# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1692 data_giles02 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H39 Co Mo O9 P2 S' _chemical_formula_weight 816.50 _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' 'S' 'S' 0.1246 0.1234 '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)/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 11.148(2) _cell_length_b 18.141(4) _cell_length_c 17.411(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.33(3) _cell_angle_gamma 90.00 _cell_volume 3511.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method ? _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4725 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4557 _reflns_number_observed 3568 _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 9 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^)+(0.0846P)^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 4548 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_obs 0.0410 _refine_ls_wR_factor_all 0.1455 _refine_ls_wR_factor_obs 0.1150 _refine_ls_goodness_of_fit_all 1.196 _refine_ls_goodness_of_fit_obs 1.108 _refine_ls_restrained_S_all 1.226 _refine_ls_restrained_S_obs 1.108 _refine_ls_shift/esd_max -0.005 _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 0.10343(5) 0.49342(3) 0.76661(3) 0.0295(2) Uani 1 d . . Co1 Co 0.04830(7) 0.34859(4) 0.78265(5) 0.0270(3) Uani 1 d . . P1 P -0.12857(15) 0.31216(9) 0.80858(10) 0.0332(4) Uani 1 d . . P2 P -0.00902(15) 0.41291(9) 0.67857(9) 0.0303(4) Uani 1 d . . S1 S 0.11040(14) 0.38468(9) 0.90880(9) 0.0334(4) Uani 1 d . . C1 C 0.2175(5) 0.4288(3) 0.8515(4) 0.0316(15) Uani 1 d . . C2 C 0.3133(6) 0.4750(4) 0.8910(4) 0.042(2) Uani 1 d . . C3 C 0.4962(8) 0.5385(5) 0.8764(5) 0.079(3) Uani 1 d . . H3A H 0.5392(8) 0.5580(5) 0.8352(5) 0.119 Uiso 1 d R . H3B H 0.5513(8) 0.5131(5) 0.9123(5) 0.119 Uiso 1 d R . H3C H 0.4589(8) 0.5781(5) 0.9023(5) 0.119 Uiso 1 d R . C4 C 0.2106(5) 0.3960(3) 0.7763(3) 0.0289(14) Uani 1 d . . C5 C 0.3091(6) 0.3598(4) 0.7401(4) 0.033(2) Uani 1 d . . C6 C 0.3689(7) 0.3136(4) 0.6208(5) 0.056(2) Uani 1 d . . H6A H 0.3368(7) 0.3095(4) 0.5682(5) 0.085 Uiso 1 d R . H6B H 0.3772(7) 0.2653(4) 0.6431(5) 0.085 Uiso 1 d R . H6C H 0.4463(7) 0.3371(4) 0.6225(5) 0.085 Uiso 1 d R . C7 C 0.2342(7) 0.5148(4) 0.7015(4) 0.041(2) Uani 1 d . . C8 C 0.0994(6) 0.2631(4) 0.7504(4) 0.037(2) Uani 1 d . . C9 C -0.2842(19) 0.3661(12) 0.9114(13) 0.069(6) Uani 0.50 d P 1 H9A H -0.2601(75) 0.3264(45) 0.9457(42) 0.103 Uiso 0.50 calc PR 1 H9B H -0.3653(25) 0.3581(74) 0.8905(14) 0.103 Uiso 0.50 calc PR 1 H9C H -0.2795(90) 0.4119(28) 0.9391(48) 0.103 Uiso 0.50 calc PR 1 C9' C -0.2101(18) 0.3768(14) 0.9315(12) 0.069(6) Uani 0.50 d P 2 H9'1 H -0.1556(89) 0.4154(49) 0.9486(15) 0.103 Uiso 0.50 calc PR 2 H9'2 H -0.1856(112) 0.3315(26) 0.9564(13) 0.103 Uiso 0.50 calc PR 2 H9'3 H -0.2899(31) 0.3892(71) 0.9442(14) 0.103 Uiso 0.50 calc PR 2 C10 C -0.3322(6) 0.2664(5) 0.7341(5) 0.069(3) Uani 1 d . . H10A H -0.3567(16) 0.2404(30) 0.6875(17) 0.103 Uiso 1 calc R . H10B H -0.3802(8) 0.3101(6) 0.7375(35) 0.103 Uiso 1 calc R . H10C H -0.3429(11) 0.2352(27) 0.7776(20) 0.103 Uiso 1 calc R . C11 C -0.1032(8) 0.1707(4) 0.8457(6) 0.074(3) Uani 1 d . . H11A H -0.1393(47) 0.1355(5) 0.8781(25) 0.112 Uiso 1 calc R . H11B H -0.0172(9) 0.1661(11) 0.8522(35) 0.112 Uiso 1 calc R . H11C H -0.1301(50) 0.1615(13) 0.7929(12) 0.112 Uiso 1 calc R . C12 C 0.1886(6) 0.3092(4) 0.9698(4) 0.045(2) Uani 1 d . . C13 C 0.0866(7) 0.2739(5) 1.0105(5) 0.065(2) Uani 1 d . . H13A H 0.0507(33) 0.3100(9) 1.0418(25) 0.097 Uiso 1 calc R . H13B H 0.1178(11) 0.2341(20) 1.0424(25) 0.097 Uiso 1 calc R . H13C H 0.0269(26) 0.2552(28) 0.9728(5) 0.097 Uiso 1 calc R . C14 C 0.2516(7) 0.2537(4) 0.9216(4) 0.058(2) Uani 1 d . . H14A H 0.2989(39) 0.2210(19) 0.9549(4) 0.088 Uiso 1 calc R . H14B H 0.3030(37) 0.2793(5) 0.8887(23) 0.088 Uiso 1 calc R . H14C H 0.1927(7) 0.2259(20) 0.8907(23) 0.088 Uiso 1 calc R . C15 C 0.2767(8) 0.3454(4) 1.0297(5) 0.061(2) Uani 1 d . . H15A H 0.3057(39) 0.3093(8) 1.0669(19) 0.092 Uiso 1 calc R . H15B H 0.2366(15) 0.3842(21) 1.0552(23) 0.092 Uiso 1 calc R . H15C H 0.3432(26) 0.3656(27) 1.0047(6) 0.092 Uiso 1 calc R . O2 O 0.3107(5) 0.5015(3) 0.9554(3) 0.0567(14) Uani 1 d . . O3 O 0.4036(4) 0.4869(3) 0.8451(3) 0.0559(14) Uani 1 d . . O5 O 0.3957(4) 0.3331(3) 0.7728(3) 0.0597(15) Uani 1 d . . O6 O 0.2884(4) 0.3570(3) 0.6636(3) 0.0462(12) Uani 1 d . . O7 O 0.3112(5) 0.5322(3) 0.6646(3) 0.067(2) Uani 1 d . . O8 O 0.1343(5) 0.2098(3) 0.7247(3) 0.065(2) Uani 1 d . . O9 O -0.2087(5) 0.3686(3) 0.8522(3) 0.0595(15) Uani 1 d . . O10 O -0.2081(4) 0.2865(3) 0.7335(3) 0.0433(12) Uani 1 d . . O11 O -0.1375(4) 0.2435(3) 0.8666(3) 0.0498(13) Uani 1 d . . C21 C -0.1683(5) 0.4307(3) 0.6448(4) 0.033(2) Uani 1 d . . C22 C -0.2493(6) 0.4564(4) 0.6954(4) 0.042(2) Uani 1 d . . H22 H -0.2235(6) 0.4639(4) 0.7468(4) 0.062 Uiso 1 d R . C23 C -0.3682(7) 0.4710(4) 0.6705(5) 0.052(2) Uani 1 d . . H23 H -0.4221(7) 0.4868(4) 0.7052(5) 0.078 Uiso 1 d R . C24 C -0.4056(7) 0.4618(4) 0.5937(5) 0.055(2) Uani 1 d . . H24 H -0.4845(7) 0.4725(4) 0.5761(5) 0.082 Uiso 1 d R . C25 C -0.3263(7) 0.4367(4) 0.5437(5) 0.052(2) Uani 1 d . . H25 H -0.3517(7) 0.4305(4) 0.4920(5) 0.079 Uiso 1 d R . C26 C -0.2097(6) 0.4208(4) 0.5686(4) 0.041(2) Uani 1 d . . H26 H -0.1575(6) 0.4029(4) 0.5337(4) 0.061 Uiso 1 d R . C31 C 0.0431(6) 0.3758(4) 0.5902(4) 0.035(2) Uani 1 d . . C32 C 0.1006(6) 0.4214(4) 0.5395(4) 0.045(2) Uani 1 d . . H32 H 