C41 C42 1.37(2) . ? C42 C43 1.40(2) . ? C44 C47 1.51(2) . ? C45 C47 1.52(2) . ? C46 C47 1.55(2) . ? C47 C48 1.57(2) . ? C48 C49 1.56(2) . ? C49 C50 1.51(2) . ? C50 C51 1.35(2) . ? C50 C52 1.480(15) . ? C52 C53 1.41(2) . ? C52 C57 1.42(2) . ? C53 C54 1.37(2) . ? C54 C55 1.38(2) . ? C55 C56 1.36(2) . ? C56 C57 1.39(2) . ? C58 Cl2 1.69(2) . ? C58 Cl1 1.69(2) . ? C59 C60 1.63(2) . ? C60 C61 1.61(2) . ? C61 C61 1.71(5) 2_667 ? C61 C61 45.07(6) 2_545 ? C62 C63 1.60(2) . ? C63 C64 1.56(2) . ? C64 C68 1.56 . ? C64 C65 1.56 . ? C65 C66 1.59(3) . ? C66 C67 1.85(4) . ? C68 C69 1.63(3) . ? C69 C70 1.60(3) . ? 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 C1 Mo1 C51 127.8(5) . . ? C1 Mo1 C5 120.0(5) . . ? C51 Mo1 C5 106.9(5) . . ? C1 Mo1 C7 83.1(5) . . ? C51 Mo1 C7 145.2(4) . . ? C5 Mo1 C7 58.0(5) . . ? C1 Mo1 C6 86.5(5) . . ? C51 Mo1 C6 142.4(5) . . ? C5 Mo1 C6 35.5(5) . . ? C7 Mo1 C6 34.5(5) . . ? C1 Mo1 C4 140.7(5) . . ? C51 Mo1 C4 91.3(5) . . ? C5 Mo1 C4 33.9(5) . . ? C7 Mo1 C4 58.3(5) . . ? C6 Mo1 C4 57.9(5) . . ? C1 Mo1 C3 114.0(5) . . ? C51 Mo1 C3 109.4(5) . . ? C5 Mo1 C3 57.9(5) . . ? C7 Mo1 C3 35.9(5) . . ? C6 Mo1 C3 58.6(5) . . ? C4 Mo1 C3 35.0(5) . . ? C1 Mo1 P2 81.3(4) . . ? C51 Mo1 P2 69.3(4) . . ? C5 Mo1 P2 147.6(4) . . ? C7 Mo1 P2 105.9(4) . . ? C6 Mo1 P2 139.9(4) . . ? C4 Mo1 P2 114.2(4) . . ? C3 Mo1 P2 92.1(4) . . ? C1 Mo1 P1 79.4(4) . . ? C51 Mo1 P1 67.8(3) . . ? C5 Mo1 P1 103.9(3) . . ? C7 Mo1 P1 142.5(4) . . ? C6 Mo1 P1 111.1(4) . . ? C4 Mo1 P1 126.2(4) . . ? C3 Mo1 P1 160.8(4) . . ? P2 Mo1 P1 103.90(11) . . ? C1 Mo1 Co1 79.4(4) . . ? C51 Mo1 Co1 48.4(3) . . ? C5 Mo1 Co1 148.1(3) . . ? C7 Mo1 Co1 153.9(3) . . ? C6 Mo1 Co1 159.5(4) . . ? C4 Mo1 Co1 139.2(4) . . ? C3 Mo1 Co1 141.2(4) . . ? P2 Mo1 Co1 52.41(8) . . ? P1 Mo1 Co1 51.86(9) . . ? C2 Co1 C51 178.8(6) . . ? C2 Co1 P3 100.0(5) . . ? C51 Co1 P3 80.9(4) . . ? C2 Co1 P1 105.2(4) . . ? C51 Co1 P1 74.9(4) . . ? P3 Co1 P1 117.80(14) . . ? C2 Co1 P2 103.4(4) . . ? C51 Co1 P2 75.6(4) . . ? P3 Co1 P2 108.32(14) . . ? P1 Co1 P2 119.13(13) . . ? C2 Co1 Mo1 126.1(5) . . ? C51 Co1 Mo1 52.9(4) . . ? P3 Co1 Mo1 133.45(10) . . ? P1 Co1 Mo1 60.32(9) . . ? P2 Co1 Mo1 59.30(10) . . ? C14 P1 C8 97.1(5) . . ? C14 P1 Co1 122.7(4) . . ? C8 P1 Co1 123.9(4) . . ? C14 P1 Mo1 125.9(4) . . ? C8 P1 Mo1 120.8(4) . . ? Co1 P1 Mo1 67.81(10) . . ? C26 P2 C20 98.7(6) . . ? C26 P2 Co1 122.0(4) . . ? C20 P2 Co1 126.2(4) . . ? C26 P2 Mo1 124.5(4) . . ? C20 P2 Mo1 117.7(4) . . ? Co1 P2 Mo1 68.28(11) . . ? C32 P3 C38 98.6(6) . . ? C32 P3 C49 106.2(6) . . ? C38 P3 C49 108.5(5) . . ? C32 P3 Co1 115.7(4) . . ? C38 P3 Co1 119.0(5) . . ? C49 P3 Co1 107.9(4) . . ? O1 C1 Mo1 178.6(11) . . ? O2 C2 Co1 174.4(13) . . ? C4 C3 C7 105.2(13) . . ? C4 C3 Mo1 72.1(7) . . ? C7 