# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _publ_contact_author_email ADW24@CUS.CAM.AC.UK _publ_contact_author_name 'Dr Anthony David Woods' _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UNITED KINGDOM ; _publ_section_title ; Synthesis of cobalt-containing cyclophanes, and the formation of an unprecedented seven-membered cyclic diyne ; loop_ _publ_author_name 'Anthony David Woods' 'Vladimir B. Golovko' 'Louisa J. Hope-Weeks' 'Martin J. Mays' 'M. McPartlin' ; A.M.Sloan ; data_comp2 _database_code_depnum_ccdc_archive 'CCDC 168438' _chemical_name_common 'C22 H10 Co4 O12' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H10 Co4 O12' _chemical_formula_weight 702.02 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.369(2) _cell_length_b 16.409(2) _cell_length_c 16.632(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2556.9(7) _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 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 2.611 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_max 1.032 _exptl_absorpt_correction_T_min 0.968 _exptl_absorpt_process_details ; Sortav Blessing (1995) multi-scan from symmetry-related measurements (Blessing 1995) ; _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_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_reflns_number 9560 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5431 _reflns_number_gt 4544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'teXsan SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0124P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(18) _refine_ls_number_reflns 5431 _refine_ls_number_parameters 345 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.11889(7) 0.02926(3) 0.60711(3) 0.03018(15) Uani 1 1 d . . . Co2 Co 0.94847(7) 0.14357(3) 0.60330(3) 0.02808(15) Uani 1 1 d . . . Co3 Co 1.24874(7) 0.27805(3) 0.76566(3) 0.02930(15) Uani 1 1 d . . . Co4 Co 1.38426(7) 0.15075(3) 0.78306(3) 0.02739(15) Uani 1 1 d . . . C103 C 1.2368(6) 0.0692(3) 0.5281(3) 0.0398(12) Uani 1 1 d . . . O103 O 1.3066(5) 0.0976(2) 0.4801(2) 0.0571(11) Uani 1 1 d . . . C102 C 1.0169(6) -0.0508(3) 0.5574(3) 0.0409(12) Uani 1 1 d . . . O102 O 0.9562(4) -0.10138(19) 0.5260(2) 0.0575(11) Uani 1 1 d . . . C101 C 1.2431(6) -0.0346(3) 0.6600(3) 0.0416(12) Uani 1 1 d . . . O101 O 1.3233(5) -0.0752(2) 0.6922(2) 0.0662(12) Uani 1 1 d . . . C203 C 0.8226(6) 0.0915(3) 0.5370(3) 0.0368(11) Uani 1 1 d . . . O203 O 0.7486(4) 0.05721(19) 0.4954(2) 0.0540(10) Uani 1 1 d . . . C202 C 1.0402(6) 0.2187(3) 0.5413(3) 0.0410(12) Uani 1 1 d . . . O202 O 1.1053(5) 0.2667(2) 0.5082(2) 0.0661(12) Uani 1 1 d . . . C201 C 0.8206(5) 0.2078(3) 0.6543(3) 0.0341(11) Uani 1 1 d . . . O201 O 0.7386(4) 0.24615(18) 0.6862(2) 0.0495(9) Uani 1 1 d . . . C303 C 1.3584(6) 0.3136(2) 0.6829(3) 0.0401(13) Uani 1 1 d U . . O303 O 1.4287(5) 0.33183(19) 0.6300(2) 0.0628(12) Uani 1 1 d . . . C302 C 1.3064(5) 0.3399(3) 0.8507(3) 0.0398(12) Uani 1 1 d . . . O302 O 1.3414(5) 0.3790(2) 0.9037(2) 0.0650(12) Uani 1 1 d . . . C301 C 1.0829(6) 0.3287(2) 0.7422(3) 0.0431(13) Uani 1 1 d . . . O301 O 0.9785(4) 0.35831(18) 0.7254(3) 0.0694(12) Uani 1 1 d . . . C403 C 1.5134(6) 0.2027(3) 0.8451(3) 0.0393(12) Uani 1 1 d . . . O403 O 1.5968(4) 0.2362(2) 0.8819(2) 0.0539(10) Uani 1 1 d . . . C402 C 1.4723(5) 0.1299(3) 0.6880(3) 0.0343(11) Uani 1 1 d . . . O402 O 1.5206(4) 0.1119(2) 0.6280(2) 0.0512(9) Uani 1 1 d . . . C401 C 1.4014(5) 0.0532(3) 0.8304(3) 0.0356(11) Uani 1 1 d . . . O401 O 1.4172(4) -0.00735(18) 0.8627(2) 0.0538(10) Uani 1 1 d . . . C5 C 1.0775(5) 0.1411(2) 0.8741(2) 0.0284(10) Uani 1 1 d . . . C4 C 1.1833(5) 0.1748(2) 0.8143(2) 0.0243(9) Uani 1 1 d . . . C3 C 1.1952(5) 0.1674(2) 0.7344(2) 0.0246(9) Uani 1 1 d . . . C2 C 1.1071(5) 0.1236(2) 0.6782(2) 0.0231(9) Uani 1 1 d . . . C1 C 0.9960(5) 0.0726(2) 0.6940(2) 0.0258(10) Uani 1 1 d . . . C9 C 0.9307(5) 0.0489(2) 0.7713(2) 0.0262(9) Uani 1 1 d . . . C8 C 1.0277(5) 0.0538(2) 0.8454(2) 0.0298(11) Uani 1 1 d . . . H8B H 1.1142 0.0211 0.8343 0.036 Uiso 1 1 calc R . . H8A H 0.9772 0.0274 0.8908 0.036 Uiso 1 1 calc R . . C6 C 0.9479(5) 0.1973(2) 0.8798(3) 0.0380(11) Uani 1 1 d . . . H6C H 0.8786 0.1743 0.9176 0.057 Uiso 1 1 calc R . . H6B H 0.9038 0.2026 0.8266 0.057 Uiso 1 1 calc R . . H6A H 0.9782 0.2512 0.8987 0.057 Uiso 1 1 calc R . . C7 C 1.1459(6) 0.1320(3) 0.9578(2) 0.0406(12) Uani 1 1 d . . . H7C H 1.0737 0.1133 0.9963 0.061 Uiso 1 1 calc R . . H7B H 1.1839 0.1847 0.9753 0.061 Uiso 1 1 calc R . . H7A H 1.2236 0.0921 0.9552 0.061 Uiso 1 1 calc R . . C10 C 0.7954(5) 0.0270(2) 0.7776(3) 0.0368(11) Uani 1 1 d . . . H10B H 0.7362 0.0261 0.7312 0.055 Uiso 1 1 calc R . . H10A H 0.7573 0.0122 0.8285 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0356(4) 0.0304(3) 0.0246(3) -0.0043(2) 0.0041(3) -0.0008(3) Co2 0.0301(3) 0.0319(3) 0.0222(3) 0.0022(2) -0.0026(3) -0.0030(3) Co3 0.0304(4) 0.0272(3) 0.0302(3) -0.0016(2) -0.0043(3) -0.0004(3) Co4 0.0244(3) 0.0330(3) 0.0247(3) 0.0011(2) -0.0007(3) 0.0023(3) C103 0.047(4) 0.039(3) 0.033(3) -0.010(2) -0.003(3) 0.002(3) O103 0.063(3) 0.072(2) 0.036(2) -0.0042(17) 0.023(2) -0.023(2) C102 0.046(3) 0.038(3) 0.039(3) 0.000(2) 0.017(2) -0.002(2) O102 0.063(3) 0.0427(19) 0.067(2) -0.0180(16) 0.003(2) -0.020(2) C101 0.047(4) 0.034(3) 0.044(3) -0.008(2) 0.009(3) 0.004(3) O101 0.075(3) 0.054(2) 0.070(3) -0.0035(18) -0.007(3) 0.025(2) C203 0.040(3) 0.042(3) 0.029(2) -0.002(2) 0.000(2) 0.000(2) O203 0.052(3) 0.059(2) 0.050(2) -0.0145(17) -0.016(2) -0.011(2) C202 0.045(3) 0.044(3) 0.034(3) 0.008(2) 0.000(3) -0.003(3) O202 0.073(3) 0.063(2) 0.062(2) 0.0283(18) 0.011(2) -0.017(2) C201 0.028(3) 0.036(3) 0.038(3) 0.0022(19) -0.008(2) -0.003(2) O201 0.036(2) 0.052(2) 0.061(2) -0.0129(16) 0.0004(19) 0.0035(19) C303 0.054(4) 0.027(2) 0.039(3) 0.004(2) -0.006(3) -0.004(2) O303 0.085(3) 0.060(2) 0.044(2) 0.0143(16) 0.008(2) -0.012(2) C302 0.033(3) 0.045(3) 0.041(3) -0.009(2) -0.005(2) 0.006(2) O302 0.063(3) 0.069(2) 0.063(3) -0.0346(19) -0.018(2) 0.007(2) C301 0.040(3) 0.026(2) 0.063(3) -0.004(2) -0.014(3) -0.001(2) O301 0.044(3) 0.0309(17) 0.133(4) -0.002(2) -0.034(3) -0.0005(18) C403 0.034(3) 0.048(3) 0.036(3) -0.003(2) -0.007(2) 0.008(3) O403 0.041(2) 0.065(2) 0.056(2) -0.0154(17) -0.019(2) 0.002(2) C402 0.031(3) 0.034(2) 0.039(3) 0.0005(19) -0.002(2) -0.005(2) O402 0.047(2) 0.071(2) 0.035(2) -0.0106(16) 0.0115(18) -0.002(2) C401 0.030(3) 0.045(3) 0.032(3) 0.0013(19) 0.003(2) 0.011(2) O401 0.060(3) 0.0477(19) 0.054(2) 0.0191(16) 0.003(2) 0.013(2) C5 0.022(2) 0.041(2) 0.022(2) -0.0006(17) 0.0006(17) 0.004(2) C4 0.021(2) 0.029(2) 0.024(2) 0.0005(16) 0.0001(18) 0.0038(18) C3 0.021(2) 0.022(2) 0.031(2) 0.0013(16) 0.0015(19) 0.0008(17) C2 0.021(2) 0.027(2) 0.022(2) -0.0006(15) -0.0015(18) 0.0027(19) C1 0.031(3) 0.026(2) 0.020(2) -0.0023(16) -0.0006(19) 0.004(2) C9 0.027(2) 0.0236(19) 0.028(2) 0.0033(16) -0.002(2) 0.0011(19) C8 0.031(3) 0.032(2) 0.026(2) 0.0079(17) 0.002(2) 0.002(2) C6 0.035(3) 0.041(2) 0.038(3) -0.0048(19) 0.008(2) 0.010(2) C7 0.037(3) 0.057(3) 0.028(2) -0.001(2) 0.004(2) 0.004(3) C10 0.033(3) 0.041(2) 0.036(3) 0.006(2) 0.003(2) -0.006(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 Co1 C101 1.796(6) . ? Co1 C102 1.823(5) . ? Co1 C103 1.838(5) . ? Co1 C2 1.952(4) . ? Co1 C1 1.980(4) . ? Co1 Co2 2.4640(9) . ? Co2 C201 1.808(5) . ? Co2 C202 1.823(5) . ? Co2 C203 1.827(5) . ? Co2 C1 1.957(4) . ? Co2 C2 1.967(4) . ? Co3 C301 1.804(5) . ? Co3 C303 1.814(5) . ? Co3 C302 1.823(5) . ? Co3 C3 1.955(4) . ? Co3 C4 1.974(4) . ? Co3 Co4 2.4617(8) . ? Co4 C401 1.791(5) . ? Co4 C403 1.804(5) . ? Co4 C402 1.815(5) . ? Co4 C3 1.966(4) . ? Co4 C4 1.993(4) . ? C103 O103 1.132(6) . ? C102 O102 1.133(5) . ? C101 O101 1.138(6) . ? C203 O203 1.129(5) . ? C202 O202 1.138(5) . ? C201 O201 1.125(5) . ? C303 O303 1.139(6) . ? C302 O302 1.138(5) . ? C301 O301 1.128(6) . ? C403 O403 1.135(5) . ? C402 O402 1.136(5) . ? C401 O401 1.139(5) . ? C5 C4 1.510(6) . ? C5 C6 1.528(6) . ? C5 C7 1.540(6) . ? C5 C8 1.581(6) . ? C4 C3 1.338(5) . ? C3 C2 1.439(6) . ? C2 C1 1.362(6) . ? C1 C9 1.476(6) . ? C9 C10 1.322(6) . ? C9 C8 1.533(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C101 Co1 C102 98.1(2) . . ? C101 Co1 C103 99.7(2) . . ? C102 Co1 C103 104.35(19) . . ? C101 Co1 C2 101.69(18) . . ? C102 Co1 C2 144.8(2) . . ? C103 Co1 C2 100.64(18) . . ? C101 Co1 C1 103.25(18) . . ? C102 Co1 C1 