0.1159(6) 0.4704(4) 0.5526(4) 0.067 Uiso 1 d R . C33 C 0.1356(8) 0.3939(5) 0.4696(5) 0.062(2) Uani 1 d . . H33 H 0.1728(8) 0.4247(5) 0.4359(5) 0.094 Uiso 1 d R . C34 C 0.1144(7) 0.3209(5) 0.4507(4) 0.060(2) Uani 1 d . . H34 H 0.1383(7) 0.3023(5) 0.4045(4) 0.090 Uiso 1 d R . C35 C 0.0572(7) 0.2750(5) 0.5003(5) 0.058(2) Uani 1 d . . H35 H 0.0427(7) 0.2259(5) 0.4872(5) 0.087 Uiso 1 d R . C36 C 0.0216(6) 0.3027(4) 0.5703(4) 0.042(2) Uani 1 d . . H36 H -0.0165(6) 0.2719(4) 0.6036(4) 0.062 Uiso 1 d R . C41 C 0.0607(7) 0.5673(4) 0.8700(5) 0.053(2) Uani 1 d . . H41 H 0.0854(7) 0.5523(4) 0.9198(5) 0.079 Uiso 1 d R . C42 C -0.0533(7) 0.5513(4) 0.8306(5) 0.049(2) Uani 1 d . . H42 H -0.1165(7) 0.5258(4) 0.8503(5) 0.074 Uiso 1 d R . C43 C -0.0520(7) 0.5819(4) 0.7552(5) 0.051(2) Uani 1 d . . H43 H -0.1139(7) 0.5790(4) 0.7164(5) 0.076 Uiso 1 d R . C44 C 0.0594(7) 0.6175(4) 0.7496(5) 0.055(2) Uani 1 d . . H44 H 0.0834(7) 0.6424(4) 0.7067(5) 0.083 Uiso 1 d R . C45 C 0.1295(7) 0.6087(4) 0.8219(5) 0.053(2) Uani 1 d . . H45 H 0.2063(7) 0.6273(4) 0.8342(5) 0.080 Uiso 1 d 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 0.0276(3) 0.0257(3) 0.0354(4) -0.0025(2) 0.0033(2) -0.0009(2) Co1 0.0211(5) 0.0269(5) 0.0329(5) -0.0017(4) 0.0022(3) 0.0004(3) P1 0.0260(9) 0.0377(10) 0.0361(10) 0.0002(8) 0.0040(7) -0.0022(8) P2 0.0258(9) 0.0323(9) 0.0327(9) -0.0009(7) 0.0011(7) 0.0006(7) S1 0.0292(9) 0.0376(10) 0.0332(9) -0.0005(7) 0.0009(7) 0.0030(7) C1 0.024(3) 0.034(4) 0.037(4) 0.003(3) -0.003(3) 0.001(3) C2 0.025(4) 0.053(5) 0.047(5) 0.003(4) 0.001(3) -0.003(3) C3 0.057(6) 0.100(7) 0.079(6) 0.002(6) -0.011(5) -0.043(5) C4 0.020(3) 0.033(3) 0.034(4) -0.002(3) 0.001(3) -0.001(3) C5 0.024(4) 0.036(4) 0.039(4) -0.001(3) 0.002(3) -0.004(3) C6 0.048(5) 0.064(5) 0.060(5) -0.013(4) 0.021(4) 0.014(4) C7 0.041(4) 0.041(4) 0.041(4) 0.001(3) 0.002(4) -0.003(3) C8 0.034(4) 0.035(4) 0.043(4) -0.002(3) 0.005(3) 0.002(3) C9 0.073(15) 0.069(13) 0.072(15) -0.017(11) 0.055(13) -0.010(13) C9' 0.059(14) 0.090(16) 0.058(13) -0.015(11) 0.012(12) 0.000(13) C10 0.038(5) 0.104(7) 0.063(6) 0.004(5) -0.010(4) -0.030(5) C11 0.077(7) 0.042(5) 0.104(8) 0.014(5) 0.011(6) -0.004(5) C12 0.043(4) 0.051(5) 0.039(4) 0.010(3) -0.008(3) 0.007(4) C13 0.063(6) 0.070(6) 0.061(5) 0.025(4) 0.011(4) 0.000(5) C14 0.060(5) 0.055(5) 0.058(5) 0.003(4) -0.012(4) 0.025(4) C15 0.061(5) 0.062(5) 0.056(5) 0.002(4) -0.024(4) -0.001(4) O2 0.057(3) 0.069(4) 0.043(3) -0.016(3) -0.004(3) -0.014(3) O3 0.036(3) 0.077(4) 0.054(3) -0.013(3) -0.002(3) -0.021(3) O5 0.029(3) 0.092(4) 0.058(3) -0.001(3) 0.000(2) 0.024(3) O6 0.032(3) 0.062(3) 0.046(3) -0.010(2) 0.006(2) 0.011(2) O7 0.062(4) 0.075(4) 0.068(4) 0.012(3) 0.026(3) -0.013(3) O8 0.075(4) 0.046(3) 0.076(4) -0.019(3) 0.015(3) 0.017(3) O9 0.051(3) 0.075(4) 0.055(3) 0.009(3) 0.019(3) 0.026(3) O10 0.031(3) 0.056(3) 0.042(3) -0.001(2) -0.002(2) -0.015(2) O11 0.047(3) 0.049(3) 0.053(3) 0.014(2) 0.005(2) -0.007(2) C21 0.024(3) 0.035(4) 0.040(4) 0.003(3) 0.000(3) -0.001(3) C22 0.035(4) 0.046(4) 0.043(4) 0.003(3) -0.003(3) 0.002(3) C23 0.041(5) 0.048(5) 0.067(6) 0.011(4) 0.008(4) 0.011(4) C24 0.036(4) 0.054(5) 0.071(6) 0.013(4) -0.017(4) 0.007(4) C25 0.046(5) 0.053(5) 0.056(5) 0.005(4) -0.011(4) 0.002(4) C26 0.036(4) 0.043(4) 0.042(4) 0.001(3) -0.003(3) -0.002(3) C31 0.033(4) 0.039(4) 0.031(4) -0.003(3) -0.003(3) 0.003(3) C32 0.049(5) 0.045(4) 0.041(4) 0.006(3) 0.005(3) -0.001(4) C33 0.074(6) 0.066(6) 0.050(5) -0.005(4) 0.021(4) -0.001(5) C34 0.061(5) 0.080(6) 0.040(5) -0.015(4) 0.016(4) 0.000(5) C35 0.056(5) 0.056(5) 0.062(5) -0.018(4) 0.005(4) -0.004(4) C36 0.035(4) 0.046(4) 0.044(4) -0.009(3) 0.009(3) -0.005(3) C41 0.060(5) 0.044(5) 0.056(5) -0.019(4) 0.011(4) 0.009(4) C42 0.046(5) 0.032(4) 0.072(6) -0.006(4) 0.020(4) 0.005(3) C43 0.048(5) 0.031(4) 0.072(5) -0.002(4) -0.002(4) 0.014(4) C44 0.064(6) 0.027(4) 0.076(6) 0.004(4) 0.019(5) 0.008(4) C45 0.052(5) 0.030(4) 0.077(6) -0.016(4) 0.006(5) -0.002(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 C7 1.953(8) . ? Mo1 C4 2.132(6) . ? Mo1 C1 2.212(6) . ? Mo1 C45 2.312(7) . ? Mo1 C44 2.318(7) . ? Mo1 C41 2.322(7) . ? Mo1 C43 2.360(7) . ? Mo1 C42 2.385(7) . ? Mo1 P2 2.401(2) . ? Mo1 Co1 2.7173(11) . ? Mo1 S1 3.162(2) . ? Co1 C8 1.759(7) . ? Co1 C4 2.014(6) . ? Co1 P1 2.159(2) . ? Co1 P2 2.209(2) . ? Co1 S1 2.346(2) . ? P1 O9 1.590(5) . ? P1 O10 1.592(5) . ? P1 O11 1.613(5) . ? P2 C31 1.816(6) . ? P2 C21 1.856(6) . ? S1 C1 1.800(6) . ? S1 C12 1.903(7) . ? C1 C4 1.434(9) . ? C1 C2 1.485(9) . ? C2 O2 1.223(8) . ? C2 O3 1.349(8) . ? C3 O3 1.467(9) . ? C4 C5 1.463(9) . ? C5 O5 1.186(8) . ? C5 O6 1.334(8) . ? C6 O6 1.444(8) . ? C7 O7 1.154(8) . ? C8 O8 1.145(8) . ? C9 O9 1.38(2) . ? C9' O9 1.39(2) . ? C10 O10 1.432(8) . ? C11 O11 1.429(9) . ? C12 C14 1.517(10) . ? C12 C13 1.525(10) . ? C12 C15 1.526(10) . ? C21 C26 1.384(9) . ? C21 C22 1.388(9) . ? C22 C23 1.389(10) . ? C23 C24 1.380(11) . ? C24 C25 1.364(11) . ? C25 C26 1.370(10) . ? C31 C36 1.387(9) . ? C31 C32 1.399(9) . ? C32 C33 1.398(10) . ? C33 C34 1.381(12) . ? C34 C35 1.389(11) . ? C35 C36 1.403(10) . ? C41 C45 1.398(11) . ? C41 C42 1.428(10) . ? C42 C43 1.427(10) . ? C43 C44 1.409(11) . ? C44 C45 1.439(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 C7 Mo1 C4 76.8(3) . . ? C7 Mo1 C1 94.4(3) . . ? C4 Mo1 C1 38.5(2) . . ? C7 Mo1 C45 89.2(3) . . ? C4 Mo1 C45 131.7(3) . . ? C1 Mo1 C45 98.9(3) . . ? C7 Mo1 C44 83.9(3) . . ? C4 Mo1 C44 157.9(3) . . ? C1 Mo1 C44 134.9(3) . . ? C45 Mo1 C44 36.2(3) . . ? C7 