C3 Mo1 70.2(7) . . ? C5 C4 C3 109.0(13) . . ? C5 C4 Mo1 71.4(7) . . ? C3 C4 Mo1 72.8(7) . . ? C4 C5 C6 109.6(12) . . ? C4 C5 Mo1 74.7(8) . . ? C6 C5 Mo1 72.8(7) . . ? C7 C6 C5 107.0(13) . . ? C7 C6 Mo1 72.3(8) . . ? C5 C6 Mo1 71.7(8) . . ? C6 C7 C3 109.2(12) . . ? C6 C7 Mo1 73.3(8) . . ? C3 C7 Mo1 73.8(7) . . ? C9 C8 C13 116.4(12) . . ? C9 C8 P1 119.8(9) . . ? C13 C8 P1 123.8(10) . . ? C10 C9 C8 122.7(13) . . ? C9 C10 C11 120.5(15) . . ? C10 C11 C12 119.2(15) . . ? C13 C12 C11 119.7(14) . . ? C12 C13 C8 121.3(14) . . ? C15 C14 C19 118.9(12) . . ? C15 C14 P1 120.0(9) . . ? C19 C14 P1 121.1(9) . . ? C14 C15 C16 118.6(12) . . ? C17 C16 C15 121.0(13) . . ? C16 C17 C18 121.6(13) . . ? C17 C18 C19 119.4(12) . . ? C18 C19 C14 120.5(12) . . ? C21 C20 C25 118.2(11) . . ? C21 C20 P2 119.2(9) . . ? C25 C20 P2 122.6(9) . . ? C20 C21 C22 121.3(12) . . ? C23 C22 C21 121.3(13) . . ? C22 C23 C24 117.5(12) . . ? C25 C24 C23 122.2(12) . . ? C24 C25 C20 119.5(12) . . ? C27 C26 C31 118.0(11) . . ? C27 C26 P2 121.0(9) . . ? C31 C26 P2 121.0(9) . . ? C26 C27 C28 123.8(12) . . ? C27 C28 C29 118.1(13) . . ? C30 C29 C28 120.7(13) . . ? C29 C30 C31 119.7(12) . . ? C30 C31 C26 119.7(12) . . ? C37 C32 C33 114.9(13) . . ? C37 C32 P3 128.4(11) . . ? C33 C32 P3 116.6(11) . . ? C34 C33 C32 122.1(17) . . ? C33 C34 C35 120.4(17) . . ? C36 C35 C34 118.2(18) . . ? C35 C36 C37 119.5(19) . . ? C32 C37 C36 124.5(17) . . ? C39 C38 C43 119.9(12) . . ? C39 C38 P3 121.8(11) . . ? C43 C38 P3 118.3(11) . . ? C38 C39 C40 119.7(15) . . ? C41 C40 C39 120.1(15) . . ? C42 C41 C40 120.5(14) . . ? C41 C42 C43 120.2(15) . . ? C42 C43 C38 119.4(14) . . ? C45 C47 C44 110.6(13) . . ? C45 C47 C46 110.0(12) . . ? C44 C47 C46 106.3(13) . . ? C45 C47 C48 105.3(12) . . ? C44 C47 C48 113.9(12) . . ? C46 C47 C48 110.7(11) . . ? C49 C48 C47 118.0(12) . . ? C50 C49 C48 111.5(10) . . ? C50 C49 P3 102.4(8) . . ? C48 C49 P3 115.2(8) . . ? C51 C50 C52 124.4(11) . . ? C51 C50 C49 119.4(10) . . ? C52 C50 C49 116.2(10) . . ? C50 C51 Co1 125.6(9) . . ? C50 C51 Mo1 155.7(9) . . ? Co1 C51 Mo1 78.7(4) . . ? C53 C52 C57 117.3(11) . . ? C53 C52 C50 120.6(11) . . ? C57 C52 C50 122.0(11) . . ? C54 C53 C52 120.7(13) . . ? C53 C54 C55 120.8(15) . . ? C56 C55 C54 120.1(12) . . ? C55 C56 C57 121.1(13) . . ? C56 C57 C52 120.0(13) . . ? Cl2 C58 Cl1 115.1(13) . . ? C61 C60 C59 106.0(17) . . ? C60 C61 C61 89.7(21) . 2_667 ? C60 C61 C61 37.4(16) . 2_545 ? C61 C61 C61 75.5(18) 2_667 2_545 ? C64 C63 C62 114.5(18) . . ? C68 C64 C63 116.2(11) . . ? C65 C64 C63 116.2(11) . . ? C64 C65 C66 121.4(18) . . ? C65 C66 C67 108.0(23) . . ? C64 C68 C69 112.4(16) . . ? C68 C69 C70 106.2(23) . . ? _refine_diff_density_max 3.572 _refine_diff_density_min -1.633 _refine_diff_density_rms 0.181