106.56(19) . . ? C103 Co1 C1 138.02(18) . . ? C2 Co1 C1 40.51(17) . . ? C101 Co1 Co2 151.23(14) . . ? C102 Co1 Co2 101.39(16) . . ? C103 Co1 Co2 95.72(15) . . ? C2 Co1 Co2 51.32(13) . . ? C1 Co1 Co2 50.83(11) . . ? C201 Co2 C202 100.6(2) . . ? C201 Co2 C203 97.4(2) . . ? C202 Co2 C203 106.2(2) . . ? C201 Co2 C1 97.80(18) . . ? C202 Co2 C1 137.0(2) . . ? C203 Co2 C1 109.54(19) . . ? C201 Co2 C2 107.48(18) . . ? C202 Co2 C2 96.6(2) . . ? C203 Co2 C2 142.45(18) . . ? C1 Co2 C2 40.60(17) . . ? C201 Co2 Co1 149.48(14) . . ? C202 Co2 Co1 102.94(17) . . ? C203 Co2 Co1 94.48(15) . . ? C1 Co2 Co1 51.68(12) . . ? C2 Co2 Co1 50.77(11) . . ? C301 Co3 C303 100.1(2) . . ? C301 Co3 C302 99.6(2) . . ? C303 Co3 C302 104.0(2) . . ? C301 Co3 C3 98.63(19) . . ? C303 Co3 C3 104.06(17) . . ? C302 Co3 C3 143.09(19) . . ? C301 Co3 C4 102.49(19) . . ? C303 Co3 C4 139.71(18) . . ? C302 Co3 C4 104.58(19) . . ? C3 Co3 C4 39.83(15) . . ? C301 Co3 Co4 149.36(14) . . ? C303 Co3 Co4 94.02(15) . . ? C302 Co3 Co4 103.20(15) . . ? C3 Co3 Co4 51.31(12) . . ? C4 Co3 Co4 51.98(12) . . ? C401 Co4 C403 96.4(2) . . ? C401 Co4 C402 100.03(19) . . ? C403 Co4 C402 106.4(2) . . ? C401 Co4 C3 112.7(2) . . ? C403 Co4 C3 140.68(18) . . ? C402 Co4 C3 94.43(19) . . ? C401 Co4 C4 98.46(19) . . ? C403 Co4 C4 112.98(19) . . ? C402 Co4 C4 133.92(19) . . ? C3 Co4 C4 39.51(15) . . ? C401 Co4 Co3 148.89(15) . . ? C403 Co4 Co3 90.67(15) . . ? C402 Co4 Co3 106.96(14) . . ? C3 Co4 Co3 50.90(10) . . ? C4 Co4 Co3 51.31(11) . . ? O103 C103 Co1 176.5(4) . . ? O102 C102 Co1 178.5(5) . . ? O101 C101 Co1 178.7(5) . . ? O203 C203 Co2 177.4(5) . . ? O202 C202 Co2 173.9(5) . . ? O201 C201 Co2 178.2(4) . . ? O303 C303 Co3 176.4(4) . . ? O302 C302 Co3 179.4(5) . . ? O301 C301 Co3 177.4(5) . . ? O403 C403 Co4 177.7(5) . . ? O402 C402 Co4 174.7(4) . . ? O401 C401 Co4 176.8(5) . . ? C4 C5 C6 110.0(3) . . ? C4 C5 C7 111.0(4) . . ? C6 C5 C7 109.5(3) . . ? C4 C5 C8 109.1(3) . . ? C6 C5 C8 109.3(4) . . ? C7 C5 C8 107.9(3) . . ? C3 C4 C5 132.5(4) . . ? C3 C4 Co3 69.3(2) . . ? C5 C4 Co3 142.0(3) . . ? C3 C4 Co4 69.2(3) . . ? C5 C4 Co4 136.0(3) . . ? Co3 C4 Co4 76.71(15) . . ? C4 C3 C2 130.0(4) . . ? C4 C3 Co3 70.9(2) . . ? C2 C3 Co3 141.5(3) . . ? C4 C3 Co4 71.3(3) . . ? C2 C3 Co4 135.6(3) . . ? Co3 C3 Co4 77.79(15) . . ? C1 C2 C3 128.3(4) . . ? C1 C2 Co1 70.9(2) . . ? C3 C2 Co1 139.2(3) . . ? C1 C2 Co2 69.3(3) . . ? C3 C2 Co2 139.7(3) . . ? Co1 C2 Co2 77.91(15) . . ? C2 C1 C9 130.3(4) . . ? C2 C1 Co2 70.1(2) . . ? C9 C1 Co2 137.2(3) . . ? C2 C1 Co1 68.6(2) . . ? C9 C1 Co1 141.4(3) . . ? Co2 C1 Co1 77.49(15) . . ? C10 C9 C1 122.5(4) . . ? C10 C9 C8 121.3(4) . . ? C1 C9 C8 116.2(4) . . ? C9 C8 C5 117.7(3) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.795 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.100 #===END data_COMPOUND_5 _database_code_depnum_ccdc_archive 'CCDC 228896' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H54 Co4 O8 P4' _chemical_formula_sum 'C68 H54 Co4 O8 P4' _chemical_formula_weight 1358.71 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.9757(2) _cell_length_b 35.2755(8) _cell_length_c 17.6562(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.167(9) _cell_angle_gamma 90.00 _cell_volume 5967.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 53547 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 1.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; The bridging 7-carbon ring system is not well defined: bond restraints and common isotropic temperature factors were applied to these atoms. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22460 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10401 _reflns_number_gt 9395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+31.5397P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 8395 _refine_ls_number_parameters 638 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_obs 0.0458 _refine_ls_wR_factor_all 0.2710 _refine_ls_wR_factor_obs 0.0997 _refine_ls_goodness_of_fit_all 1.131 _refine_ls_goodness_of_fit_obs 1.148 _refine_ls_restrained_S_all 3.012 _refine_ls_restrained_S_obs 1.157 _refine_ls_shift/esd_max 0.180 _refine_ls_shift/esd_mean 0.015 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 Co1 Co -0.88253(8) -0.60513(2) 0.99099(5) 0.0272(2) Uani 1 d . . Co2 Co -0.93821(8) -0.55587(2) 0.88690(5) 0.0248(2) Uani 1 d . . Co3 Co -1.03003(8) -0.64479(2) 0.70648(5) 0.0268(2) Uani 1 d D . Co4 Co -0.97966(8) -0.69382(2) 0.81113(5) 0.0242(2) Uani 1 d D . P1 P -0.9181(2) -0.57127(4) 1.09062(9) 0.0259(4) Uani 1 d . . P2 P -0.9052(2) -0.51000(4) 0.97662(10) 0.0242(4) Uani 1 d . . P3 P -1.1641(2) -0.67897(4) 0.60738(10) 0.0258(4) Uani 1 d . . P4 P -1.0357(2) -0.73983(4) 0.72188(10) 0.0242(4) Uani 1 d . . O102 O -0.8895(7) -0.68218(15) 1.0509(3) 0.065(2) Uani 1 d . . O101 O -0.5858(6) -0.6077(2) 0.9968(4) 0.060(2) Uani 1 d . . O202 O -1.1456(6) -0.51300(14) 0.7687(3) 0.0531(14) Uani 1 d . . O201 O -0.7131(6) -0.5653(2) 0.8114(4) 0.058(2) Uani 1 d . . O302 O -0.7407(6) -0.6422(2) 0.6989(3) 0.057(2) Uani 1 d . . O301 O -1.0963(7) -0.5677(2) 0.6469(3) 0.065(2) Uani 1 d . . O402 O -0.6798(5) -0.6838(2) 0.8845(4) 0.059(2) Uani 1 d . . O401 O -1.0647(6) -0.73676(15) 0.9307(3) 0.0557(15) Uani 1 d . . C1 C -1.0657(6) -0.5923(2) 0.9156(4) 0.0269(14) Uani 1 d . . C2 C -0.9820(6) -0.6105(2) 0.8783(3) 0.0222(13) Uani 1 d D . C3 C -1.0144(35) -0.6393(3) 0.8194(7) 0.0205(13) Uiso 0.592(8) d PD 1 C4 C -1.1371(17) -0.6570(7) 0.7833(15) 0.0276(14) Uiso 0.592(8) d PD 1 C6 C -1.3633(11) -0.6186(3) 0.7523(6) 0.034(2) Uiso 0.592(8) d PD 1 H6A H -1.3055(11) -0.5957(3) 0.7577(6) 0.051 Uiso 0.592(8) calc PR 1 H6B H -1.4433(11) -0.6136(3) 0.7728(6) 0.051 Uiso 0.592(8) calc PR 1 H6C H -1.3967(11) -0.6257(3) 0.6965(6) 0.051 Uiso 0.592(8) calc PR 1 C8 C -1.2593(11) -0.6395(2) 0.8895(5) 0.030(2) Uiso 0.592(8) d PD 1 H8A H -1.3487(11) -0.6438(2) 0.9022(5) 0.035 Uiso 0.592(8) calc PR 1 H8B H -1.1875(11) -0.6557(2) 0.9247(5) 0.035 Uiso 0.592(8) calc PR 1 C3' C -1.0125(51) -0.6393(5) 0.8195(10) 0.0205(13) Uiso 0.408(8) d PD 2 C4' C -1.1363(23) -0.6566(11) 0.7840(22) 0.0276(14) Uiso 0.408(8) d PD 2 C6' C -1.2652(16) -0.6311(4) 0.9461(9) 0.034(2) Uiso 0.408(8) d PD 2 H6'1 H -1.2097(16) -0.6536(4) 0.9427(9) 0.051 Uiso 0.408(8) calc PR 2 H6'2 H -1.3640(16) -0.6363(4) 0.9206(9) 0.051 Uiso 0.408(8) calc PR 2 H6'3 H -1.2529(16) -0.6247(4) 1.0016(9) 0.051 Uiso 0.408(8) calc PR 2 C8' C -1.2944(15) -0.6083(3) 0.8138(6) 0.030(2) Uiso 0.408(8) d PD 2 H8'1 H -1.3949(15) -0.6022(3) 0.8021(6) 0.035 Uiso 0.408(8) calc PR 2 H8'2 H -1.2546(15) -0.5931(3) 0.7782(6) 0.035 Uiso 0.408(8) calc PR 2 C5 C -1.2763(7) -0.6511(2) 0.7990(4) 0.036(2) Uiso 1 d D . C7 C -1.3660(8) -0.6841(2) 0.7892(4) 0.044(2) Uiso 1 d . . H7A H -1.4566(26) -0.6768(4) 0.7961(40) 0.065 Uiso 0.592(8) calc PR 1 H7B H -1.3226(34) -0.7033(8) 0.8286(26) 0.065 Uiso 0.592(8) calc PR 1 H7C H -1.3794(58) -0.6946(12) 0.7362(15) 0.065 Uiso 0.592(8) calc PR 1 H7D H -1.3353(29) -0.7077(5) 0.7740(39) 0.065 Uiso 0.408(8) calc PR 2 H7E H -1.4555(30) -0.6822(5) 0.7979(39) 0.065 Uiso 0.408(8) calc PR 2 C9 C -1.2167(7) -0.5976(2) 0.9043(4) 0.037(2) Uiso 1 d D . C10 C -1.3014(8) -0.5668(2) 0.9121(4) 0.043(2) Uiso 1 d . . H10A H -1.2614(8) -0.5423(2) 0.9246(4) 0.064 Uiso 0.592(8) calc PR 1 H10B H -1.3986(8) -0.5704(2) 0.9047(4) 0.064 Uiso 0.592(8) calc PR 1 H10C H -1.3085(8) -0.5657(2) 0.9663(4) 0.064 Uiso 0.408(8) calc PR 2 H10D H -1.3947(8) -0.5700(2) 0.8756(4) 0.064 Uiso 0.408(8) calc PR 2 H10E H -1.2600(8) -0.5432(2) 0.8997(4) 0.064 Uiso 0.408(8) calc PR 2 C102 C -0.8929(7) -0.6519(2) 1.0273(4) 0.036(2) Uani 1 d . . C101 C -0.7002(8) -0.6059(2) 0.9965(4) 0.040(2) Uani 1 d . . C202 C -1.0642(7) -0.5302(2) 0.8136(4) 0.035(2) Uani 1 d . . C201 C -0.7954(8) -0.5604(2) 0.8435(4) 0.037(2) Uani 1 d . . C11 C -0.9849(6) -0.5243(2) 1.0536(4) 0.0278(14) Uani 1 d . . H11B H -1.0877(6) -0.5253(2) 1.0319(4) 0.033 Uiso 1 calc R . H11A H -0.9619(6) -0.5056(2) 1.0972(4) 0.033 Uiso 1 calc R . C12 C -1.0561(4) -0.58914(12) 1.1328(3) 0.032(2) Uani 1 d G . C13 C -1.1789(5) -0.56910(13) 1.1257(3) 0.057(2) Uani 1 d G . H13 H -1.1891(8) -0.54421(15) 1.1044(5) 0.069 Uiso 1 calc R . C14 C -1.2868(4) -0.5855(2) 1.1500(4) 0.078(3) Uani 1 d G . H14 H -1.3707(5) -0.5718(2) 1.1452(5) 0.094 Uiso 1 calc R . C15 C -1.2718(6) -0.6219(2) 1.1813(3) 0.071(3) Uani 1 d G . H15 H -1.3455(7) -0.6331(2) 