Mo1 C41 122.8(3) . . ? C4 Mo1 C41 124.3(3) . . ? C1 Mo1 C41 85.9(3) . . ? C45 Mo1 C41 35.1(3) . . ? C44 Mo1 C41 59.0(3) . . ? C7 Mo1 C43 113.0(3) . . ? C4 Mo1 C43 166.9(3) . . ? C1 Mo1 C43 143.0(3) . . ? C45 Mo1 C43 59.2(3) . . ? C44 Mo1 C43 35.0(3) . . ? C41 Mo1 C43 58.7(3) . . ? C7 Mo1 C42 142.1(3) . . ? C4 Mo1 C42 138.9(2) . . ? C1 Mo1 C42 109.0(3) . . ? C45 Mo1 C42 58.7(3) . . ? C44 Mo1 C42 58.4(3) . . ? C41 Mo1 C42 35.3(3) . . ? C43 Mo1 C42 35.0(3) . . ? C7 Mo1 P2 97.3(2) . . ? C4 Mo1 P2 79.0(2) . . ? C1 Mo1 P2 110.5(2) . . ? C45 Mo1 P2 149.2(2) . . ? C44 Mo1 P2 114.5(2) . . ? C41 Mo1 P2 135.9(2) . . ? C43 Mo1 P2 90.9(2) . . ? C42 Mo1 P2 101.5(2) . . ? C7 Mo1 Co1 115.9(2) . . ? C4 Mo1 Co1 47.2(2) . . ? C1 Mo1 Co1 62.7(2) . . ? C45 Mo1 Co1 148.7(2) . . ? C44 Mo1 Co1 154.8(2) . . ? C41 Mo1 Co1 114.6(2) . . ? C43 Mo1 Co1 119.8(2) . . ? C42 Mo1 Co1 101.4(2) . . ? P2 Mo1 Co1 50.67(4) . . ? C7 Mo1 S1 127.1(2) . . ? C4 Mo1 S1 56.0(2) . . ? C1 Mo1 S1 33.6(2) . . ? C45 Mo1 S1 104.1(2) . . ? C44 Mo1 S1 134.3(2) . . ? C41 Mo1 S1 75.4(2) . . ? C43 Mo1 S1 117.7(2) . . ? C42 Mo1 S1 83.4(2) . . ? P2 Mo1 S1 95.81(5) . . ? Co1 Mo1 S1 46.27(4) . . ? C8 Co1 C4 92.6(3) . . ? C8 Co1 P1 96.9(2) . . ? C4 Co1 P1 168.7(2) . . ? C8 Co1 P2 106.5(2) . . ? C4 Co1 P2 86.3(2) . . ? P1 Co1 P2 96.95(7) . . ? C8 Co1 S1 117.7(2) . . ? C4 Co1 S1 74.3(2) . . ? P1 Co1 S1 95.70(7) . . ? P2 Co1 S1 131.87(7) . . ? C8 Co1 Mo1 137.6(2) . . ? C4 Co1 Mo1 51.0(2) . . ? P1 Co1 Mo1 122.32(6) . . ? P2 Co1 Mo1 57.22(5) . . ? S1 Co1 Mo1 76.90(5) . . ? O9 P1 O10 106.4(3) . . ? O9 P1 O11 97.7(3) . . ? O10 P1 O11 103.4(3) . . ? O9 P1 Co1 117.2(2) . . ? O10 P1 Co1 112.2(2) . . ? O11 P1 Co1 117.9(2) . . ? C31 P2 C21 99.0(3) . . ? C31 P2 Co1 114.1(2) . . ? C21 P2 Co1 124.2(2) . . ? C31 P2 Mo1 125.6(2) . . ? C21 P2 Mo1 122.5(2) . . ? Co1 P2 Mo1 72.11(6) . . ? C1 S1 C12 109.5(3) . . ? C1 S1 Co1 76.5(2) . . ? C12 S1 Co1 114.4(2) . . ? C1 S1 Mo1 42.8(2) . . ? C12 S1 Mo1 150.3(2) . . ? Co1 S1 Mo1 56.83(4) . . ? C4 C1 C2 130.0(6) . . ? C4 C1 S1 109.3(4) . . ? C2 C1 S1 118.5(5) . . ? C4 C1 Mo1 67.8(3) . . ? C2 C1 Mo1 111.5(4) . . ? S1 C1 Mo1 103.5(3) . . ? O2 C2 O3 123.4(6) . . ? O2 C2 C1 125.5(6) . . ? O3 C2 C1 111.1(6) . . ? C1 C4 C5 126.1(6) . . ? C1 C4 Co1 96.5(4) . . ? C5 C4 Co1 122.6(4) . . ? C1 C4 Mo1 73.7(3) . . ? C5 C4 Mo1 140.6(5) . . ? Co1 C4 Mo1 81.8(2) . . ? O5 C5 O6 122.6(6) . . ? O5 C5 C4 125.9(6) . . ? O6 C5 C4 111.5(6) . . ? O7 C7 Mo1 175.5(6) . . ? O8 C8 Co1 175.3(6) . . ? C14 C12 C13 111.8(7) . . ? C14 C12 C15 111.3(6) . . ? C13 C12 C15 109.2(6) . . ? C14 C12 S1 112.3(5) . . ? C13 C12 S1 103.6(5) . . ? C15 C12 S1 108.4(5) . . ? C2 O3 C3 114.7(6) . . ? C5 O6 C6 117.9(6) . . ? C9 O9 P1 137.0(10) . . ? C9' O9 P1 126.3(11) . . ? C10 O10 P1 123.2(5) . . ? C11 O11 P1 121.6(5) . . ? C26 C21 C22 117.8(6) . . ? C26 C21 P2 121.5(5) . . ? C22 C21 P2 120.7(5) . . ? C21 C22 C23 121.2(7) . . ? C24 C23 C22 119.4(7) . . ? C25 C24 C23 119.7(7) . . ? C24 C25 C26 120.9(7) . . ? C25 C26 C21 121.1(7) . . ? C36 C31 C32 119.2(6) . . ? C36 C31 P2 120.4(5) . . ? C32 C31 P2 120.4(5) . . ? C33 C32 C31 120.5(7) . . ? C34 C33 C32 119.7(8) . . ? C33 C34 C35 120.3(7) . . ? C34 C35 C36 119.9(7) . . ? C31 C36 C35 120.2(7) . . ? C45 C41 C42 109.2(7) . . ? C45 C41 Mo1 72.0(4) . . ? C42 C41 Mo1 74.8(4) . . ? C43 C42 C41 107.0(7) . . ? C43 C42 Mo1 71.5(4) . . ? C41 C42 Mo1 69.9(4) . . ? C44 C43 C42 108.2(7) . . ? C44 C43 Mo1 70.9(4) . . ? C42 C43 Mo1 73.5(4) . . ? C43 C44 C45 108.2(7) . . ? C43 C44 Mo1 74.1(4) . . ? C45 C44 Mo1 71.7(4) . . ? C41 C45 C44 107.3(7) . . ? C41 C45 Mo1 72.8(4) . . ? C44 C45 Mo1 72.1(4) . . ? _refine_diff_density_max 0.493 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.124 data_mm9617 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H36 Co Mo O8 P S' _chemical_formula_weight 838.57 _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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 9.517(2) _cell_length_b 9.699(2) _cell_length_c 40.567(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.39(3) _cell_angle_gamma 90.00 _cell_volume 3743.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method ? _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type 'semi empirical (4 psi scans)' _exptl_absorpt_correction_T_min 0.932 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(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 'Rigaku AFC5R' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.7% _diffrn_reflns_number 10498 _diffrn_reflns_av_R_equivalents 0.1335 _diffrn_reflns_av_sigmaI/netI 0.1708 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4896 _reflns_number_observed 2527 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Rigaku control software' _computing_cell_refinement 'Rigaku control software' _computing_data_reduction 'TeXsan' _computing_structure_solution 'SIR 92' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 20 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^)+(0.0174P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4876 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1603 _refine_ls_R_factor_obs 0.0481 _refine_ls_wR_factor_all 0.5203 _refine_ls_wR_factor_obs 0.0814 _refine_ls_goodness_of_fit_all 0.967 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 4.805 _refine_ls_restrained_S_obs 1.097 _refine_ls_shift/esd_max 0.022 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.07059(7) -0.25275(7) 0.41836(2) 0.0345(2) Uani 1 d . . Co1 Co 0.27454(10) -0.20376(10) 0.37419(2) 0.0318(3) Uani 1 d . . P1 P 0.3616(2) -0.0689(2) 0.33523(5) 0.0335(5) Uani 1 d . . S1 S 0.5249(2) -0.1876(2) 0.31419(5) 0.0431(6) Uani 1 d . . O1 O 0.5459(6) -0.2845(7) 0.40407(15) 0.080(2) Uani 1 d . . C1 C 0.4383(9) -0.2578(9) 0.3925(2) 0.050(2) Uani 1 d . . C2 C 0.2234(8) -0.3485(8) 0.3499(2) 0.036(2) Uani 1 d . . O2 O 0.1927(6) -0.4481(6) 0.33622(14) 0.063(2) Uani 1 d . . C3 C -0.0793(10) -0.1171(10) 0.4304(2) 0.056(3) Uani 1 d . . O3 O -0.1647(8) -0.0440(7) 0.4376(2) 0.088(2) Uani 1 d . . C4 C -0.0573(9) -0.3069(9) 0.3805(2) 0.052(3) Uani 1 d . . O4 O -0.1337(7) -0.3442(7) 0.3604(2) 0.081(2) Uani 1 d . . C5 C 0.4769(10) 0.1063(9) 0.4582(2) 0.082(3) Uani 1 d . . H5A H 0.5681(28) 0.0723(29) 0.4648(13) 0.123 Uiso 1 calc R . H5B H 0.4223(34) 0.1220(48) 0.4775(8) 0.123 Uiso 1 calc R . H5C H 0.4869(59) 0.1913(22) 0.4464(6) 0.123 Uiso 1 calc R . O5 O 0.4067(6) 0.0063(6) 0.43732(14) 0.060(2) Uani 1 d . . C6 C 0.2678(10) 0.0228(8) 0.4316(2) 0.041(2) Uani 1 d . . O6 O 0.2016(7) 0.1110(6) 0.4447(2) 0.074(2) Uani 1 d . . C7 C 0.2130(8) -0.0837(7) 0.4094(2) 0.034(2) Uani 1 d . . O7 O -0.0951(6) -0.0139(6) 0.35613(15) 0.064(2) Uani 1 d . . C8 C 0.1123(8) -0.0876(7) 0.3851(2) 0.034(2) Uani 1 d . . O8 O 0.0919(5) 0.1247(5) 0.35829(12) 0.0441(14) Uani 1 d . . C9 C 0.0250(9) 0.0078(8) 0.3652(2) 0.036(2) Uani 1 d . . C10 C 0.0171(9) 0.2178(8) 0.3358(2) 0.062(3) Uani 1 d . . H10A H 0.0788(19) 0.2909(31) 0.3294(10) 0.093 Uiso 1 calc R . H10B H -0.0628(33) 0.2559(42) 0.3466(5) 0.093 Uiso 1 calc R . H10C H -0.0140(48) 0.1678(14) 0.3165(6) 0.093 Uiso 1 calc R . C11 C 0.1823(11) -0.4559(9) 0.4399(2) 0.049(2) Uani 1 d . . C12 C 0.2036(11) -0.3460(9) 0.4627(2) 0.054(3) Uani 1 d . . C13 C 0.0740(15) -0.3020(10) 0.4744(2) 0.073(3) Uani 1 d . . C14 C -0.0300(11) -0.3878(12) 0.4580(3) 0.068(3) Uani 1 d . . C15 C 0.0378(13) -0.4796(9) 0.4371(2) 0.061(3) Uani 1 d . . C16 C 0.2969(12) -0.5458(9) 0.4262(2) 0.107(5) Uani 1 d . . H16A H 0.3020(54) -0.6307(34) 0.4383(12) 0.160 Uiso 1 calc R . H16B H 0.3854(17) -0.4986(33) 0.4281(16) 0.160 Uiso 1 calc R . H16C H 0.2759(41) -0.5652(63) 0.4034(6) 0.160 Uiso 1 calc R . C17 C 0.3487(11) -0.2978(11) 0.4766(2) 0.111(4) Uani 1 d . . H17A H 0.3617(35) -0.3307(66) 0.4988(7) 0.167 Uiso 1 calc R . H17B H 0.3526(29) -0.1989(11) 0.4765(17) 0.167 Uiso 1 calc R . H17C H 0.4217(11) -0.3340(62) 0.4632(11) 0.167 Uiso 1 calc R . C18 C 0.0536(16) -0.1998(11) 0.5015(2) 0.162(7) Uani 1 d . . H18A H 0.0786(116) -0.2414(40) 0.5223(3) 0.244 Uiso 1 calc R . H18B H -0.0431(27) -0.1716(87) 0.5016(18) 0.244 Uiso 1 calc R . H18C H 0.1121(88) -0.1208(53) 0.4980(15) 0.244 Uiso 1 calc R . C19 C -0.1854(12) -0.3920(13) 0.4658(3) 0.165(7) Uani 1 d . . H19A H -0.1990(18) -0.4492(94) 0.4848(17) 0.247 Uiso 1 calc R . H19B H -0.2375(18) -0.4292(103) 0.4473(11) 0.247 Uiso 1 calc R . H19C H -0.2179(29) -0.3004(21) 0.4703(26) 0.247 Uiso 1 calc R . C20 C -0.0234(13) -0.5975(9) 0.4169(3) 0.131(5) Uani 1 d . . H20A H -0.0119(87) -0.6821(16) 0.4290(10) 0.196 Uiso 1 calc R . H20B H 0.0244(63) -0.6041(59) 0.3964(10) 0.196 Uiso 1 calc R . H20C H -0.1217(23) -0.5811(46) 0.4126(19) 0.196 Uiso 1 calc R . C21 C 0.5891(8) -0.0804(8) 0.2814(2) 0.040(2) Uani 1 d . . C22 C 0.6877(9) 0.0187(9) 0.2877(2) 0.054(3) Uani 1 d . . H22 H 0.7257(9) 0.0283(9) 0.3089(2) 0.064 Uiso 1 calc R . C23 C 0.7318(9) 0.1050(9) 0.2628(2) 0.061(3) Uani 1 d . . H23 H 0.7940(9) 0.1768(9) 0.2675(2) 0.073 Uiso 1 calc R . C24 C 0.6824(9) 0.0832(9) 0.2312(2) 0.061(3) Uani 1 d . . H24 H 0.7145(9) 0.1381(9) 0.2141(2) 0.073 Uiso 1 calc R . C25 C 0.5864(9) -0.0188(9) 0.2245(2) 0.053(2) Uani 1 d . . H25 H 0.5533(9) -0.0325(9) 0.2030(2) 0.064 Uiso 1 calc R . C26 C 0.5392(8) -0.1003(8) 0.2493(2) 0.045(2) Uani 1 d . . H26 H 0.4735(8) -0.1692(8) 0.2447(2) 0.054 Uiso 1 calc R . C27 C 0.2513(8) -0.0262(7) 0.2995(2) 0.032(2) Uani 1 d . . C28 C 0.2905(8) 0.0703(7) 0.2755(2) 0.039(2) Uani 1 d . . H28 H 0.3720(8) 0.1223(7) 0.2784(2) 0.047 Uiso 1 calc R . C29 C 0.2052(9) 0.0870(9) 0.2470(2) 0.052(3) Uani 1 d . . H29 H 0.2293(9) 0.1526(9) 0.2314(2) 0.062 Uiso 1 calc R . C30 C 0.0869(10) 0.0084(9) 0.2418(2) 0.052(3) Uani 1 d . . H30 H 0.0329(10) 0.0191(9) 0.2225(2) 0.063 Uiso 1 calc R . C31 C 0.0484(9) -0.0867(8) 0.2652(2) 0.049(2) Uani 1 d . . H31 H -0.0321(9) -0.1396(8) 0.2618(2) 0.059 Uiso 1 calc R . C32 C 0.1289(8) -0.1036(7) 0.2936(2) 0.037(2) Uani 1 d . . H32 H 0.1014(8) -0.1678(7) 0.3092(2) 0.045 Uiso 1 calc R . C33 C 0.4524(8) 0.0908(8) 0.3482(2) 0.037(2) Uani 1 d . . C34 C 0.5722(9) 0.0785(9) 0.3682(2) 0.051(2) Uani 1 d . . H34 H 0.6050(9) -0.0088(9) 0.3739(2) 0.061 Uiso 1 calc R . C35 C 0.6433(10) 0.1930(11) 0.3798(2) 0.064(3) Uani 1 d . . H35 H 0.7213(10) 0.1825(11) 0.3938(2) 0.077 Uiso 1 calc R . C36 C 0.5993(10) 0.3215(10) 0.3708(2) 0.062(3) Uani 1 d . . H36 H 0.6508(10) 0.3983(10) 0.3776(2) 0.074 Uiso 1 calc R . C37 C 0.4790(10) 0.3384(9) 0.3516(2) 0.066(3) Uani 1 d . . H37 H 0.4469(10) 0.4263(9) 0.3461(2) 0.080 Uiso 1 calc R . C38 C 0.4061(8) 0.2223(8) 0.3404(2) 0.051(2) Uani 1 d . . H38 H 0.3248(8) 0.2334(8) 0.3275(2) 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 0.0417(4) 0.0351(4) 0.0268(3) 0.0053(4) 0.0016(3) 0.0013(4) Co1 0.0346(6) 0.0320(6) 0.0289(6) 0.0032(5) 0.0002(5) 0.0030(5) P1 0.0327(13) 0.0337(13) 0.0343(12) 0.0024(10) 0.0022(10) -0.0005(11) S1 0.0406(13) 0.0415(13) 0.0474(13) 0.0012(11) 0.0081(11) 0.0090(11) O1 0.046(4) 0.104(6) 0.090(5) 0.032(4) -0.015(4) 0.015(4) C1 0.053(6) 