1.1979(5) 0.085 Uiso 1 calc R . C16 C -1.1489(7) -0.64195(12) 1.1883(3) 0.074(3) Uani 1 d G . H16 H -1.1387(10) -0.66684(14) 1.2097(5) 0.089 Uiso 1 calc R . C17 C -1.0411(5) -0.62556(12) 1.1640(3) 0.050(2) Uani 1 d G . H17 H -0.9571(6) -0.6393(2) 1.1688(5) 0.060 Uiso 1 calc R . C18 C -0.7791(4) -0.55883(12) 1.1805(2) 0.0277(15) Uani 1 d G . C19 C -0.8142(3) -0.54188(13) 1.2435(2) 0.039(2) Uani 1 d G . H19 H -0.9095(4) -0.5386(2) 1.2418(4) 0.047 Uiso 1 calc R . C20 C -0.7098(5) -0.52975(13) 1.3089(2) 0.041(2) Uani 1 d G . H20 H -0.7338(6) -0.5182(2) 1.3519(3) 0.049 Uiso 1 calc R . C21 C -0.5704(4) -0.53456(14) 1.3114(2) 0.046(2) Uani 1 d G . H21 H -0.4990(5) -0.5263(2) 1.3561(3) 0.056 Uiso 1 calc R . C22 C -0.5353(3) -0.55151(14) 1.2484(3) 0.050(2) Uani 1 d G . H22 H -0.4400(3) -0.5548(2) 1.2501(4) 0.061 Uiso 1 calc R . C23 C -0.6397(4) -0.56364(13) 1.1830(2) 0.039(2) Uani 1 d G . H23 H -0.6157(6) -0.5752(2) 1.1400(3) 0.047 Uiso 1 calc R . C24 C -0.7291(3) -0.49514(12) 1.0333(2) 0.0279(14) Uani 1 d G . C25 C -0.7117(4) -0.47124(12) 1.0979(3) 0.039(2) Uani 1 d G . H25 H -0.7909(5) -0.4619(2) 1.1119(4) 0.047 Uiso 1 calc R . C26 C -0.5783(5) -0.46097(13) 1.1421(2) 0.052(2) Uani 1 d G . H26 H -0.5664(7) -0.4446(2) 1.1863(3) 0.063 Uiso 1 calc R . C27 C -0.4623(4) -0.47459(15) 1.1217(3) 0.056(2) Uani 1 d G . H27 H -0.3712(4) -0.4676(2) 1.1519(4) 0.067 Uiso 1 calc R . C28 C -0.4797(4) -0.49850(14) 1.0571(3) 0.046(2) Uani 1 d G . H28 H -0.4004(4) -0.5078(2) 1.0431(4) 0.055 Uiso 1 calc R . C29 C -0.6131(4) -0.50877(12) 1.0129(2) 0.039(2) Uani 1 d G . H29 H -0.6250(6) -0.5251(2) 0.9687(3) 0.047 Uiso 1 calc R . C30 C -0.9925(4) -0.46414(9) 0.9446(3) 0.0292(14) Uani 1 d G . C31 C -0.9160(3) -0.43460(11) 0.9252(3) 0.040(2) Uani 1 d G . H31 H -0.8189(3) -0.4376(2) 0.9313(4) 0.048 Uiso 1 calc R . C32 C -0.9815(4) -0.40064(10) 0.8968(3) 0.050(2) Uani 1 d G . H32 H -0.9292(6) -0.38045(13) 0.8835(5) 0.061 Uiso 1 calc R . C33 C -1.1236(4) -0.39621(10) 0.8878(3) 0.040(2) Uani 1 d G . H33 H -1.1684(6) -0.37300(12) 0.8683(4) 0.048 Uiso 1 calc R . C34 C -1.2001(3) -0.42575(12) 0.9072(3) 0.045(2) Uani 1 d G . H34 H -1.2972(3) -0.4227(2) 0.9011(5) 0.054 Uiso 1 calc R . C35 C -1.1346(4) -0.45971(10) 0.9357(3) 0.044(2) Uani 1 d G . H35 H -1.1869(5) -0.47990(14) 0.9489(4) 0.052 Uiso 1 calc R . C302 C -0.8540(8) -0.6436(2) 0.6992(4) 0.035(2) Uani 1 d . . C301 C -1.0753(8) -0.5980(2) 0.6712(4) 0.040(2) Uani 1 d . . C402 C -0.7938(8) -0.6896(2) 0.8536(4) 0.037(2) Uani 1 d . . C401 C -1.0303(7) -0.7197(2) 0.8853(4) 0.0315(15) Uani 1 d . . C36 C -1.1933(6) -0.7257(2) 0.6445(4) 0.0266(14) Uani 1 d . . H36B H -1.2133(6) -0.7444(2) 0.6010(4) 0.032 Uiso 1 calc R . H36A H -1.2744(6) -0.7248(2) 0.6664(4) 0.032 Uiso 1 calc R . C37 C -1.1149(4) -0.69145(12) 0.5171(2) 0.0267(15) Uani 1 d G . C38 C -0.9777(4) -0.68701(13) 0.5147(2) 0.040(2) Uani 1 d G . H38 H -0.9110(5) -0.6756(2) 0.5578(3) 0.048 Uiso 1 calc R . C39 C -0.9382(3) -0.69931(14) 0.4493(3) 0.049(2) Uani 1 d G . H39 H -0.8445(4) -0.6963(2) 0.4476(4) 0.059 Uiso 1 calc R . C40 C -1.0359(5) -0.71605(14) 0.3863(2) 0.045(2) Uani 1 d G . H40 H -1.0089(6) -0.7245(2) 0.3415(3) 0.054 Uiso 1 calc R . C41 C -1.1731(4) -0.72049(13) 0.3887(2) 0.038(2) Uani 1 d G . H41 H -1.2399(5) -0.7319(2) 0.3457(3) 0.045 Uiso 1 calc R . C42 C -1.2126(3) -0.70819(13) 0.4542(2) 0.037(2) Uani 1 d G . H42 H -1.3064(4) -0.7112(2) 0.4558(3) 0.045 Uiso 1 calc R . C43 C -1.3442(4) -0.66143(12) 0.5656(3) 0.0302(15) Uani 1 d G . C44 C -1.3615(4) -0.62478(12) 0.5355(3) 0.044(2) Uani 1 d G . H44 H -1.2829(6) -0.6107(2) 0.5312(4) 0.053 Uiso 1 calc R . C45 C -1.4940(6) -0.60878(11) 0.5118(3) 0.067(3) Uani 1 d G . H45 H -1.5059(8) -0.58373(13) 0.4912(5) 0.081 Uiso 1 calc R . C46 C -1.6091(4) -0.6294(2) 0.5181(3) 0.065(3) Uani 1 d G . H46 H -1.6996(5) -0.6185(2) 0.5018(5) 0.079 Uiso 1 calc R . C47 C -1.5917(4) -0.6661(2) 0.5482(3) 0.065(3) Uani 1 d G . H47 H -1.6704(5) -0.6802(2) 0.5525(5) 0.078 Uiso 1 calc R . C48 C -1.4593(5) -0.68207(11) 0.5720(3) 0.050(2) Uani 1 d G . H48 H -1.4474(7) -0.70712(13) 0.5925(5) 0.061 Uiso 1 calc R . C49 C -1.0890(4) -0.78574(9) 0.7543(3) 0.0292(14) Uani 1 d G . C50 C -1.2212(4) -0.79016(11) 0.7648(3) 0.046(2) Uani 1 d G . H50 H -1.2866(5) -0.76997(14) 0.7521(5) 0.055 Uiso 1 calc R . C51 C -1.2575(4) -0.82412(12) 0.7937(3) 0.049(2) Uani 1 d G . H51 H -1.3479(5) -0.8271(2) 0.8009(5) 0.059 Uiso 1 calc R . C52 C -1.1617(5) -0.85366(10) 0.8123(3) 0.045(2) Uani 1 d G . H52 H -1.1866(7) -0.87687(12) 0.8321(4) 0.054 Uiso 1 calc R . C53 C -1.0296(4) -0.84924(10) 0.8019(3) 0.050(2) Uani 1 d G . H53 H -0.9641(6) -0.86943(13) 0.8145(5) 0.060 Uiso 1 calc R . C54 C -0.9932(4) -0.81528(11) 0.7729(3) 0.043(2) Uani 1 d G . H54 H -0.9028(4) -0.8123(2) 0.7657(4) 0.051 Uiso 1 calc R . C55 C -0.9167(4) -0.75493(12) 0.6647(2) 0.0284(14) Uani 1 d G . C56 C -0.7803(4) -0.74150(12) 0.6846(2) 0.036(2) Uani 1 d G . H56 H -0.7480(6) -0.7251(2) 0.7285(3) 0.043 Uiso 1 calc R . C57 C -0.6912(4) -0.75213(14) 0.6402(3) 0.047(2) Uani 1 d G . H57 H -0.5980(4) -0.7430(2) 0.6538(4) 0.056 Uiso 1 calc R . C58 C -0.7384(5) -0.7762(2) 0.5759(3) 0.054(2) Uani 1 d G . H58 H -0.6775(7) -0.7834(2) 0.5456(4) 0.065 Uiso 1 calc R . C59 C -0.8748(6) -0.78960(13) 0.5560(2) 0.056(2) Uani 1 d G . H59 H -0.9071(7) -0.8060(2) 0.5121(3) 0.068 Uiso 1 calc R . C60 C -0.9639(4) -0.77898(12) 0.6004(3) 0.041(2) Uani 1 d G . H60 H -1.0571(4) -0.7882(2) 0.5868(4) 0.049 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 Co1 0.0381(5) 0.0194(4) 0.0222(5) -0.0004(4) 0.0053(4) 0.0037(4) Co2 0.0317(5) 0.0189(4) 0.0237(5) -0.0003(4) 0.0076(4) 0.0008(3) Co3 0.0373(5) 0.0189(4) 0.0230(5) -0.0005(4) 0.0066(4) -0.0036(4) Co4 0.0293(5) 0.0187(4) 0.0233(5) -0.0001(4) 0.0052(4) 0.0002(3) P1 0.0335(9) 0.0212(8) 0.0223(9) 0.0000(7) 0.0070(7) 0.0009(7) P2 0.0306(9) 0.0173(8) 0.0243(9) 0.0001(7) 0.0068(7) 0.0013(6) P3 0.0325(9) 0.0199(8) 0.0231(9) -0.0009(7) 0.0044(7) -0.0023(7) P4 0.0271(9) 0.0188(8) 0.0265(9) 0.0005(7) 0.0071(7) 0.0007(6) O102 0.119(5) 0.021(3) 0.045(4) 0.007(3) 0.008(3) -0.001(3) O101 0.033(3) 0.073(4) 0.070(4) -0.008(3) 0.010(3) 0.012(3) O202 0.060(3) 0.044(3) 0.040(3) 0.005(3) -0.010(3) 0.014(3) O201 0.060(4) 0.061(4) 0.068(4) -0.015(3) 0.042(3) -0.008(3) O302 0.043(3) 0.071(4) 0.065(4) -0.006(3) 0.029(3) -0.014(3) O301 0.115(5) 0.029(3) 0.043(3) 0.010(3) 0.012(3) 0.008(3) O402 0.028(3) 0.062(4) 0.079(4) -0.012(3) 0.002(3) -0.004(2) O401 0.092(4) 0.045(3) 0.039(3) 0.007(3) 0.033(3) -0.014(3) C1 0.037(4) 0.021(3) 0.022(3) 0.009(3) 0.008(3) 0.006(3) C2 0.021(3) 0.018(3) 0.027(3) 0.005(3) 0.005(3) 0.001(2) C102 0.045(4) 0.037(4) 0.022(4) -0.007(3) 0.003(3) -0.002(3) C101 0.043(5) 0.037(4) 0.032(4) -0.006(3) -0.004(3) 0.005(3) C202 0.039(4) 0.024(3) 0.039(4) -0.002(3) 0.005(3) 0.000(3) C201 0.047(4) 0.031(4) 0.039(4) -0.006(3) 0.020(4) -0.004(3) C11 0.030(3) 0.026(3) 0.030(4) -0.005(3) 0.012(3) 0.001(3) C12 0.044(4) 0.031(4) 0.020(3) -0.002(3) 0.006(3) -0.012(3) C13 0.043(5) 0.083(6) 0.050(5) 0.028(5) 0.020(4) 0.001(4) C14 0.063(6) 0.125(10) 0.056(6) 0.022(6) 0.031(5) 0.000(6) C15 0.076(7) 0.089(8) 0.058(6) -0.017(6) 0.037(5) -0.043(6) C16 0.136(10) 0.046(5) 0.059(6) -0.014(4) 0.057(6) -0.037(6) C17 0.079(6) 0.028(4) 0.053(5) 0.003(4) 0.038(5) -0.002(4) C18 0.040(4) 0.021(3) 0.024(4) -0.002(3) 0.011(3) -0.001(3) C19 0.051(4) 0.032(4) 0.034(4) -0.008(3) 0.009(3) -0.002(3) C20 0.055(5) 0.035(4) 0.030(4) -0.006(3) 0.006(3) 0.003(3) C21 0.064(5) 0.035(4) 0.030(4) -0.001(3) -0.004(4) -0.001(3) C22 0.033(4) 0.063(5) 0.051(5) -0.002(4) 0.003(4) 0.005(4) C23 0.044(4) 0.044(4) 0.030(4) -0.001(3) 0.010(3) 0.009(3) C24 0.034(4) 0.017(3) 0.028(4) 0.004(3) 0.002(3) -0.003(3) C25 0.047(4) 0.031(4) 0.037(4) -0.002(3) 0.009(3) -0.010(3) C26 0.060(5) 0.049(5) 0.037(5) 0.001(4) -0.006(4) -0.020(4) C27 0.044(5) 0.050(5) 0.058(6) 0.007(4) -0.010(4) -0.021(4) C28 0.029(4) 0.050(5) 0.055(5) 0.017(4) 0.007(3) 0.004(3) C29 0.036(4) 0.038(4) 0.037(4) 0.010(3) 0.001(3) 0.001(3) C30 0.036(4) 0.020(3) 0.024(3) -0.002(3) -0.003(3) 0.005(3) C31 0.039(4) 0.025(4) 0.055(5) 0.009(3) 0.014(3) 0.007(3) C32 0.056(5) 0.025(4) 0.072(6) 0.018(4) 0.021(4) 0.008(3) C33 0.042(4) 0.027(4) 0.044(5) 0.003(3) 0.003(3) 0.009(3) C34 0.037(4) 0.035(4) 0.055(5) 0.000(4) -0.002(3) 0.014(3) C35 0.038(4) 0.023(3) 0.062(5) 0.002(3) 0.000(4) 0.000(3) C302 0.047(5) 0.036(4) 0.029(4) -0.005(3) 