0.050(6) 0.046(5) 0.019(5) 0.006(4) 0.003(6) C2 0.045(5) 0.031(5) 0.033(5) -0.003(4) 0.002(4) 0.006(4) O2 0.073(5) 0.044(4) 0.070(4) -0.017(3) -0.007(4) -0.005(4) C3 0.059(7) 0.065(7) 0.045(6) 0.019(5) 0.019(5) 0.008(6) O3 0.092(6) 0.092(6) 0.083(5) 0.009(4) 0.034(5) 0.044(5) C4 0.042(6) 0.057(7) 0.055(6) 0.017(5) -0.005(5) -0.002(5) O4 0.070(5) 0.091(5) 0.081(5) 0.000(4) -0.024(4) -0.019(4) C5 0.085(8) 0.072(8) 0.088(8) -0.028(6) -0.034(6) -0.015(6) O5 0.058(4) 0.051(4) 0.069(4) -0.022(3) -0.013(4) -0.002(4) C6 0.058(7) 0.033(5) 0.031(5) 0.007(4) 0.000(5) 0.015(5) O6 0.070(5) 0.061(5) 0.091(5) -0.041(4) 0.001(4) 0.009(4) C7 0.038(5) 0.025(5) 0.039(5) 0.006(4) -0.002(4) 0.001(4) O7 0.033(4) 0.064(4) 0.094(5) 0.036(4) -0.020(4) -0.002(3) C8 0.040(5) 0.030(5) 0.034(5) 0.006(4) -0.001(4) 0.004(4) O8 0.050(4) 0.033(3) 0.049(4) 0.016(3) -0.009(3) 0.005(3) C9 0.033(5) 0.033(5) 0.040(5) 0.003(4) 0.004(4) 0.009(5) C10 0.075(7) 0.043(6) 0.069(6) 0.031(5) -0.004(5) -0.001(5) C11 0.063(7) 0.040(6) 0.045(6) 0.014(5) 0.005(5) 0.016(6) C12 0.077(8) 0.050(6) 0.036(6) 0.016(5) -0.018(6) -0.006(6) C13 0.136(11) 0.057(7) 0.026(5) 0.020(5) 0.013(7) 0.026(8) C14 0.056(7) 0.079(9) 0.069(8) 0.050(7) 0.012(6) 0.017(7) C15 0.089(9) 0.042(6) 0.051(6) 0.020(5) -0.016(6) -0.009(6) C16 0.146(11) 0.065(7) 0.112(9) 0.046(7) 0.046(9) 0.061(8) C17 0.119(10) 0.111(9) 0.100(8) 0.052(7) -0.074(8) -0.046(8) C18 0.366(22) 0.104(10) 0.019(5) 0.004(6) 0.028(9) 0.093(12) C19 0.087(10) 0.221(16) 0.189(14) 0.161(13) 0.053(10) 0.028(10) C20 0.222(15) 0.057(8) 0.110(10) 0.015(7) -0.083(10) -0.052(9) C21 0.029(5) 0.052(6) 0.041(5) 0.001(5) 0.009(4) 0.013(5) C22 0.039(6) 0.082(7) 0.040(5) 0.002(5) -0.005(5) -0.014(5) C23 0.047(6) 0.067(7) 0.069(7) 0.001(6) 0.003(6) -0.019(5) C24 0.049(6) 0.066(7) 0.068(7) 0.009(6) 0.007(6) -0.016(6) C25 0.062(7) 0.057(6) 0.041(6) 0.004(5) 0.006(5) -0.003(6) C26 0.046(6) 0.033(5) 0.057(6) -0.021(5) 0.009(5) -0.002(4) C27 0.040(5) 0.027(5) 0.030(5) 0.001(4) 0.006(4) 0.009(4) C28 0.035(5) 0.037(5) 0.046(5) -0.003(4) 0.012(4) -0.006(4) C29 0.061(7) 0.058(6) 0.037(5) 0.018(5) 0.007(5) 0.017(6) C30 0.061(7) 0.053(6) 0.041(6) 0.004(5) -0.016(5) 0.015(6) C31 0.042(6) 0.044(6) 0.061(6) 0.008(5) -0.015(5) 0.000(5) C32 0.040(5) 0.033(5) 0.039(5) 0.006(4) -0.004(4) -0.006(4) C33 0.035(5) 0.036(5) 0.039(5) -0.007(4) 0.001(4) -0.006(4) C34 0.053(6) 0.037(5) 0.062(6) -0.007(5) -0.009(5) 0.004(5) C35 0.056(7) 0.064(7) 0.072(7) -0.013(6) -0.018(5) -0.003(6) C36 0.047(7) 0.048(7) 0.091(8) -0.021(6) 0.003(6) -0.012(6) C37 0.056(7) 0.041(7) 0.102(8) -0.003(6) -0.007(6) -0.002(5) C38 0.040(5) 0.043(6) 0.068(6) -0.006(5) -0.009(5) 0.005(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 C3 2.009(10) . ? Mo1 C4 2.005(9) . ? Mo1 C8 2.138(7) . ? Mo1 C7 2.163(7) . ? Mo1 C14 2.301(9) . ? Mo1 C13 2.322(8) . ? Mo1 C15 2.350(8) . ? Mo1 C12 2.356(8) . ? Mo1 C11 2.395(8) . ? Mo1 Co1 2.7153(14) . ? Co1 C2 1.776(8) . ? Co1 C1 1.789(9) . ? Co1 C7 1.945(7) . ? Co1 C8 1.970(7) . ? Co1 P1 2.227(2) . ? P1 C27 1.816(7) . ? P1 C33 1.844(8) . ? P1 S1 2.129(3) . ? S1 C21 1.808(8) . ? O1 C1 1.146(8) . ? C2 O2 1.148(8) . ? C3 O3 1.123(9) . ? C4 O4 1.140(8) . ? C5 O5 1.442(8) . ? O5 C6 1.346(9) . ? C6 O6 1.195(8) . ? C6 C7 1.457(10) . ? C7 C8 1.360(9) . ? O7 C9 1.210(8) . ? C8 C9 1.471(10) . ? O8 C9 1.334(8) . ? O8 C10 1.457(8) . ? C11 C15 1.396(12) . ? C11 C12 1.423(11) . ? C11 C16 1.513(11) . ? C12 C13 1.398(12) . ? C12 C17 1.551(11) . ? C13 C14 1.443(13) . ? C13 C18 1.497(12) . ? C14 C15 1.399(12) . ? C14 C19 1.521(12) . ? C15 C20 1.514(11) . ? C21 C22 1.364(10) . ? C21 C26 1.387(9) . ? C22 C23 1.385(10) . ? C23 C24 1.374(10) . ? C24 C25 1.369(10) . ? C25 C26 1.365(10) . ? C27 C32 1.402(9) . ? C27 C28 1.409(9) . ? C28 C29 1.406(9) . ? C29 C30 1.371(10) . ? C30 C31 1.381(10) . ? C31 C32 1.377(9) . ? C33 C38 1.384(9) . ? C33 C34 1.390(10) . ? C34 C35 1.377(10) . ? C35 C36 1.362(11) . ? C36 C37 1.380(11) . ? C37 C38 1.392(10) . ? 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 C3 Mo1 C4 86.3(4) . . ? C3 Mo1 C8 78.8(3) . . ? C4 Mo1 C8 80.3(3) . . ? C3 Mo1 C7 89.8(3) . . ? C4 Mo1 C7 116.2(3) . . ? C8 Mo1 C7 36.9(2) . . ? C3 Mo1 C14 83.9(4) . . ? C4 Mo1 C14 97.5(4) . . ? C8 Mo1 C14 162.7(3) . . ? C7 Mo1 C14 145.2(4) . . ? C3 Mo1 C13 83.7(4) . . ? C4 Mo1 C13 133.6(4) . . ? C8 Mo1 C13 140.7(3) . . ? C7 Mo1 C13 109.0(4) . . ? C14 Mo1 C13 36.4(3) . . ? C3 Mo1 C15 115.7(4) . . ? C4 Mo1 C15 85.4(3) . . ? C8 Mo1 C15 158.9(3) . . ? C7 Mo1 C15 148.4(4) . . ? C14 Mo1 C15 35.0(3) . . ? C13 Mo1 C15 59.4(3) . . ? C3 Mo1 C12 116.0(4) . . ? C4 Mo1 C12 142.1(3) . . ? C8 Mo1 C12 131.7(3) . . ? C7 Mo1 C12 95.3(3) . . ? C14 Mo1 C12 58.1(3) . . ? C13 Mo1 C12 34.8(3) . . ? C15 Mo1 C12 57.8(3) . . ? C3 Mo1 C11 139.6(3) . . ? C4 Mo1 C11 108.7(3) . . ? C8 Mo1 C11 139.4(3) . . ? C7 Mo1 C11 114.2(3) . . ? C14 Mo1 C11 57.6(3) . . ? C13 Mo1 C11 58.5(3) . . ? C15 Mo1 C11 34.2(3) . . ? C12 Mo1 C11 34.8(3) . . ? C3 Mo1 Co1 124.6(2) . . ? C4 Mo1 Co1 88.3(2) . . ? C8 Mo1 Co1 46.0(2) . . ? C7 Mo1 Co1 45.3(2) . . ? C14 Mo1 Co1 151.3(3) . . ? C13 Mo1 Co1 133.5(4) . . ? C15 Mo1 Co1 118.6(3) . . ? C12 Mo1 Co1 101.1(3) . . ? C11 Mo1 Co1 93.8(2) . . ? C2 Co1 C1 102.9(4) . . ? C2 Co1 C7 142.9(3) . . ? C1 Co1 C7 98.3(3) . . ? C2 Co1 C8 111.8(3) . . ? C1 Co1 C8 138.9(3) . . ? C7 Co1 C8 40.7(3) . . ? C2 Co1 P1 100.0(2) . . ? C1 Co1 P1 97.6(3) . . ? C7 Co1 P1 107.1(2) . . ? C8 Co1 P1 97.5(2) . . ? C2 Co1 Mo1 92.1(2) . . ? C1 Co1 Mo1 107.7(2) . . ? C7 Co1 Mo1 52.2(2) . . ? C8 Co1 Mo1 51.3(2) . . ? P1 Co1 Mo1 148.81(7) . . ? C27 P1 C33 107.1(4) . . ? C27 P1 S1 102.5(2) . . ? C33 P1 S1 103.1(3) . . ? C27 P1 Co1 118.8(3) . . ? C33 P1 Co1 118.1(3) . . ? S1 P1 Co1 104.75(11) . . ? C21 S1 P1 104.3(3) . . ? O1 C1 Co1 175.9(9) . . ? O2 C2 Co1 175.0(7) . . ? O3 C3 Mo1 178.1(8) . . ? O4 C4 Mo1 175.4(8) . . ? C6 O5 C5 117.4(7) . . ? O6 C6 O5 122.3(8) . . ? O6 C6 C7 126.7(9) . . ? O5 C6 C7 110.9(7) . . ? C8 C7 C6 134.6(7) . . ? C8 C7 Co1 70.7(4) . . ? C6 C7 Co1 140.2(6) . . ? C8 C7 Mo1 70.6(4) . . ? C6 C7 Mo1 130.6(5) . . ? Co1 C7 Mo1 82.6(3) . . ? C7 C8 C9 139.4(7) . . ? C7 C8 Co1 68.7(4) . . ? C9 C8 Co1 132.2(5) . . ? C7 C8 Mo1 72.6(4) . . ? C9 C8 Mo1 134.9(6) . . ? Co1 C8 Mo1 82.6(3) . . ? C9 O8 C10 115.5(6) . . ? O7 C9 O8 122.4(7) . . ? O7 C9 C8 125.0(8) . . ? O8 C9 C8 112.6(7) . . ? C15 C11 C12 107.6(8) . . ? C15 C11 C16 126.2(10) . . ? C12 C11 C16 125.4(10) . . ? C15 C11 Mo1 71.2(5) . . ? C12 C11 Mo1 71.1(5) . . ? C16 C11 Mo1 131.1(6) . . ? C13 C12 C11 109.6(9) . . ? C13 C12 C17 124.8(10) . . ? C11 C12 C17 125.0(10) . . ? C13 C12 Mo1 71.3(5) . . ? C11 C12 Mo1 74.1(5) . . ? C17 C12 Mo1 128.2(6) . . ? C12 C13 C14 105.6(9) . . ? C12 C13 C18 125.6(12) . . ? C14 C13 C18 128.4(13) . . ? C12 C13 Mo1 74.0(5) . . ? C14 C13 Mo1 71.0(5) . . ? C18 C13 Mo1 125.8(6) . . ? C15 C14 C13 109.0(9) . . ? C15 C14 C19 125.1(13) . . ? C13 C14 C19 125.4(12) . . ? C15 C14 Mo1 74.5(5) . . ? C13 C14 Mo1 72.6(5) . . ? C19 C14 Mo1 125.8(6) . . ? C11 C15 C14 108.2(9) . . ? C11 C15 C20 122.3(11) . . ? C14 C15 C20 129.2(12) . . ? C11 C15 Mo1 74.6(5) . . ? C14 C15 Mo1 70.6(5) . . ? C20 C15 Mo1 125.8(6) . . ? C22 C21 C26 119.6(8) . . ? C22 C21 S1 120.6(7) . . ? C26 C21 S1 119.8(7) . . ? C21 C22 C23 120.5(8) . . ? C24 C23 C22 119.1(9) . . ? C23 C24 C25 120.5(9) . . ? C26 C25 C24 120.2(8) . . ? C25 C26 C21 120.0(8) . . ? C32 C27 C28 118.0(7) . . ? C32 C27 P1 118.5(6) . . ? C28 C27 P1 123.1(6) . . ? C27 C28 C29 119.3(7) . . ? C30 C29 C28 121.1(8) . . ? C29 C30 C31 119.8(8) . . ? C32 C31 C30 120.2(8) . . ? C31 C32 C27 121.6(7) . . ? C38 C33 C34 117.7(7) . . ? C38 C33 P1 124.4(6) . . ? C34 C33 P1 117.8(6) . . ? C35 C34 C33 121.4(8) . . ? C36 C35 C34 120.1(9) . . ? C35 C36 C37 120.4(9) . . ? C36 C37 C38 119.2(8) . . ? C33 C38 C37 121.2(8) . . ? _refine_diff_density_max 0.363 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.088 data_torq01 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C37 H32 Co O6 P S2 W' _chemical_formula_weight 910.50 _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' 'S' 'S' 0.1246 0.1234 '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' 'W' 'W' -0.8490 6.8722 '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 9.555(2) _cell_length_b 10.419(2) _cell_length_c 19.358(4) _cell_angle_alpha 76.22(3) _cell_angle_beta 76.57(3) _cell_angle_gamma 73.19(3) _cell_volume 1763.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method ? _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 3.937 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4918 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0959 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 22.52 _reflns_number_total 4618 _reflns_number_observed 3460 _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^)+(0.0528P)^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 4618 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_obs 0.0509 _refine_ls_wR_factor_all 0.1224 _refine_ls_wR_factor_obs 0.1078 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.062 _refine_ls_restrained_S_all 1.027 _refine_ls_restrained_S_obs 1.062 _refine_ls_shift/esd_max 0.035 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.07529(5) 0.20656(5) 0.08725(3) 0.0352(2) Uani 1 d . . Co1 Co -0.1167(2) 0.14101(15) 0.19997(8) 0.0316(4) Uani 1 d . . P1 P -0.2254(3) 0.1342(3) 0.3139(2) 0.0371(7) Uani 1 d . . S1 S 0.1253(3) 0.0860(3) 0.2071(2) 0.0390(7) Uani 1 d . . S2 S -0.1215(4) 0.2260(4) 0.3676(2) 0.0494(8) Uani 1 d . . C1 C 0.1700(16) 0.3460(20) -0.0180(9) 0.082(6) Uani 1 d . . H1 H 0.1126(16) 0.4049(20) -0.0509(9) 0.123 Uiso 1 d R . C2 C 0.2008(16) 0.3806(16) 0.0414(10) 0.071(5) Uani 1 d . . H2 H 0.1643(16) 0.4653(16) 0.0553(10) 0.106 Uiso 1 d R . C3 C 0.2925(15) 0.2681(19) 0.0761(9) 0.072(5) Uani 1 d . . H3 H 0.3310(15) 0.2646(19) 0.1166(9) 0.109 Uiso 1 d R . C4 C 0.3189(14) 0.1612(17) 0.0387(7) 0.062(4) Uani 1 d . . H4 H 0.3774(14) 0.0735(17) 0.0507(7) 0.094 Uiso 1 d R . C5 C 0.2392(17) 0.2096(19) -0.0203(8) 0.072(4) Uani 1 d . . H5 H 0.2350(17) 0.1599(19) -0.0535(8) 0.107 Uiso 1 d R . C6 C 0.0730(12) 0.0261(16) 0.0724(6) 0.045(3) Uani 1 d . . C7 C -0.1893(14) 0.0164(13) 0.1845(7) 0.048(3) Uani 1 d . . O6 O 0.0746(11) -0.0781(10) 0.0611(5) 0.066(3) Uani 1 d . . O7 O -0.2449(11) -0.0569(10) 0.1718(6) 0.075(3) Uani 1 d . . C1' C -0.3691(14) 0.3274(15) -0.0117(6) 0.062(4) Uani 1 d . . H1'1 H -0.4681(14) 0.3637(15) -0.0219(6) 0.093 Uiso 1 d R . H1'2 H -0.3366(14) 0.2327(15) -0.0154(6) 0.093 Uiso 1 d R . H1'3 H -0.3035(14) 0.3766(15) -0.0456(6) 0.093 Uiso 1 d R . C2' C -0.2360(12) 0.3150(11) 0.0811(6) 0.035(3) Uani 1 d . . C3' C -0.2300(11) 0.3271(11) 0.1508(5) 0.034(3) Uani 1 d . . H3' H -0.3123(11) 0.3355(11) 0.1877(5) 0.051 Uiso 1 calc R . C4' C -0.0853(11) 0.3252(11) 0.1597(6) 0.034(3) Uani 1 d . . C5' C -0.0611(14) 0.4156(12) 0.2009(6) 0.041(3) Uani 1 d . . C6' C -0.1723(17) 0.5908(15) 0.2683(9) 0.080(5) Uani 1 d . . H6'1 H -0.1747(17) 0.5460(15) 0.3178(9) 0.120 Uiso 