0.023(3) -0.015(3) C301 0.065(5) 0.032(4) 0.022(4) -0.011(3) 0.010(3) 0.000(3) C402 0.047(5) 0.027(4) 0.033(4) -0.001(3) 0.002(3) 0.004(3) C401 0.038(4) 0.028(3) 0.030(4) -0.002(3) 0.012(3) 0.001(3) C36 0.028(3) 0.024(3) 0.025(3) -0.006(3) 0.003(3) -0.003(2) C37 0.032(4) 0.024(3) 0.025(4) -0.002(3) 0.009(3) 0.002(3) C38 0.049(4) 0.040(4) 0.029(4) -0.002(3) 0.007(3) 0.001(3) C39 0.052(5) 0.055(5) 0.044(5) 0.000(4) 0.020(4) -0.008(4) C40 0.066(5) 0.043(4) 0.027(4) -0.002(3) 0.014(4) 0.000(4) C41 0.044(4) 0.035(4) 0.033(4) -0.004(3) 0.008(3) -0.002(3) C42 0.049(4) 0.034(4) 0.026(4) -0.010(3) 0.004(3) -0.008(3) C43 0.034(4) 0.032(4) 0.027(4) -0.004(3) 0.011(3) 0.009(3) C44 0.053(5) 0.030(4) 0.040(5) 0.002(3) -0.003(4) 0.005(3) C45 0.084(7) 0.041(5) 0.052(6) -0.006(4) -0.023(5) 0.024(4) C46 0.046(5) 0.077(7) 0.060(6) -0.012(5) -0.008(4) 0.026(5) C47 0.037(5) 0.088(7) 0.065(6) 0.007(5) 0.005(4) 0.001(4) C48 0.031(4) 0.069(6) 0.052(5) 0.018(4) 0.013(3) 0.012(4) C49 0.046(4) 0.017(3) 0.027(4) 0.000(3) 0.014(3) -0.003(3) C50 0.066(5) 0.025(4) 0.054(5) 0.005(3) 0.031(4) 0.005(3) C51 0.063(5) 0.033(4) 0.064(6) -0.003(4) 0.039(4) -0.011(4) C52 0.069(5) 0.028(4) 0.043(5) 0.002(3) 0.025(4) -0.007(3) C53 0.053(5) 0.033(4) 0.064(5) 0.018(4) 0.017(4) 0.004(3) C54 0.044(4) 0.028(4) 0.058(5) 0.008(4) 0.016(4) -0.001(3) C55 0.042(4) 0.020(3) 0.029(4) 0.007(3) 0.020(3) 0.008(3) C56 0.047(4) 0.033(4) 0.031(4) 0.005(3) 0.018(3) 0.004(3) C57 0.041(4) 0.054(5) 0.051(5) 0.019(4) 0.021(4) 0.008(3) C58 0.062(6) 0.062(5) 0.051(5) 0.015(4) 0.035(4) 0.025(4) C59 0.073(6) 0.059(6) 0.038(5) -0.001(4) 0.018(4) 0.028(5) C60 0.052(5) 0.032(4) 0.037(4) -0.004(3) 0.007(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C102 1.782(7) . ? Co1 C101 1.795(8) . ? Co1 C2 1.970(6) . ? Co1 C1 1.990(6) . ? Co1 P1 2.235(2) . ? Co1 Co2 2.4772(11) . ? Co2 C202 1.780(7) . ? Co2 C201 1.803(7) . ? Co2 C1 1.972(6) . ? Co2 C2 1.972(6) . ? Co2 P2 2.224(2) . ? Co3 C301 1.777(7) . ? Co3 C302 1.796(7) . ? Co3 C3' 1.96(2) . ? Co3 C3 1.966(13) . ? Co3 C4 1.993(12) . ? Co3 C4' 2.00(2) . ? Co3 P3 2.236(2) . ? Co3 Co4 2.4781(11) . ? Co4 C401 1.781(7) . ? Co4 C402 1.802(7) . ? Co4 C3' 1.96(2) . ? Co4 C3 1.968(13) . ? Co4 C4 1.992(12) . ? Co4 C4' 2.00(2) . ? Co4 P4 2.223(2) . ? P1 C11 1.837(6) . ? P1 C18 1.846(3) . ? P1 C12 1.848(4) . ? P2 C11 1.827(6) . ? P2 C24 1.840(3) . ? P2 C30 1.849(3) . ? P3 C36 1.828(6) . ? P3 C37 1.846(3) . ? P3 C43 1.848(3) . ? P4 C55 1.839(3) . ? P4 C36 1.841(6) . ? P4 C49 1.845(3) . ? O102 C102 1.145(8) . ? O101 C101 1.141(8) . ? O202 C202 1.139(7) . ? O201 C201 1.134(8) . ? O302 C302 1.133(8) . ? O301 C301 1.149(8) . ? O402 C402 1.134(8) . ? O401 C401 1.130(8) . ? C1 C2 1.360(8) . ? C1 C9 1.475(9) . ? C2 C3' 1.423(10) . ? C2 C3 1.424(9) . ? C3 C4 1.364(9) . ? C4 C5 1.503(10) . ? C6 C5 1.534(10) . ? C8 C9 1.538(8) . ? C8 C5 1.612(8) . ? C3' C4' 1.364(10) . ? C4' C5 1.504(11) . ? C6' C9 1.539(11) . ? C8' C5 1.552(9) . ? C8' C9 1.614(9) . ? C5 C7 1.450(9) . ? C9 C10 1.408(9) . ? C12 C13 1.39 . ? C12 C17 1.39 . ? C13 C14 1.39 . ? C14 C15 1.39 . ? C15 C16 1.39 . ? C16 C17 1.39 . ? C18 C19 1.39 . ? C18 C23 1.39 . ? C19 C20 1.39 . ? C20 C21 1.39 . ? C21 C22 1.39 . ? C22 C23 1.39 . ? C24 C25 1.39 . ? C24 C29 1.39 . ? C25 C26 1.39 . ? C26 C27 1.39 . ? C27 C28 1.39 . ? C28 C29 1.39 . ? C30 C31 1.39 . ? C30 C35 1.39 . ? C31 C32 1.39 . ? C32 C33 1.39 . ? C33 C34 1.39 . ? C34 C35 1.39 . ? C37 C38 1.39 . ? C37 C42 1.39 . ? C38 C39 1.39 . ? C39 C40 1.39 . ? C40 C41 1.39 . ? C41 C42 1.39 . ? C43 C44 1.39 . ? C43 C48 1.39 . ? C44 C45 1.39 . ? C45 C46 1.39 . ? C46 C47 1.39 . ? C47 C48 1.39 . ? C49 C50 1.39 . ? C49 C54 1.39 . ? C50 C51 1.39 . ? C51 C52 1.39 . ? C52 C53 1.39 . ? C53 C54 1.39 . ? C55 C56 1.39 . ? C55 C60 1.39 . ? C56 C57 1.39 . ? C57 C58 1.39 . ? C58 C59 1.39 . ? C59 C60 1.39 . ? 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 C102 Co1 C101 97.3(3) . . ? C102 Co1 C2 102.2(3) . . ? C101 Co1 C2 105.7(3) . . ? C102 Co1 C1 108.4(3) . . ? C101 Co1 C1 140.1(3) . . ? C2 Co1 C1 40.2(2) . . ? C102 Co1 P1 100.0(2) . . ? C101 Co1 P1 110.2(2) . . ? C2 Co1 P1 134.5(2) . . ? C1 Co1 P1 95.0(2) . . ? C102 Co1 Co2 153.2(2) . . ? C101 Co1 Co2 93.7(2) . . ? C2 Co1 Co2 51.1(2) . . ? C1 Co1 Co2 51.0(2) . . ? P1 Co1 Co2 99.04(5) . . ? C202 Co2 C201 102.5(3) . . ? C202 Co2 C1 98.3(3) . . ? C201 Co2 C1 134.0(3) . . ? C202 Co2 C2 110.2(3) . . ? C201 Co2 C2 93.8(3) . . ? C1 Co2 C2 40.3(2) . . ? C202 Co2 P2 94.7(2) . . ? C201 Co2 P2 112.9(2) . . ? C1 Co2 P2 105.6(2) . . ? C2 Co2 P2 138.7(2) . . ? C202 Co2 Co1 149.7(2) . . ? C201 Co2 Co1 102.3(2) . . ? C1 Co2 Co1 51.6(2) . . ? C2 Co2 Co1 51.0(2) . . ? P2 Co2 Co1 91.36(5) . . ? C301 Co3 C302 96.4(3) . . ? C301 Co3 C3' 101.9(6) . . ? C302 Co3 C3' 104.9(15) . . ? C301 Co3 C3 101.8(5) . . ? C302 Co3 C3 105.5(10) . . ? C301 Co3 C4 107.9(6) . . ? C302 Co3 C4 140.7(6) . . ? C3 Co3 C4 40.3(3) . . ? C301 Co3 C4' 107.6(8) . . ? C302 Co3 C4' 140.4(8) . . ? C3' Co3 C4' 40.3(4) . . ? C301 Co3 P3 100.8(2) . . ? C302 Co3 P3 109.9(2) . . ? C3' Co3 P3 135.5(11) . . ? C3 Co3 P3 135.1(8) . . ? C4 Co3 P3 95.7(10) . . ? C4' Co3 P3 96.2(14) . . ? C301 Co3 Co4 152.7(2) . . ? C302 Co3 Co4 94.0(2) . . ? C3' Co3 Co4 50.9(5) . . ? C3 Co3 Co4 51.0(4) . . ? C4 Co3 Co4 51.5(4) . . ? C4' Co3 Co4 51.6(5) . . ? P3 Co3 Co4 99.21(5) . . ? C401 Co4 C402 101.9(3) . . ? C401 Co4 C3' 111.1(10) . . ? C402 Co4 C3' 93.5(14) . . ? C401 Co4 C3 110.8(7) . . ? C402 Co4 C3 94.0(10) . . ? C401 Co4 C4 98.7(4) . . ? C402 Co4 C4 134.2(9) . . ? C3 Co4 C4 40.3(3) . . ? C401 Co4 C4' 98.7(6) . . ? C402 Co4 C4' 133.8(13) . . ? C3' Co4 C4' 40.3(4) . . ? C401 Co4 P4 94.6(2) . . ? C402 Co4 P4 112.4(2) . . ? C3' Co4 P4 139.0(6) . . ? C3 Co4 P4 138.8(5) . . ? C4 Co4 P4 106.0(10) . . ? C4' Co4 P4 106.6(14) . . ? C401 Co4 Co3 150.0(2) . . ? C402 Co4 Co3 102.9(2) . . ? C3' Co4 Co3 50.9(6) . . ? C3 Co4 Co3 50.9(4) . . ? C4 Co4 Co3 51.6(4) . . ? C4' Co4 Co3 51.6(5) . . ? P4 Co4 Co3 91.27(5) . . ? C11 P1 C18 101.7(2) . . ? C11 P1 C12 102.3(2) . . ? C18 P1 C12 101.5(2) . . ? C11 P1 Co1 108.9(2) . . ? C18 P1 Co1 123.94(15) . . ? C12 P1 Co1 115.7(2) . . ? C11 P2 C24 102.8(3) . . ? C11 P2 C30 101.7(2) . . ? C24 P2 C30 102.4(2) . . ? C11 P2 Co2 108.7(2) . . ? C24 P2 Co2 121.6(2) . . ? C30 P2 Co2 117.1(2) . . ? C36 P3 C37 101.6(2) . . ? C36 P3 C43 102.2(2) . . ? C37 P3 C43 101.4(2) . . ? C36 P3 Co3 109.0(2) . . ? C37 P3 Co3 123.97(15) . . ? C43 P3 Co3 115.8(2) . . ? C55 P4 C36 102.7(3) . . ? C55 P4 C49 101.7(2) . . ? C36 P4 C49 101.9(2) . . ? C55 P4 Co4 121.9(2) . . ? C36 P4 Co4 108.8(2) . . ? C49 P4 Co4 117.3(2) . . ? C2 C1 C9 128.1(6) . . ? C2 C1 Co2 69.8(3) . . ? C9 C1 Co2 139.0(4) . . ? C2 C1 Co1 69.1(3) . . ? C9 C1 Co1 140.8(5) . . ? Co2 C1 Co1 77.4(2) . . ? C1 C2 C3' 130.9(21) . . ? C1 C2 C3 130.1(15) . . ? C1 C2 Co1 70.7(4) . . ? C3' C2 Co1 138.6(11) . . ? C3 C2 Co1 138.9(8) . . ? C1 C2 Co2 69.8(3) . . ? C3' C2 Co2 138.7(11) . . ? C3 C2 Co2 138.9(8) . . ? Co1 C2 Co2 77.9(2) . . ? C4 C3 C2 131.2(32) . . ? C4 C3 Co3 70.9(8) . . ? C2 C3 Co3 138.5(12) . . ? C4 C3 Co4 70.8(8) . . ? C2 C3 Co4 137.9(12) . . ? Co3 C3 Co4 78.1(4) . . ? C3 C4 C5 127.3(31) . . ? C3 C4 Co4 68.9(8) . . ? C5 C4 Co4 138.5(10) . . ? C3 C4 Co3 68.8(8) . . ? C5 C4 Co3 142.5(11) . . ? Co4 C4 Co3 76.9(3) . . ? C9 C8 C5 111.2(6) . . ? C4' C3' C2 129.5(46) . . ? C4' C3' Co4 71.1(11) . . ? C2 C3' Co4 138.4(16) . . ? C4' C3' Co3 71.1(11) . . ? C2 C3' Co3 138.7(16) . . ? Co4 C3' Co3 78.2(5) . . ? C3' C4' C5 128.9(44) . . ? C3' C4' Co3 68.6(11) . . ? C5 C4' Co3 142.2(15) . . ? C3' C4' Co4 68.6(10) . . ? C5 C4' Co4 138.2(15) . . ? Co3 C4' Co4 76.8(4) . . ? C5 C8' C9 110.3(7) . . ? C7 C5 C4 116.0(13) . . ? C7 C5 C4' 116.6(18) . . ? C7 C5 C6 107.4(7) . . ? C4 C5 C6 114.6(9) . . ? C7 C5 C8' 134.8(8) . . ? C4' C5 C8' 108.2(17) . . ? C7 C5 C8 102.4(6) . . ? C4 C5 C8 111.7(13) . . ? C6 C5 C8 103.3(6) . . ? C10 C9 C1 120.4(6) . . ? C10 C9 C8 127.9(7) . . ? C1 C9 C8 111.6(6) . . ? C10 C9 C6' 105.6(8) . . ? C1 C9 C6' 118.5(8) . . ? C10 C9 C8' 98.1(6) . . ? C1 C9 C8' 110.7(7) . . ? C6' C9 C8' 99.6(8) . . ? O102 C102 Co1 175.0(7) . . ? O101 C101 Co1 176.4(7) . . ? O202 C202 Co2 177.7(6) . . ? O201 C201 Co2 173.7(7) . . ? P2 C11 P1 108.9(3) . . ? C13 C12 C17 120.0 . . ? C13 C12 P1 121.8(3) . . ? C17 C12 P1 117.7(3) . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C17 120.0 . . ? C16 C17 C12 120.0 . . ? C19 C18 C23 120.0 . . ? C19 C18 P1 119.6(2) . . ? C23 C18 P1 120.2(2) . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C23 C18 120.0 . . ? C25 C24 C29 120.0 . . ? C25 C24 P2 120.1(2) . . ? C29 C24 P2 119.9(2) . . ? C26 C25 C24 120.0 . . ? C25 C26 C27 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C24 120.0 . . ? C31 C30 C35 120.0 . . ? C31 C30 P2 119.1(2) . . ? C35 C30 P2 120.8(2) . . ? C32 C31 C30 120.0 . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C34 C35 C30 120.0 . . ? O302 C302 Co3 176.2(6) . . ? O301 C301 Co3 175.3(7) . . ? O402 C402 Co4 173.0(6) . . ? O401 C401 Co4 178.1(6) . . ? P3 C36 P4 108.8(3) . . ? C38 C37 C42 120.0 . . ? C38 C37 P3 120.0(2) . . ? C42 C37 P3 119.7(2) . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C41 C40 C39 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C37 120.0 . . ? C44 C43 C48 120.0 . . ? C44 C43 P3 117.9(3) . . ? C48 C43 P3 121.7(3) . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C47 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C43 120.0 . . ? C50 C49 C54 120.0 . . ? C50 C49 P4 120.4(2) . . ? C54 C49 P4 119.5(2) . . ? C51 C50 C49 120.0 . . ? C50 C51 C52 120.0 . . ? C53 C52 C51 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C49 120.0 . . ? C56 C55 C60 120.0 . . ? C56 C55 P4 119.9(2) . . ? C60 C55 P4 120.1(2) . . ? C55 C56 C57 120.0 . . ? C58 C57 C56 120.0 . . ? C57 C58 C59 120.0 . . ? C60 C59 C58 120.0 . . ? C59 C60 C55 120.0 . . ? _refine_diff_density_max 0.758 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.073 #===END data_mm0215i_COMPOUND_7 _database_code_depnum_ccdc_archive 'CCDC 228897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H32 Co4 O10 P2' _chemical_formula_weight 1030.37 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.7446(5) _cell_length_b 15.4562(2) _cell_length_c 16.7757(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.1710(10) _cell_angle_gamma 90.00 _cell_volume 10303.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 49447 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.623 _exptl_absorpt_correction_T_max 0.678 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_reflns_number 45396 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11771 _reflns_number_gt 8629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution teXsan _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' #_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1227P)^2^+30.5078P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11771 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.2091 _refine_ls_wR_factor_gt 0.1882 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.070 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co2 Co 0.091276(13) 0.30677(4) 0.61114(3) 0.03265(16) Uani 1 1 d . . . Co1 Co 0.141503(13) 0.23755(4) 0.67431(3) 0.03112(15) Uani 1 1 d . . . Co3 Co 0.162402(15) 0.09598(4) 0.45834(4) 0.04087(18) Uani 1 1 d . . . Co4 Co 0.110660(16) 0.14908(4) 0.39270(4) 0.04437(18) Uani 1 1 d . . . P2 P 0.08353(3) 0.39414(7) 0.71403(6) 0.0319(2) Uani 1 1 d . . . P1 P 0.15108(3) 0.33075(7) 0.77296(6) 0.0339(2) Uani 1 1 d . . . C10 C 0.15630(16) 0.4652(3) 0.5456(3) 0.0595(14) Uani 1 1 d . . . H10A H 0.1402 0.4888 0.5807 0.071 Uiso 1 1 calc R . . H10B H 0.1701 0.5026 0.5154 0.071 Uiso 1 1 calc R . . C9 C 0.15953(12) 0.3800(3) 0.5389(3) 0.0421(10) Uani 1 1 d . . . C8 C 0.18454(12) 0.3394(3) 0.4830(3) 0.0466(11) Uani 1 1 d . . . H8A H 0.1973 0.2946 0.5131 0.056 Uiso 1 1 calc R . . H8B H 0.2008 0.3846 0.4675 0.056 Uiso 1 1 calc R . . C5 C 0.16986(12) 0.2966(3) 0.4047(3) 0.0456(11) Uani 1 1 d . . . C7 C 0.20005(16) 0.2768(4) 0.3506(4) 0.0682(16) Uani 1 1 d . . . H7A H 0.1918 0.2502 0.3009 0.102 Uiso 1 1 calc R . . H7B H 0.2155 0.2370 0.3782 0.102 Uiso 1 1 calc R . . H7C H 0.2119 0.3307 0.3385 0.102 Uiso 1 1 calc R . . C6 C 0.14594(15) 0.3598(4) 0.3623(3) 0.0585(14) Uani 1 1 d . . . H6A H 0.1368 0.3329 0.3136 0.088 Uiso 1 1 calc R . . H6B H 0.1582 0.4125 0.3485 0.088 Uiso 1 1 calc R . . H6C H 0.1275 0.3746 0.3977 0.088 Uiso 1 1 calc R . . C4 C 0.15088(11) 0.2156(3) 0.4259(3) 0.0386(9) Uani 1 1 d . . . C3 C 0.13329(10) 0.1926(3) 0.4905(2) 0.0322(8) Uani 1 1 d . . . C2 C 0.12719(10) 0.2394(3) 0.5629(2) 0.0314(8) Uani 1 1 d . . . C1 C 0.13877(10) 0.3200(3) 0.5843(2) 0.0324(8) Uani 1 1 d . . . O202 O 0.06572(13) 0.4261(3) 0.4909(2) 0.0795(14) Uani 1 1 d . . . C202 C 0.07510(13) 0.3785(4) 0.5374(3) 0.0506(12) Uani 1 1 d . . . O201 O 0.04256(10) 0.1641(3) 0.5988(3) 0.0770(13) Uani 1 1 d . . . C201 C 0.05995(12) 0.2216(3) 0.6082(3) 0.0474(11) Uani 1 1 d . . . O102 O 0.20784(10) 0.1567(3) 0.6720(3) 0.0731(12) Uani 1 1 d . . . C102 C 0.18190(13) 0.1889(3) 0.6725(3) 0.0448(11) Uani 1 1 d . . . O101 O 0.10409(11) 0.0945(3) 0.7447(3) 0.0665(11) Uani 1 1 d . . . C101 C 0.11884(12) 0.1504(3) 0.7193(3) 0.0429(10) Uani 1 1 d . . . C36 C 0.12428(10) 0.4263(3) 0.7582(3) 0.0351(9) Uani 1 1 d . . . H36A H 0.1207 0.4551 0.8101 0.042 Uiso 1 1 calc R . . H36B H 0.1355 0.4679 0.7226 0.042 Uiso 1 1 calc R . . C30 C 0.06315(11) 0.4988(3) 0.6938(2) 0.0361(9) Uani 1 1 d . . . C35 C 0.02971(11) 0.4979(3) 0.6672(3) 0.0461(11) Uani 1 1 d . . . H35A H 0.0182 0.4443 0.6611 0.055 Uiso 1 1 calc R . . C34 C 0.01328(13) 0.5739(4) 0.6498(3) 0.0550(13) Uani 1 1 d . . . H34A H -0.0094 0.5725 0.6311 0.066 Uiso 1 1 calc R . . C33 C 0.02964(14) 0.6533(3) 0.6591(3) 0.0517(12) Uani 1 1 d . . . H33A H 0.0179 0.7059 0.6490 0.062 Uiso 1 1 calc R . . C32 C 0.06229(15) 0.6547(3) 0.6827(4) 0.0580(14) Uani 1 1 d . . . H32A H 0.0738 0.7084 0.6870 0.070 Uiso 1 1 calc R . . C31 C 0.07927(13) 0.5776(3) 0.7010(3) 0.0503(12) Uani 1 1 d . . . H31A H 0.1021 0.5796 0.7184 0.060 Uiso 1 1 calc R . . C23 C 0.06046(10) 0.3558(3) 0.8005(3) 0.0356(9) Uani 1 1 d . . . C28 C 0.05313(12) 0.4125(3) 0.8622(3) 0.0430(10) Uani 1 1 d . . . H28A H 0.0588 0.4720 0.8579 0.052 Uiso 1 1 calc R . . C27 C 0.03743(13) 0.3820(4) 0.9306(3) 0.0523(12) Uani 1 1 d . . . H27A H 0.0330 0.4205 0.9732 0.063 Uiso 1 1 calc R . . C26 C 0.02843(15) 0.2972(4) 0.9362(3) 0.0581(14) Uani 1 1 d . . . H26A H 0.0173 0.2771 0.9823 0.070 Uiso 1 1 calc R . . C25 C 0.03536(17) 0.2408(4) 0.8758(4) 0.0656(16) Uani 1 1 d . . . H25A H 0.0292 0.1816 0.8801 0.079 Uiso 1 1 calc R . . C24 C 0.05152(14) 0.2704(3) 0.8076(3) 0.0528(12) Uani 1 1 d . . . H24A H 0.0563 0.2311 0.7659 0.063 Uiso 1 1 calc R . . C17 C 0.19275(11) 0.3811(3) 0.7820(3) 0.0415(10) Uani 1 1 d . . . C22 C 0.21385(15) 0.3838(4) 0.7165(4) 0.0671(16) Uani 1 1 d . . . H22A H 0.2066 0.3578 0.6678 0.081 Uiso 1 1 calc R . . C21 C 0.24501(17) 0.4235(5) 0.7211(5) 0.082(2) Uani 1 1 d . . . H21A H 0.2591 0.4248 0.6760 0.098 Uiso 1 1 calc R . . C20 C 0.25531(15) 0.4608(5) 0.7911(5) 0.081(2) Uani 1 1 d . . . H20A H 0.2769 0.4870 0.7952 0.097 Uiso 1 1 calc R . . C19 C 0.23502(17) 0.4607(6) 0.8545(5) 0.103(3) Uani 1 1 d . . . H19A H 0.2421 0.4890 0.9022 0.124 Uiso 1 1 calc R . . C18 C 0.20384(14) 0.4198(5) 0.8509(4) 0.080(2) Uani 1 1 d . . . H18A H 0.1902 0.4187 0.8967 0.095 Uiso 1 1 calc R . . C11 C 0.14409(16) 0.2939(3) 0.8742(3) 0.0562(14) Uani 1 1 d . . . C16 C 0.12803(16) 0.3417(4) 0.9320(3) 0.0623(15) Uani 1 1 d . . . H16A H 0.1198 0.3981 0.9206 0.075 Uiso 1 1 calc R . . C15 C 0.1241(2) 0.3050(6) 1.0078(4) 0.100(3) Uani 1 1 d . . . H15A H 0.1133 0.3382 1.0474 0.120 Uiso 1 1 calc R . . C14 C 0.1345(5) 0.2288(6) 1.0260(5) 0.183(8) Uani 1 1 d . . . H14A H 0.1318 0.2060 1.0781 0.220 Uiso 1 1 calc R . . C13 C 0.1493(7) 0.1827(5) 0.9692(5) 0.286(14) Uani 1 1 d . . . H13A H 0.1555 0.1247 0.9811 0.343 Uiso 1 1 calc R . . C12 C 0.1561(4) 0.2148(4) 0.8932(4) 0.157(6) Uani 1 1 d . . . H12A H 0.1688 0.1821 0.8564 0.189 Uiso 1 1 calc R . . O303 O 0.23279(11) 0.1254(4) 0.5034(3) 0.0888(15) Uani 1 1 d . . . C303 C 0.20495(15) 0.1146(4) 0.4884(4) 0.0596(14) Uani 1 1 d . . . O302 O 0.13928(17) -0.0080(3) 0.5944(3) 0.1013(19) Uani 1 1 d . . . C302 C 0.14790(17) 0.0282(4) 0.5407(3) 0.0607(14) Uani 1 1 d . . . O301 O 0.17531(11) -0.0145(3) 0.3194(3) 0.0662(11) Uani 1 1 d . . . C301 C 0.17069(13) 0.0280(3) 0.3735(3) 0.0490(11) Uani 1 1 d . . . O403 O 0.07466(15) -0.0103(4) 0.4303(4) 0.110(2) Uani 1 1 d . . . C403 C 0.08792(16) 0.0508(5) 0.4161(4) 0.0685(16) Uani 1 1 d . . . O402 O 0.12580(17) 0.1431(4) 0.2219(2) 0.105(2) Uani 1 1 d . . . C402 C 0.11966(17) 0.1438(4) 0.2860(3) 0.0656(16) Uani 1 1 d . . . O401 O 0.05295(12) 0.2668(4) 0.3884(3) 0.0879(16) Uani 1 1 d . . . C401 C 0.07565(14) 0.2230(4) 0.3898(3) 0.0577(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co2 0.0327(3) 0.0334(3) 0.0319(3) -0.0043(2) 0.0005(2) 0.0037(2) Co1 0.0352(3) 0.0289(3) 0.0292(3) -0.0001(2) -0.0005(2) 0.0017(2) Co3 0.0439(3) 0.0381(3) 0.0408(3) -0.0037(3) 0.0063(3) 0.0074(3) Co4 0.0457(4) 0.0522(4) 0.0351(3) -0.0089(3) -0.0011(3) 0.0032(3) P2 0.0322(5) 0.0313(5) 0.0324(5) -0.0033(4) 0.0042(4) 0.0006(4) P1 0.0402(6) 0.0312(5) 0.0300(5) -0.0001(4) -0.0035(4) -0.0011(4) C10 0.088(4) 0.040(3) 0.051(3) 0.008(2) 0.013(3) -0.004(3) C9 0.044(2) 0.042(3) 0.041(2) 0.0039(19) -0.0009(19) -0.0036(19) C8 0.043(2) 0.045(3) 0.052(3) 0.007(2) 0.006(2) -0.008(2) C5 0.050(3) 0.049(3) 0.038(2) 0.008(2) 0.013(2) 0.000(2) C7 0.076(4) 0.067(4) 0.062(4) 0.002(3) 0.036(3) -0.002(3) C6 0.070(3) 0.059(3) 0.047(3) 0.009(2) -0.006(3) 0.004(3) C4 0.045(2) 0.037(2) 0.034(2) -0.0012(17) 0.0021(18) 0.0033(19) C3 0.0310(19) 0.034(2) 0.032(2) -0.0003(16) -0.0019(16) 0.0034(16) C2 0.0328(19) 0.033(2) 0.0280(19) -0.0015(15) 0.0019(15) 0.0031(16) C1 0.035(2) 0.032(2) 0.0304(19) 0.0011(16) 0.0012(16) 0.0034(16) O202 0.111(4) 0.079(3) 0.048(2) 0.006(2) -0.012(2) 0.049(3) C202 0.054(3) 0.056(3) 0.041(3) -0.008(2) -0.004(2) 0.020(2) O201 0.056(2) 0.062(3) 0.113(4) -0.025(3) 0.000(2) -0.020(2) C201 0.038(2) 0.051(3) 0.053(3) -0.013(2) 0.000(2) 0.004(2) O102 0.051(2) 0.084(3) 0.083(3) 0.002(2) -0.006(2) 0.029(2) C102 0.052(3) 0.042(3) 0.040(2) 0.0011(19) -0.005(2) 0.005(2) O101 0.074(3) 0.047(2) 0.079(3) 0.015(2) 0.013(2) -0.0103(19) C101 0.049(3) 0.040(3) 0.040(2) 0.0014(19) 0.001(2) 0.001(2) C36 0.037(2) 0.030(2) 0.038(2) -0.0036(17) 0.0036(17) -0.0016(17) C30 0.040(2) 0.035(2) 0.033(2) -0.0031(17) 0.0064(17) 0.0049(17) C35 0.037(2) 0.042(3) 0.059(3) 0.001(2) 0.003(2) 0.0026(19) C34 0.043(3) 0.057(3) 0.065(3) 0.005(3) 0.006(2) 0.016(2) C33 0.061(3) 0.043(3) 0.051(3) 0.002(2) 0.013(2) 0.019(2) C32 0.070(4) 0.037(3) 0.067(3) -0.004(2) 0.000(3) 0.000(2) C31 0.046(3) 0.037(3) 0.068(3) 0.001(2) -0.002(2) 0.000(2) C23 0.031(2) 0.038(2) 0.037(2) -0.0009(17) 0.0063(17) -0.0021(17) C28 0.048(2) 0.040(2) 0.041(2) -0.0063(19) 0.009(2) -0.004(2) C27 0.053(3) 0.061(3) 0.043(3) -0.009(2) 0.014(2) -0.004(2) C26 0.067(3) 0.061(3) 0.047(3) 0.007(2) 0.020(3) -0.012(3) C25 0.084(4) 0.050(3) 0.064(4) 0.005(3) 0.026(3) -0.016(3) C24 0.061(3) 0.044(3) 0.054(3) -0.004(2) 0.022(2) -0.007(2) C17 0.040(2) 0.035(2) 0.049(3) -0.0072(19) -0.007(2) 0.0043(18) C22 0.063(3) 0.081(4) 0.058(3) -0.001(3) 0.001(3) -0.029(3) C21 0.064(4) 0.099(5) 0.082(5) -0.007(4) 0.009(3) -0.029(4) C20 0.046(3) 0.083(5) 0.113(6) -0.044(4) 0.006(3) -0.010(3) C19 0.055(4) 0.135(7) 0.121(6) -0.088(6) 0.000(4) -0.017(4) C18 0.045(3) 0.110(5) 0.084(4) -0.060(4) 0.001(3) -0.006(3) C11 0.094(4) 0.043(3) 0.032(2) 0.001(2) -0.005(2) -0.018(3) C16 0.071(4) 0.083(4) 0.033(2) 0.004(3) 0.003(2) -0.017(3) C15 0.142(7) 0.124(7) 0.034(3) -0.005(4) 0.011(4) -0.051(6) C14 0.44(2) 0.073(6) 0.038(4) 0.012(4) 0.019(7) -0.074(9) C13 0.77(4) 0.037(4) 0.048(5) 0.016(3) -0.010(11) 0.006(11) C12 0.400(19) 0.035(3) 0.037(3) 0.005(3) 0.001(6) 0.027(6) O303 0.050(2) 0.115(4) 0.101(4) -0.002(3) -0.012(2) 0.014(2) C303 0.058(3) 0.065(4) 0.057(3) -0.001(3) 0.003(3) 0.019(3) O302 0.186(6) 0.055(3) 0.065(3) 0.012(2) 0.044(3) 0.002(3) C302 0.091(4) 0.038(3) 0.054(3) 0.000(2) 0.015(3) 0.008(3) O301 0.073(3) 0.061(2) 0.065(2) -0.022(2) 0.020(2) 0.000(2) C301 0.049(3) 0.041(3) 0.058(3) -0.004(2) 0.011(2) 0.003(2) O403 0.104(4) 0.091(4) 0.137(5) 0.001(4) 0.007(4) -0.045(3) C403 0.060(3) 0.071(4) 0.075(4) -0.010(3) -0.003(3) -0.017(3) O402 0.167(6) 0.118(5) 0.030(2) -0.005(2) 0.012(3) 0.031(4) C402 0.079(4) 0.075(4) 0.043(3) -0.012(3) -0.005(3) 0.017(3) O401 0.065(3) 0.109(4) 0.088(3) -0.025(3) -0.024(2) 0.039(3) C401 0.055(3) 0.070(4) 0.048(3) -0.015(3) -0.012(2) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co2 C202 1.772(5) . ? Co2 C201 1.812(5) . ? Co2 C2 1.956(4) . ? Co2 C1 1.960(4) . ? Co2 P2 2.2181(12) . ? Co2 Co1 2.4831(7) . ? Co1 C102 1.774(5) . ? Co1 C101 1.796(5) . ? Co1 C2 1.943(4) . ? Co1 C1 1.976(4) . ? Co1 P1 2.2210(12) . ? Co3 C303 1.778(6) . ? Co3 C301 1.804(5) . ? Co3 C302 1.836(6) . ? Co3 C3 1.971(4) . ? Co3 C4 1.978(5) . ? Co3 Co4 2.4542(9) . ? Co4 C401 1.800(6) . ? Co4 C403 1.815(7) . ? Co4 C402 1.835(6) . ? Co4 C4 1.971(5) . ? Co4 C3 1.973(4) . ? P2 C23 1.830(4) . ? P2 C36 1.836(4) . ? P2 C30 1.837(4) . ? P1 C11 1.818(5) . ? P1 C17 1.833(5) . ? P1 C36 1.834(4) . ? C10 C9 1.328(7) . ? C9 C1 1.466(6) . ? C9 C8 1.516(7) . ? C8 C5 1.572(7) . ? C5 C4 1.508(7) . ? C5 C6 1.529(7) . ? C5 C7 1.550(7) . ? C4 C3 1.349(6) . ? C3 C2 1.438(6) . ? C2 C1 1.373(6) . ? O202 C202 1.130(6) . ? O201 C201 1.134(6) . ? O102 C102 1.145(6) . ? O101 C101 1.132(6) . ? C30 C31 1.381(7) . ? C30 C35 1.393(6) . ? C35 C34 1.374(7) . ? C34 C33 1.396(8) . ? C33 C32 1.349(8) . ? C32 C31 1.400(7) . ? C23 C24 1.373(7) . ? C23 C28 1.391(6) . ? C28 C27 1.399(7) . ? C27 C26 1.363(8) . ? C26 C25 1.369(8) . ? C25 C24 1.400(7) . ? C17 C18 1.367(7) . ? C17 C22 1.396(8) . ? C22 C21 1.383(8) . ? C21 C20 1.363(10) . ? C20 C19 1.348(10) . ? C19 C18 1.392(9) . ? C11 C12 1.348(9) . ? C11 C16 1.385(8) . ? C16 C15 1.403(9) . ? C15 C14 1.284(14) . ? C14 C13 1.334(18) . ? C13 C12 1.401(12) . ? O303 C303 1.142(7) . ? O302 C302 1.120(7) . ? O301 C301 1.139(6) . ? O403 C403 1.109(8) . ? O402 C402 1.107(7) . ? O401 C401 1.128(7) . ? 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 C202 Co2 C201 101.3(3) . . ? C202 Co2 C2 107.5(2) . . ? C201 Co2 C2 96.24(19) . . ? C202 Co2 C1 96.4(2) . . ? C201 Co2 C1 137.21(19) . . ? C2 Co2 C1 41.07(17) . . ? C202 Co2 P2 96.23(16) . . ? C201 Co2 P2 110.95(16) . . ? C2 Co2 P2 139.51(12) . . ? C1 Co2 P2 105.35(12) . . ? C202 Co2 Co1 147.62(18) . . ? C201 Co2 Co1 104.17(16) . . ? C2 Co2 Co1 50.22(12) . . ? C1 Co2 Co1 51.18(12) . . ? P2 Co2 Co1 93.06(4) . . ? C102 Co1 C101 98.7(2) . . ? C102 Co1 C2 103.70(19) . . ? C101 Co1 C2 106.02(19) . . ? C102 Co1 C1 107.2(2) . . ? C101 Co1 C1 141.68(19) . . ? C2 Co1 C1 41.01(17) . . ? C102 Co1 P1 98.43(16) . . ? C101 Co1 P1 104.66(15) . . ? C2 Co1 P1 138.57(13) . . ? C1 Co1 P1 99.03(12) . . ? C102 Co1 Co2 153.55(16) . . ? C101 Co1 Co2 95.56(15) . . ? C2 Co1 Co2 50.66(12) . . ? C1 Co1 Co2 50.60(12) . . ? P1 Co1 Co2 99.36(4) . . ? C303 Co3 C301 97.5(2) . . ? C303 Co3 C302 101.0(3) . . ? C301 Co3 C302 109.1(2) . . ? C303 Co3 C3 111.1(2) . . ? C301 Co3 C3 140.7(2) . . ? C302 Co3 C3 91.8(2) . . ? C303 Co3 C4 98.1(2) . . ? C301 Co3 C4 111.8(2) . . ? C302 Co3 C4 131.7(2) . . ? C3 Co3 C4 39.93(17) . . ? C303 Co3 Co4 148.9(2) . . ? C301 Co3 Co4 90.33(17) . . ? C302 Co3 Co4 104.8(2) . . ? C3 Co3 Co4 51.54(11) . . ? C4 Co3 Co4 51.45(13) . . ? C401 Co4 C403 98.6(3) . . ? C401 Co4 C402 99.7(3) . . ? C403 Co4 C402 106.4(3) . . ? C401 Co4 C4 107.4(2) . . ? C403 Co4 C4 141.3(2) . . ? C402 Co4 C4 97.2(3) . . ? C401 Co4 C3 98.3(2) . . ? C403 Co4 C3 109.0(2) . . ? C402 Co4 C3 137.0(3) . . ? C4 Co4 C3 40.00(17) . . ? C401 Co4 Co3 149.80(17) . . ? C403 Co4 Co3 92.3(2) . . ? C402 Co4 Co3 104.2(2) . . ? C4 Co4 Co3 51.71(13) . . ? C3 Co4 Co3 51.50(12) . . ? C23 P2 C36 102.7(2) . . ? C23 P2 C30 101.81(19) . . ? C36 P2 C30 102.6(2) . . ? C23 P2 Co2 119.98(15) . . ? C36 P2 Co2 110.11(14) . . ? C30 P2 Co2 117.39(14) . . ? C11 P1 C17 102.2(2) . . ? C11 P1 C36 106.2(2) . . ? C17 P1 C36 101.0(2) . . ? C11 P1 Co1 117.76(17) . . ? C17 P1 Co1 118.51(16) . . ? C36 P1 Co1 109.36(14) . . ? C10 C9 C1 121.8(5) . . ? C10 C9 C8 122.0(5) . . ? C1 C9 C8 116.2(4) . . ? C9 C8 C5 117.0(4) . . ? C4 C5 C6 109.3(4) . . ? C4 C5 C7 111.8(4) . . ? C6 C5 C7 109.6(4) . . ? C4 C5 C8 109.4(4) . . ? C6 C5 C8 109.6(4) . . ? C7 C5 C8 107.1(4) . . ? C3 C4 C5 132.6(4) . . ? C3 C4 Co4 70.1(3) . . ? C5 C4 Co4 140.7(3) . . ? C3 C4 Co3 69.8(3) . . ? C5 C4 Co3 136.6(3) . . ? Co4 C4 Co3 76.84(17) . . ? C4 C3 C2 130.2(4) . . ? C4 C3 Co3 70.3(3) . . ? C2 C3 Co3 136.2(3) . . ? C4 C3 Co4 69.9(3) . . ? C2 C3 Co4 142.3(3) . . ? Co3 C3 Co4 76.96(15) . . ? C1 C2 C3 128.0(4) . . ? C1 C2 Co1 70.8(2) . . ? C3 C2 Co1 138.9(3) . . ? C1 C2 Co2 69.6(2) . . ? C3 C2 Co2 139.0(3) . . ? Co1 C2 Co2 79.12(15) . . ? C2 C1 C9 128.8(4) . . ? C2 C1 Co2 69.3(2) . . ? C9 C1 Co2 137.7(3) . . ? C2 C1 Co1 68.2(2) . . ? C9 C1 Co1 141.5(3) . . ? Co2 C1 Co1 78.22(15) . . ? O202 C202 Co2 177.5(6) . . ? O201 C201 Co2 171.5(5) . . ? O102 