1 d R . H6'2 H -0.2527(17) 0.6713(15) 0.2651(9) 0.120 Uiso 1 d R . H6'3 H -0.0796(17) 0.6157(15) 0.2498(9) 0.120 Uiso 1 d R . O1' O -0.3680(8) 0.3416(9) 0.0613(4) 0.050(2) Uani 1 d . . O2' O -0.1185(8) 0.2843(7) 0.0358(4) 0.037(2) Uani 1 d . . O5' O 0.0603(9) 0.4179(9) 0.2106(5) 0.059(2) Uani 1 d . . O6' O -0.1865(9) 0.5006(8) 0.2268(5) 0.053(2) Uani 1 d . . C11 C 0.2319(12) -0.0846(13) 0.2020(6) 0.041(3) Uani 1 d . . C12 C 0.1684(15) -0.1925(13) 0.2066(6) 0.049(3) Uani 1 d . . H12 H 0.0658(15) -0.1766(13) 0.2127(6) 0.074 Uiso 1 d R . C13 C 0.2559(16) -0.3220(14) 0.2027(7) 0.059(4) Uani 1 d . . H13 H 0.2134(16) -0.3944(14) 0.2082(7) 0.089 Uiso 1 d R . C14 C 0.4068(19) -0.3431(16) 0.1902(8) 0.076(5) Uani 1 d . . H14 H 0.4655(19) -0.4300(16) 0.1856(8) 0.114 Uiso 1 d R . C15 C 0.4747(16) -0.2399(19) 0.1846(8) 0.074(5) Uani 1 d . . H15 H 0.5777(16) -0.2569(19) 0.1760(8) 0.112 Uiso 1 d R . C16 C 0.3864(13) -0.1109(15) 0.1917(6) 0.055(4) Uani 1 d . . H16 H 0.4306(13) -0.0410(15) 0.1895(6) 0.082 Uiso 1 d R . C21 C -0.2144(13) 0.2172(13) 0.4598(6) 0.045(3) Uani 1 d . . C22 C -0.2989(17) 0.3364(17) 0.4824(8) 0.073(5) Uani 1 d . . H22 H -0.3130(17) 0.4183(17) 0.4496(8) 0.109 Uiso 1 d R . C23 C -0.3630(20) 0.3328(24) 0.5547(9) 0.108(7) Uani 1 d . . H23 H -0.4205(20) 0.4130(24) 0.5700(9) 0.162 Uiso 1 d R . C24 C -0.3438(20) 0.2173(26) 0.6027(8) 0.098(7) Uani 1 d . . H24 H -0.3869(20) 0.2178(26) 0.6509(8) 0.146 Uiso 1 d R . C25 C -0.2636(21) 0.1003(21) 0.5817(8) 0.087(5) Uani 1 d . . H25 H -0.2517(21) 0.0195(21) 0.6155(8) 0.130 Uiso 1 d R . C26 C -0.1969(16) 0.0988(15) 0.5085(7) 0.063(4) Uani 1 d . . H26 H -0.1413(16) 0.0174(15) 0.4938(7) 0.094 Uiso 1 d R . C31 C -0.2196(14) -0.0326(13) 0.3732(6) 0.046(3) Uani 1 d . . C32 C -0.3399(16) -0.0682(15) 0.4207(8) 0.069(4) Uani 1 d . . H32 H -0.4327(16) -0.0068(15) 0.4222(8) 0.103 Uiso 1 d R . C33 C -0.3241(19) -0.1944(18) 0.4663(9) 0.081(5) Uani 1 d . . H33 H -0.4044(19) -0.2157(18) 0.5002(9) 0.121 Uiso 1 d R . C34 C -0.1884(20) -0.2884(17) 0.4608(9) 0.086(5) Uani 1 d . . H34 H -0.1789(20) -0.3757(17) 0.4884(9) 0.129 Uiso 1 d R . C35 C -0.0681(19) -0.2531(14) 0.4149(8) 0.076(5) Uani 1 d . . H35 H 0.0244(19) -0.3148(14) 0.4141(8) 0.114 Uiso 1 d R . C36 C -0.0825(15) -0.1268(14) 0.3698(7) 0.059(4) Uani 1 d . . H36 H -0.0007(15) -0.1053(14) 0.3372(7) 0.089 Uiso 1 d R . C41 C -0.4222(12) 0.2213(12) 0.3234(6) 0.037(3) Uani 1 d . . C42 C -0.4795(15) 0.3486(14) 0.3426(7) 0.055(4) Uani 1 d . . H42 H -0.4196(15) 0.3914(14) 0.3560(7) 0.082 Uiso 1 d R . C43 C -0.6304(15) 0.4125(15) 0.3418(8) 0.067(4) Uani 1 d . . H43 H -0.6692(15) 0.4992(15) 0.3532(8) 0.101 Uiso 1 d R . C44 C -0.7195(15) 0.3509(17) 0.3243(8) 0.063(4) Uani 1 d . . H44 H -0.8205(15) 0.3923(17) 0.3273(8) 0.095 Uiso 1 d R . C45 C -0.6642(15) 0.2313(18) 0.3036(8) 0.070(4) Uani 1 d . . H45 H -0.7265(15) 0.1914(18) 0.2899(8) 0.105 Uiso 1 d R . C46 C -0.5145(13) 0.1649(14) 0.3012(7) 0.055(4) Uani 1 d . . H46 H -0.4771(13) 0.0824(14) 0.2849(7) 0.082 Uiso 1 d R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0276(3) 0.0405(3) 0.0328(3) 0.0006(2) -0.0020(2) -0.0097(2) Co1 0.0298(8) 0.0357(9) 0.0303(9) -0.0034(7) -0.0043(7) -0.0125(7) P1 0.035(2) 0.049(2) 0.030(2) -0.0049(15) -0.0052(13) -0.0164(15) S1 0.036(2) 0.043(2) 0.040(2) -0.0017(14) -0.0108(13) -0.0142(14) S2 0.052(2) 0.064(2) 0.042(2) -0.008(2) -0.011(2) -0.029(2) C1 0.054(10) 0.108(15) 0.063(11) 0.049(10) -0.007(8) -0.043(10) C2 0.055(10) 0.057(10) 0.089(13) -0.002(9) 0.016(9) -0.029(8) C3 0.038(8) 0.097(13) 0.077(11) 0.001(11) 0.003(8) -0.032(9) C4 0.039(8) 0.085(12) 0.043(9) 0.009(8) 0.011(7) -0.016(8) C5 0.078(11) 0.085(13) 0.054(10) -0.016(9) 0.018(9) -0.044(10) C6 0.027(6) 0.086(11) 0.014(6) -0.008(7) -0.009(5) 0.003(7) C7 0.052(8) 0.052(8) 0.048(8) -0.016(7) -0.007(6) -0.023(7) O6 0.088(8) 0.049(6) 0.059(6) -0.020(5) -0.027(5) 0.003(6) O7 0.078(7) 0.074(7) 0.096(8) -0.037(6) -0.013(6) -0.039(6) C1' 0.051(8) 0.101(12) 0.043(8) -0.015(8) -0.019(7) -0.023(8) C2' 0.031(7) 0.031(7) 0.039(7) 0.000(5) -0.008(6) -0.005(5) C3' 0.033(6) 0.049(7) 0.016(6) 0.000(5) -0.001(5) -0.012(6) C4' 0.031(6) 0.032(7) 0.037(7) -0.002(5) -0.001(5) -0.009(5) C5' 0.046(8) 0.033(7) 0.039(7) -0.004(6) -0.010(6) -0.004(6) C6' 0.090(12) 0.062(10) 0.098(13) -0.047(9) -0.026(10) 0.001(9) O1' 0.034(5) 0.073(6) 0.043(5) -0.010(4) -0.006(4) -0.017(4) O2' 0.033(4) 0.043(5) 0.029(4) -0.005(4) 0.003(4) -0.009(4) O5' 0.045(6) 0.060(6) 0.081(7) -0.017(5) -0.020(5) -0.016(5) O6' 0.059(6) 0.041(5) 0.065(6) -0.026(5) -0.018(5) -0.004(4) C11 0.033(7) 0.061(9) 0.022(6) 0.002(6) -0.004(5) -0.009(6) C12 0.057(8) 0.055(9) 0.035(7) 0.005(6) -0.011(6) -0.020(7) C13 0.062(10) 0.042(9) 0.057(9) -0.005(7) -0.006(7) 0.007(7) C14 0.087(13) 0.051(10) 0.063(10) -0.005(8) -0.009(9) 0.015(9) C15 0.047(9) 0.096(13) 0.054(10) 0.006(9) -0.011(7) 0.009(10) C16 0.030(7) 0.079(11) 0.039(8) 0.005(7) -0.009(6) 0.000(7) C21 0.043(7) 0.056(9) 0.039(7) -0.012(7) -0.001(6) -0.018(7) C22 0.084(11) 0.085(12) 0.060(10) -0.036(9) -0.038(9) 0.000(9) C23 0.112(15) 0.168(21) 0.051(12) -0.063(13) -0.030(11) 0.002(14) C24 0.084(13) 0.178(22) 0.026(9) -0.027(12) -0.007(9) -0.021(13) C25 0.114(15) 0.124(16) 0.041(10) -0.011(10) -0.011(10) -0.061(13) C26 0.077(10) 0.070(10) 0.051(9) -0.010(8) -0.019(8) -0.028(8) C31 0.049(8) 0.057(8) 0.034(7) -0.004(6) -0.003(6) -0.024(7) C32 0.069(10) 0.065(10) 0.069(10) 0.011(8) -0.012(8) -0.033(8) C33 0.074(11) 0.094(13) 0.073(11) 0.012(10) -0.006(9) -0.046(10) C34 