C102 Co1 179.1(5) . . ? O101 C101 Co1 177.2(5) . . ? P2 C36 P1 110.0(2) . . ? C31 C30 C35 118.3(4) . . ? C31 C30 P2 124.0(3) . . ? C35 C30 P2 117.7(3) . . ? C34 C35 C30 120.4(5) . . ? C35 C34 C33 120.7(5) . . ? C32 C33 C34 119.3(5) . . ? C33 C32 C31 120.5(5) . . ? C30 C31 C32 120.8(5) . . ? C24 C23 C28 118.9(4) . . ? C24 C23 P2 121.0(4) . . ? C28 C23 P2 120.1(3) . . ? C23 C28 C27 120.1(5) . . ? C26 C27 C28 120.3(5) . . ? C27 C26 C25 120.3(5) . . ? C26 C25 C24 119.9(5) . . ? C23 C24 C25 120.6(5) . . ? C18 C17 C22 117.6(5) . . ? C18 C17 P1 122.1(4) . . ? C22 C17 P1 120.3(4) . . ? C21 C22 C17 121.5(6) . . ? C20 C21 C22 119.2(7) . . ? C19 C20 C21 120.3(6) . . ? C20 C19 C18 120.9(6) . . ? C17 C18 C19 120.5(6) . . ? C12 C11 C16 119.0(6) . . ? C12 C11 P1 116.4(5) . . ? C16 C11 P1 124.6(4) . . ? C15 C16 C11 118.7(7) . . ? C14 C15 C16 123.0(9) . . ? C15 C14 C13 117.7(7) . . ? C14 C13 C12 123.8(9) . . ? C11 C12 C13 117.5(10) . . ? O303 C303 Co3 176.1(6) . . ? O302 C302 Co3 175.0(5) . . ? O301 C301 Co3 178.7(5) . . ? O403 C403 Co4 178.4(7) . . ? O402 C402 Co4 177.5(7) . . ? O401 C401 Co4 177.5(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.711 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.129 #===END data_mm0133_COMPOUND_10 _database_code_depnum_ccdc_archive 'CCDC 228898' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79.50 H70 Cl4 Co4 O10 P4' _chemical_formula_weight 1686.76 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 40.5806(5) _cell_length_b 11.9801(2) _cell_length_c 36.1936(5) _cell_angle_alpha 90.00 _cell_angle_beta 118.245(8) _cell_angle_gamma 90.00 _cell_volume 15500.8(4) _cell_formula_units_Z 8 _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 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6904 _exptl_absorpt_coefficient_mu 1.119 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8156 _exptl_absorpt_correction_T_max 0.9462 _exptl_absorpt_process_details ? _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52975 _diffrn_reflns_av_R_equivalents 0.1132 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 25.05 _reflns_number_total 13600 _reflns_number_gt 10536 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0918P)^2^+63.6949P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13600 _refine_ls_number_parameters 922 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1800 _refine_ls_wR_factor_gt 0.1521 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.073 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.198524(16) 0.72024(5) 0.860770(19) 0.03329(17) Uani 1 1 d . . . P1 P 0.17696(3) 0.50197(10) 0.79110(4) 0.0303(3) Uani 1 1 d . . . O1 O 0.12015(11) 0.3683(3) 0.93055(11) 0.0521(9) Uani 1 1 d . . . C1 C 0.14275(17) 0.3453(4) 0.91047(19) 0.0504(13) Uani 1 1 d . . . C01 C 0.0000 0.3093(11) 0.7500 0.102(4) Uani 1 2 d SD . . H01 H 0.005(5) 0.358(3) 0.7745(16) 0.122 Uiso 0.50 1 d PD . . Co2 Co 0.144466(16) 0.64416(5) 0.797565(19) 0.03167(16) Uani 1 1 d . . . P2 P 0.24072(3) 0.58907(11) 0.86988(4) 0.0342(3) Uani 1 1 d . . . O2 O 0.14743(11) 0.4736(4) 1.00776(14) 0.0482(10) Uani 1 1 d . . . HO2 H 0.1418(13) 0.443(4) 0.9906(15) 0.017(14) Uiso 1 1 d . . . C2 C 0.14781(13) 0.4488(4) 0.89176(16) 0.0397(11) Uani 1 1 d . . . C02 C 0.2802(2) 0.1484(8) 0.9204(2) 0.098(3) Uani 1 1 d . . . H02A H 0.3020 0.1068 0.9424 0.118 Uiso 1 1 calc R . . Co3 Co 0.018316(15) 0.83280(5) 0.905702(18) 0.02811(16) Uani 1 1 d . . . P3 P 0.00179(3) 0.74715(9) 0.94983(3) 0.0280(2) Uani 1 1 d . . . C3 C 0.15178(12) 0.5334(4) 0.87672(14) 0.0318(10) Uani 1 1 d . . . Co4 Co 0.011150(16) 0.66999(5) 0.860410(18) 0.03081(16) Uani 1 1 d . . . P4 P -0.00916(3) 0.55553(9) 0.89274(3) 0.0277(2) Uani 1 1 d . . . C4 C 0.15704(12) 0.6259(4) 0.85654(14) 0.0321(10) Uani 1 1 d . . . C5 C 0.14493(12) 0.7322(4) 0.84399(15) 0.0347(10) Uani 1 1 d . . . C6 C 0.12150(14) 0.8211(4) 0.84992(19) 0.0454(12) Uani 1 1 d . . . C7 C 0.13776(16) 0.8423(6) 0.89925(19) 0.0630(17) Uani 1 1 d . . . H7A H 0.1633 0.8715 0.9110 0.094 Uiso 1 1 calc R . . H7B H 0.1380 0.7719 0.9131 0.094 Uiso 1 1 calc R . . H7C H 0.1219 0.8965 0.9037 0.094 Uiso 1 1 calc R . . C8 C 0.12312(17) 0.9301(4) 0.8291(2) 0.0599(16) Uani 1 1 d . . . H8A H 0.1134 0.9180 0.7990 0.090 Uiso 1 1 calc R . . H8B H 0.1491 0.9559 0.8415 0.090 Uiso 1 1 calc R . . H8C H 0.1079 0.9867 0.8336 0.090 Uiso 1 1 calc R . . C9 C 0.08252(13) 0.7774(4) 0.83490(17) 0.0419(11) Uani 1 1 d . . . H9A H 0.0845 0.7026 0.8474 0.050 Uiso 1 1 calc R . . H9B H 0.0710 0.7671 0.8041 0.050 Uiso 1 1 calc R . . C10 C 0.05598(15) 0.8462(4) 0.84396(18) 0.0465(13) Uani 1 1 d . . . C11 C 0.03950(14) 0.9384(4) 0.82310(17) 0.0454(12) Uani 1 1 d . . . H11A H 0.0207 0.9734 0.8276 0.054 Uiso 1 1 calc R . . H11B H 0.0465 0.9694 0.8037 0.054 Uiso 1 1 calc R . . Cl11 Cl -0.03963(8) 0.2277(3) 0.73621(8) 0.1369(10) Uani 1 1 d . . . C12 C 0.04531(12) 0.7969(4) 0.87425(15) 0.0324(10) Uani 1 1 d . . . C13 C 0.05668(11) 0.7275(3) 0.90808(14) 0.0301(9) Uani 1 1 d . . . C14 C 0.08892(12) 0.6790(4) 0.94050(15) 0.0323(10) Uani 1 1 d . . . C15 C 0.11552(12) 0.6370(4) 0.96914(14) 0.0342(10) Uani 1 1 d . . . C16 C 0.15101(13) 0.5909(4) 1.00334(15) 0.0402(11) Uani 1 1 d . . . C17 C 0.15869(18) 0.6412(6) 1.04504(18) 0.0636(17) Uani 1 1 d . . . H17A H 0.1378 0.6244 1.0506 0.095 Uiso 1 1 calc R . . H17B H 0.1614 0.7222 1.0441 0.095 Uiso 1 1 calc R . . H17C H 0.1818 0.6094 1.0674 0.095 Uiso 1 1 calc R . . C18 C 0.18267(13) 0.6140(5) 0.99319(18) 0.0537(14) Uani 1 1 d . . . H18A H 0.1768 0.5805 0.9661 0.081 Uiso 1 1 calc R . . H18B H 0.2059 0.5817 1.0151 0.081 Uiso 1 1 calc R . . H18C H 0.1857 0.6948 0.9919 0.081 Uiso 1 1 calc R . . C19 C 0.1229(3) 0.2573(6) 0.8765(3) 0.101(3) Uani 1 1 d . . . H19A H 0.0993 0.2878 0.8547 0.152 Uiso 1 1 calc R . . H19B H 0.1178 0.1912 0.8890 0.152 Uiso 1 1 calc R . . H19C H 0.1389 0.2363 0.8641 0.152 Uiso 1 1 calc R . . C20 C 0.1802(2) 0.3044(6) 0.9461(3) 0.082(2) Uani 1 1 d . . . H20A H 0.1917 0.3640 0.9669 0.123 Uiso 1 1 calc R . . H20B H 0.1970 0.2840 0.9346 0.123 Uiso 1 1 calc R . . H20C H 0.1759 0.2391 0.9595 0.123 Uiso 1 1 calc R . . C21 C 0.21514(11) 0.4623(4) 0.84312(14) 0.0319(9) Uani 1 1 d . . . H21A H 0.2047 0.4257 0.8598 0.038 Uiso 1 1 calc R . . H21B H 0.2323 0.4090 0.8399 0.038 Uiso 1 1 calc R . . Cl21 Cl 0.27676(11) 0.2644(3) 0.93695(13) 0.1698(14) Uani 1 1 d . . . C22 C 0.15355(13) 0.3682(4) 0.77041(15) 0.0369(10) Uani 1 1 d . . . Cl22 Cl 0.28652(7) 0.1720(4) 0.87733(8) 0.1496(14) Uani 1 1 d . . . C23 C 0.12497(13) 0.3642(4) 0.72923(16) 0.0429(11) Uani 1 1 d . . . H23A H 0.1180 0.4305 0.7129 0.051 Uiso 1 1 calc R . . Cl23 Cl 0.23835(8) 0.0801(3) 0.90939(10) 0.1520(13) Uani 1 1 d . . . C24 C 0.10654(14) 0.2656(5) 0.71166(17) 0.0485(13) Uani 1 1 d . . . H24A H 0.0873 0.2643 0.6833 0.058 Uiso 1 1 calc R . . C25 C 0.11596(16) 0.1694(5) 0.7351(2) 0.0542(14) Uani 1 1 d . . . H25A H 0.1030 0.1019 0.7232 0.065 Uiso 1 1 calc R . . C26 C 0.14423(19) 0.1714(5) 0.7758(2) 0.0649(17) Uani 1 1 d . . . H26A H 0.1511 0.1048 0.7920 0.078 Uiso 1 1 calc R . . C27 C 0.16275(17) 0.2700(5) 0.79334(18) 0.0543(14) Uani 1 1 d . . . H27A H 0.1821 0.2704 0.8216 0.065 Uiso 1 1 calc R . . C28 C 0.20242(11) 0.5222(4) 0.76124(13) 0.0314(9) Uani 1 1 d . . . C29 C 0.20958(12) 0.6293(4) 0.75221(14) 0.0354(10) Uani 1 1 d . . . H29A H 0.1995 0.6917 0.7596 0.042 Uiso 1 1 calc R . . C30 C 0.23147(13) 0.6460(4) 0.73249(15) 0.0405(11) Uani 1 1 d . . . H30A H 0.2363 0.7197 0.7266 0.049 Uiso 1 1 calc R . . C31 C 0.24615(14) 0.5558(5) 0.72149(16) 0.0443(12) Uani 1 1 d . . . H31A H 0.2614 0.5673 0.7084 0.053 Uiso 1 1 calc R . . C32 C 0.23857(13) 0.4481(4) 0.72956(16) 0.0428(12) Uani 1 1 d . . . H32A H 0.2485 0.3859 0.7218 0.051 Uiso 1 1 calc R . . C33 C 0.21661(12) 0.4314(4) 0.74886(15) 0.0377(10) Uani 1 1 d . . . H33A H 0.2111 0.3575 0.7538 0.045 Uiso 1 1 calc R . . C34 C 0.27567(12) 0.6077(4) 0.85175(15) 0.0405(11) Uani 1 1 d . . . C35 C 0.28745(13) 0.7155(5) 0.84975(16) 0.0486(13) Uani 1 1 d . . . H35A H 0.2776 0.7774 0.8577 0.058 Uiso 1 1 calc R . . C36 C 0.31393(14) 0.7321(6) 0.83590(18) 0.0588(17) Uani 1 1 d . . . H36A H 0.3218 0.8056 0.8341 0.071 Uiso 1 1 calc R . . C37 C 0.32852(15) 0.6432(7) 0.82497(19) 0.070(2) Uani 1 1 d . . . H37A H 0.3464 0.6556 0.8154 0.084 Uiso 1 1 calc R . . C38 C 0.31785(15) 0.5377(7) 0.8275(2) 0.0668(18) Uani 1 1 d . . . H38A H 0.3282 0.4765 0.8198 0.080 Uiso 1 