0.097(14) 0.068(12) 0.086(13) 0.021(10) -0.021(11) -0.037(11) C35 0.101(13) 0.047(9) 0.066(10) 0.006(8) -0.005(9) -0.018(9) C36 0.058(9) 0.074(10) 0.041(8) -0.004(7) 0.007(7) -0.027(8) C41 0.036(7) 0.053(8) 0.025(6) -0.011(6) -0.001(5) -0.016(6) C42 0.062(9) 0.056(9) 0.047(9) -0.013(7) -0.016(7) -0.009(7) C43 0.057(10) 0.063(10) 0.078(11) -0.010(8) -0.022(8) -0.003(8) C44 0.045(8) 0.078(11) 0.066(10) -0.004(9) -0.022(7) -0.011(8) C45 0.050(9) 0.092(13) 0.082(11) -0.008(10) -0.026(8) -0.033(9) C46 0.044(8) 0.071(10) 0.064(9) -0.023(8) -0.009(7) -0.030(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C6 1.98(2) . ? W1 C4' 2.140(11) . ? W1 O2' 2.163(7) . ? W1 C4 2.254(12) . ? W1 C5 2.296(13) . ? W1 C3 2.293(13) . ? W1 C2 2.348(13) . ? W1 C1 2.361(12) . ? W1 S1 2.443(3) . ? W1 Co1 2.598(2) . ? Co1 C7 1.749(13) . ? Co1 C4' 1.973(10) . ? Co1 C3' 2.055(11) . ? Co1 P1 2.202(3) . ? Co1 S1 2.244(3) . ? P1 C41 1.823(11) . ? P1 C31 1.834(12) . ? P1 S2 2.118(4) . ? S1 C11 1.788(12) . ? S2 C21 1.793(12) . ? C1 C5 1.39(2) . ? C1 C2 1.40(2) . ? C2 C3 1.38(2) . ? C3 C4 1.40(2) . ? C4 C5 1.43(2) . ? C6 O6 1.153(15) . ? C7 O7 1.145(13) . ? C1' O1' 1.458(13) . ? C2' O2' 1.265(12) . ? C2' O1' 1.337(12) . ? C2' C3' 1.400(15) . ? C3' C4' 1.427(14) . ? C4' C5' 1.47(2) . ? C5' O5' 1.225(13) . ? C5' O6' 1.337(13) . ? C6' O6' 1.425(15) . ? C11 C16 1.40(2) . ? C11 C12 1.40(2) . ? C12 C13 1.38(2) . ? C13 C14 1.37(2) . ? C14 C15 1.38(2) . ? C15 C16 1.38(2) . ? C21 C26 1.36(2) . ? C21 C22 1.38(2) . ? C22 C23 1.39(2) . ? C23 C24 1.33(3) . ? C24 C25 1.34(2) . ? C25 C26 1.42(2) . ? C31 C32 1.38(2) . ? C31 C36 1.39(2) . ? C32 C33 1.39(2) . ? C33 C34 1.38(2) . ? C34 C35 1.36(2) . ? C35 C36 1.38(2) . ? C41 C46 1.38(2) . ? C41 C42 1.38(2) . ? C42 C43 1.40(2) . ? C43 C44 1.34(2) . ? C44 C45 1.32(2) . ? C45 C46 1.39(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 C6 W1 C4' 126.0(4) . . ? C6 W1 O2' 85.7(4) . . ? C4' W1 O2' 75.6(3) . . ? C6 W1 C4 88.1(6) . . ? C4' W1 C4 141.4(5) . . ? O2' W1 C4 130.4(4) . . ? C6 W1 C5 83.8(5) . . ? C4' W1 C5 146.3(5) . . ? O2' W1 C5 93.8(5) . . ? C4 W1 C5 36.6(5) . . ? C6 W1 C3 122.1(6) . . ? C4' W1 C3 105.8(5) . . ? O2' W1 C3 135.6(5) . . ? C4 W1 C3 35.9(5) . . ? C5 W1 C3 60.0(6) . . ? C6 W1 C2 141.8(5) . . ? C4' W1 C2 91.9(5) . . ? O2' W1 C2 102.0(5) . . ? C4 W1 C2 58.3(5) . . ? C5 W1 C2 58.6(6) . . ? C3 W1 C2 34.5(5) . . ? C6 W1 C1 114.1(7) . . ? C4' W1 C1 111.7(6) . . ? O2' W1 C1 79.9(4) . . ? C4 W1 C1 58.3(5) . . ? C5 W1 C1 34.7(5) . . ? C3 W1 C1 57.9(5) . . ? C2 W1 C1 34.6(5) . . ? C6 W1 S1 84.8(3) . . ? C4' W1 S1 75.7(3) . . ? O2' W1 S1 135.8(2) . . ? C4 W1 S1 92.2(4) . . ? C5 W1 S1 127.7(5) . . ? C3 W1 S1 84.5(4) . . ? C2 W1 S1 111.8(5) . . ? C1 W1 S1 142.5(4) . . ? C6 W1 Co1 80.1(3) . . ? C4' W1 Co1 48.0(3) . . ? O2' W1 Co1 83.1(2) . . ? C4 W1 Co1 143.7(4) . . ? C5 W1 Co1 163.8(4) . . ? C3 W1 Co1 131.6(4) . . ? C2 W1 Co1 137.6(4) . . ? C1 W1 Co1 156.7(5) . . ? S1 W1 Co1 52.76(8) . . ? C7 Co1 C4' 143.0(5) . . ? C7 Co1 C3' 107.5(5) . . ? C4' Co1 C3' 41.4(4) . . ? C7 Co1 P1 96.0(4) . . ? C4' Co1 P1 108.6(3) . . ? C3' Co1 P1 102.3(3) . . ? C7 Co1 S1 117.9(4) . . ? C4' Co1 S1 83.8(3) . . ? C3' Co1 S1 124.7(3) . . ? P1 Co1 S1 102.69(12) . . ? C7 Co1 W1 109.0(4) . . ? C4' Co1 W1 53.8(3) . . ? C3' Co1 W1 76.9(3) . . ? P1 Co1 W1 154.12(10) . . ? S1 Co1 W1 60.07(8) . . ? C41 P1 C31 104.5(5) . . ? C41 P1 S2 108.3(4) . . ? C31 P1 S2 101.7(4) . . ? C41 P1 Co1 112.3(4) . . ? C31 P1 Co1 118.7(4) . . ? S2 P1 Co1 110.4(2) . . ? C11 S1 Co1 118.9(4) . . ? C11 S1 W1 109.5(4) . . ? Co1 S1 W1 67.16(9) . . ? C21 S2 P1 108.3(4) . . ? C5 C1 C2 109.2(14) . . ? C5 C1 W1 70.1(8) . . ? C2 C1 W1 72.2(8) . . ? C3 C2 C1 108.6(15) . . ? C3 C2 W1 70.6(8) . . ? C1 C2 W1 73.2(8) . . ? C2 C3 C4 107.8(15) . . ? C2 C3 W1 74.9(8) . . ? C4 C3 W1 70.5(8) . . ? C3 C4 C5 108.4(14) . . ? C3 C4 W1 73.6(8) . . ? C5 C4 W1 73.3(8) . . ? C1 C5 C4 106.0(15) . . ? C1 C5 W1 75.2(8) . . ? C4 C5 W1 70.1(7) . . ? O6 C6 W1 177.4(10) . . ? O7 C7 Co1 174.6(12) . . ? O2' C2' O1' 119.5(10) . . ? O2' C2' C3' 121.0(10) . . ? O1' C2' C3' 119.4(10) . . ? C2' C3' C4' 113.4(9) . . ? C2' C3' Co1 107.5(8) . . ? C4' C3' Co1 66.2(6) . . ? C3' C4' C5' 122.2(10) . . ? C3' C4' Co1 72.4(6) . . ? C5' C4' Co1 125.3(8) . . ? C3' C4' W1 108.5(8) . . ? C5' C4' W1 128.1(8) . . ? Co1 C4' W1 78.2(4) . . ? O5' C5' O6' 121.7(11) . . ? O5' C5' C4' 125.0(11) . . ? O6' C5' C4' 113.3(10) . . ? C2' O1' C1' 117.6(9) . . ? C2' O2' W1 111.5(7) . . ? C5' O6' C6' 116.7(10) . . ? C16 C11 C12 118.4(12) . . ? C16 C11 S1 118.2(10) . . ? C12 C11 S1 123.3(9) . . ? C13 C12 C11 120.8(13) . . ? C14 C13 C12 119.1(14) . . ? C13 C14 C15 122.2(14) . . ? C14 C15 C16 118.7(14) . . ? C15 C16 C11 120.7(14) . . ? C26 C21 C22 119.3(13) . . ? C26 C21 S2 122.0(11) . . ? C22 C21 S2 118.6(11) . . ? C21 C22 C23 119.3(16) . . ? C24 C23 C22 121.5(18) . . ? C23 C24 C25 120.3(16) . . ? C24 C25 C26 120.3(17) . . ? C21 C26 C25 119.4(15) . . ? C32 C31 C36 119.0(12) . . ? C32 C31 P1 124.5(11) . . ? C36 C31 P1 116.5(9) . . ? C31 C32 C33 120.8(14) . . ? C34 C33 C32 119.5(14) . . ? C35 C34 C33 119.9(15) . . ? C34 C35 C36 120.7(15) . . ? C35 C36 C31 119.9(13) . . ? C46 C41 C42 118.5(12) . . ? C46 C41 P1 117.6(10) . . ? C42 C41 P1 123.4(9) . . ? C41 C42 C43 118.9(13) . . ? C44 C43 C42 121.1(14) . . ? C45 C44 C43 120.2(14) . . ? C44 C45 C46 121.3(13) . . ? C41 C46 C45 119.9(13) . . ? _refine_diff_density_max 1.270 _refine_diff_density_min -1.307 _refine_diff_density_rms 0.146