1 calc R . . C39 C 0.29156(14) 0.5188(5) 0.84158(18) 0.0536(14) Uani 1 1 d . . . H39A H 0.2846 0.4446 0.8441 0.064 Uiso 1 1 calc R . . C40 C 0.27021(13) 0.5431(4) 0.92409(15) 0.0411(11) Uani 1 1 d . . . C41 C 0.25313(15) 0.5177(5) 0.94876(17) 0.0535(14) Uani 1 1 d . . . H41A H 0.2266 0.5199 0.9367 0.064 Uiso 1 1 calc R . . C42 C 0.27430(18) 0.4898(6) 0.99010(19) 0.0646(16) Uani 1 1 d . . . H42A H 0.2624 0.4727 1.0065 0.078 Uiso 1 1 calc R . . C43 C 0.31266(17) 0.4861(5) 1.00814(18) 0.0621(16) Uani 1 1 d . . . H43A H 0.3270 0.4662 1.0368 0.075 Uiso 1 1 calc R . . C44 C 0.32999(17) 0.5109(6) 0.9851(2) 0.0659(17) Uani 1 1 d . . . H44A H 0.3565 0.5091 0.9978 0.079 Uiso 1 1 calc R . . C45 C 0.30908(14) 0.5390(5) 0.94271(18) 0.0528(14) Uani 1 1 d . . . H45A H 0.3214 0.5554 0.9266 0.063 Uiso 1 1 calc R . . C46 C 0.00997(12) 0.5971(4) 0.94815(13) 0.0298(9) Uani 1 1 d . . . H46A H -0.0025 0.5548 0.9615 0.036 Uiso 1 1 calc R . . H46B H 0.0371 0.5810 0.9635 0.036 Uiso 1 1 calc R . . C47 C 0.02992(11) 0.7812(3) 1.00571(13) 0.0288(9) Uani 1 1 d . . . C48 C 0.01428(12) 0.8131(4) 1.03094(14) 0.0357(10) Uani 1 1 d . . . H48A H -0.0121 0.8140 1.0197 0.043 Uiso 1 1 calc R . . C49 C 0.03677(14) 0.8437(4) 1.07232(16) 0.0398(11) Uani 1 1 d . . . H49A H 0.0256 0.8655 1.0891 0.048 Uiso 1 1 calc R . . C50 C 0.07507(14) 0.8427(4) 1.08943(15) 0.0398(11) Uani 1 1 d . . . H50A H 0.0903 0.8633 1.1179 0.048 Uiso 1 1 calc R . . C51 C 0.09136(13) 0.8110(4) 1.06446(15) 0.0403(11) Uani 1 1 d . . . H51A H 0.1178 0.8108 1.0759 0.048 Uiso 1 1 calc R . . C52 C 0.06894(13) 0.7801(4) 1.02322(15) 0.0375(10) Uani 1 1 d . . . H52A H 0.0801 0.7577 1.0065 0.045 Uiso 1 1 calc R . . C53 C -0.04550(12) 0.7592(4) 0.94359(14) 0.0328(10) Uani 1 1 d . . . C54 C -0.06245(12) 0.6745(4) 0.95538(14) 0.0360(10) Uani 1 1 d . . . H54A H -0.0500 0.6052 0.9653 0.043 Uiso 1 1 calc R . . C55 C -0.09754(13) 0.6918(4) 0.95259(16) 0.0435(12) Uani 1 1 d . . . H55A H -0.1092 0.6334 0.9599 0.052 Uiso 1 1 calc R . . C56 C -0.11540(15) 0.7933(5) 0.93930(19) 0.0536(14) Uani 1 1 d . . . H56A H -0.1390 0.8054 0.9382 0.064 Uiso 1 1 calc R . . C57 C -0.09903(15) 0.8766(5) 0.9277(2) 0.0558(15) Uani 1 1 d . . . H57A H -0.1115 0.9460 0.9181 0.067 Uiso 1 1 calc R . . C58 C -0.06403(14) 0.8595(4) 0.92994(18) 0.0460(12) Uani 1 1 d . . . H58A H -0.0529 0.9179 0.9220 0.055 Uiso 1 1 calc R . . C59 C -0.05921(12) 0.5422(4) 0.87592(13) 0.0303(9) Uani 1 1 d . . . C60 C -0.07332(12) 0.4539(4) 0.88912(15) 0.0356(10) Uani 1 1 d . . . H60A H -0.0570 0.3957 0.9054 0.043 Uiso 1 1 calc R . . C61 C -0.11066(13) 0.4497(4) 0.87883(16) 0.0408(11) Uani 1 1 d . . . H61A H -0.1201 0.3884 0.8876 0.049 Uiso 1 1 calc R . . C62 C -0.13440(13) 0.5358(4) 0.85545(16) 0.0429(12) Uani 1 1 d . . . H62A H -0.1600 0.5340 0.8488 0.051 Uiso 1 1 calc R . . C63 C -0.12106(12) 0.6235(4) 0.84185(15) 0.0391(11) Uani 1 1 d . . . H63A H -0.1374 0.6818 0.8258 0.047 Uiso 1 1 calc R . . C64 C -0.08355(12) 0.6267(4) 0.85167(14) 0.0358(10) Uani 1 1 d . . . H64A H -0.0744 0.6866 0.8418 0.043 Uiso 1 1 calc R . . C65 C 0.00587(12) 0.4113(4) 0.89435(14) 0.0302(9) Uani 1 1 d . . . C66 C 0.03572(13) 0.3634(4) 0.92918(15) 0.0363(10) Uani 1 1 d . . . H66A H 0.0474 0.4035 0.9549 0.044 Uiso 1 1 calc R . . C67 C 0.04854(14) 0.2585(4) 0.92683(17) 0.0417(11) Uani 1 1 d . . . H67A H 0.0688 0.2269 0.9509 0.050 Uiso 1 1 calc R . . C68 C 0.03220(15) 0.1992(4) 0.88976(18) 0.0462(12) Uani 1 1 d . . . H68A H 0.0414 0.1273 0.8882 0.055 Uiso 1 1 calc R . . C69 C 0.00237(15) 0.2449(4) 0.85493(17) 0.0455(12) Uani 1 1 d . . . H69A H -0.0093 0.2039 0.8295 0.055 Uiso 1 1 calc R . . C70 C -0.01040(14) 0.3501(4) 0.85717(15) 0.0384(11) Uani 1 1 d . . . H70A H -0.0306 0.3813 0.8329 0.046 Uiso 1 1 calc R . . O101 O 0.20852(11) 0.9100(3) 0.81637(15) 0.0635(11) Uani 1 1 d . . . C101 C 0.20612(14) 0.8358(5) 0.83469(18) 0.0446(12) Uani 1 1 d . . . O102 O 0.23241(13) 0.7950(4) 0.94814(14) 0.0766(13) Uani 1 1 d . . . C102 C 0.21874(15) 0.7672(5) 0.91354(18) 0.0495(13) Uani 1 1 d . . . O201 O 0.07216(10) 0.5292(3) 0.75992(14) 0.0604(11) Uani 1 1 d . . . C201 C 0.10026(14) 0.5756(4) 0.77441(16) 0.0427(12) Uani 1 1 d . . . O202 O 0.13089(11) 0.8175(3) 0.73439(12) 0.0583(10) Uani 1 1 d . . . C202 C 0.13643(13) 0.7488(4) 0.75823(16) 0.0420(11) Uani 1 1 d . . . O301 O -0.04638(11) 0.9631(4) 0.84616(12) 0.0610(11) Uani 1 1 d . . . C301 C -0.02138(14) 0.9123(4) 0.87001(15) 0.0395(11) Uani 1 1 d . . . O302 O 0.06699(12) 1.0012(3) 0.96419(14) 0.0701(13) Uani 1 1 d . . . C302 C 0.04734(13) 0.9367(4) 0.94065(16) 0.0402(11) Uani 1 1 d . . . O401 O -0.04592(11) 0.7661(4) 0.78141(12) 0.0621(11) Uani 1 1 d . . . C401 C -0.02560(14) 0.7233(4) 0.81184(16) 0.0430(12) Uani 1 1 d . . . O402 O 0.04435(15) 0.4975(4) 0.83188(19) 0.0900(18) Uani 1 1 d . . . C402 C 0.03082(16) 0.5656(5) 0.84207(19) 0.0510(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0337(3) 0.0358(4) 0.0363(4) 0.0035(3) 0.0215(3) -0.0024(2) P1 0.0300(5) 0.0344(6) 0.0300(6) 0.0042(5) 0.0172(5) 0.0007(5) O1 0.067(2) 0.057(2) 0.048(2) 0.0008(18) 0.0406(19) -0.0135(19) C1 0.074(4) 0.036(3) 0.062(4) 0.006(2) 0.049(3) -0.003(2) C01 0.130(10) 0.082(8) 0.104(10) 0.000 0.065(9) 0.000 Co2 0.0299(3) 0.0364(3) 0.0325(3) 0.0072(3) 0.0178(3) 0.0032(2) P2 0.0302(6) 0.0416(7) 0.0326(6) 0.0065(5) 0.0164(5) 0.0001(5) O2 0.059(2) 0.044(2) 0.043(2) 0.007(2) 0.024(2) 0.0124(18) C2 0.045(3) 0.039(3) 0.041(3) 0.004(2) 0.026(2) -0.001(2) C02 0.084(5) 0.141(8) 0.060(5) 0.018(5) 0.026(4) 0.042(5) Co3 0.0286(3) 0.0262(3) 0.0318(3) 0.0022(2) 0.0161(3) 0.0014(2) P3 0.0295(5) 0.0286(6) 0.0284(6) -0.0006(4) 0.0158(5) 0.0000(4) C3 0.036(2) 0.032(2) 0.033(2) -0.0014(19) 0.021(2) -0.0032(18) Co4 0.0363(3) 0.0318(3) 0.0304(3) 0.0003(2) 0.0207(3) -0.0019(2) P4 0.0295(5) 0.0277(6) 0.0275(6) -0.0001(4) 0.0148(5) -0.0016(4) C4 0.034(2) 0.037(2) 0.033(2) 0.0004(19) 0.0225(19) -0.0040(19) C5 0.035(2) 0.036(3) 0.042(3) 0.003(2) 0.025(2) -0.0054(19) C6 0.045(3) 0.032(3) 0.075(4) 0.004(2) 0.041(3) -0.001(2) C7 0.055(3) 0.082(5) 0.057(4) -0.026(3) 0.030(3) -0.007(3) C8 0.068(4) 0.036(3) 0.104(5) 0.013(3) 0.065(4) 0.004(3) C9 0.048(3) 0.031(3) 0.059(3) 0.003(2) 0.036(3) 0.000(2) C10 0.056(3) 0.037(3) 0.064(4) 0.014(2) 0.043(3) 0.007(2) C11 0.054(3) 0.037(3) 0.061(3) 0.015(2) 0.040(3) 0.010(2) Cl11 0.138(2) 0.177(3) 0.0822(16) -0.0153(17) 0.0408(15) -0.035(2) C12 0.033(2) 0.026(2) 0.045(3) 0.0017(19) 0.024(2) 0.0013(18) C13 0.028(2) 0.027(2) 0.039(3) 0.0014(19) 0.0189(19) 0.0003(17) C14 0.035(2) 0.029(2) 0.041(3) 0.000(2) 0.025(2) -0.0011(19) C15 0.030(2) 0.038(3) 0.035(3) 0.003(2) 0.016(2) 0.0035(19) C16 0.038(2) 0.048(3) 0.032(3) 0.004(2) 0.014(2) 0.011(2) C17 0.068(4) 0.069(4) 0.043(3) -0.006(3) 0.017(3) 0.019(3) C18 0.035(3) 0.070(4) 0.054(3) 0.006(3) 0.019(2) 0.007(3) C19 0.196(9) 0.057(4) 0.100(6) -0.034(4) 0.110(7) -0.054(5) C20 0.098(5) 0.058(4) 0.110(6) 0.041(4) 0.065(5) 0.029(4) C21 0.030(2) 0.037(2) 0.033(2) 0.0027(19) 0.0188(19) -0.0001(18) Cl21 0.178(3) 0.109(2) 0.196(4) -0.034(2) 0.068(3) 0.003(2) C22 0.039(2) 0.037(3) 0.046(3) -0.002(2) 0.030(2) -0.002(2) Cl22 0.0917(15) 0.297(5) 0.0697(14) 0.013(2) 0.0465(12) 0.009(2) C23 0.040(3) 0.045(3) 0.047(3) 0.000(2) 0.023(2) 0.000(2) Cl23 0.1084(18) 0.219(4) 0.133(2) 0.062(2) 0.0608(18) 0.010(2) C24 0.043(3) 0.058(3) 0.047(3) -0.012(3) 0.023(2) -0.004(2) C25 0.060(3) 0.041(3) 0.075(4) -0.011(3) 0.042(3) -0.016(3) C26 0.084(4) 0.044(3) 0.071(4) 0.006(3) 0.040(4) -0.016(3) C27 0.072(4) 0.048(3) 0.046(3) 0.009(3) 0.030(3) -0.007(3) C28 0.030(2) 0.040(3) 0.025(2) 0.0042(19) 0.0137(18) 0.0027(18) C29 0.037(2) 0.042(3) 0.033(2) 0.000(2) 0.020(2) -0.001(2) C30 0.045(3) 0.047(3) 0.038(3) -0.001(2) 0.026(2) -0.010(2) C31 0.043(3) 0.058(3) 0.045(3) -0.004(2) 0.031(2) -0.004(2) C32 0.045(3) 0.050(3) 0.044(3) -0.005(2) 0.030(2) 0.001(2) C33 0.037(2) 0.041(3) 0.036(3) 0.001(2) 0.017(2) 0.001(2) C34 0.030(2) 0.057(3) 0.031(3) 0.008(2) 0.012(2) -0.001(2) C35 0.032(2) 0.069(4) 0.039(3) 0.014(3) 0.011(2) -0.006(2) C36 0.035(3) 0.088(5) 0.046(3) 0.017(3) 0.013(2) -0.017(3) C37 0.033(3) 0.132(7) 0.044(3) 0.011(4) 0.017(3) -0.015(4) C38 0.040(3) 0.109(6) 0.059(4) -0.008(4) 0.030(3) -0.004(3) C39 0.037(3) 0.072(4) 0.056(3) 0.001(3) 0.026(3) -0.002(3) C40 0.039(2) 0.045(3) 0.034(3) 0.005(2) 0.012(2) 0.000(2) C41 0.048(3) 0.073(4) 0.037(3) 0.017(3) 0.019(2) 0.009(3) C42 0.073(4) 0.079(4) 0.043(3) 0.015(3) 0.028(3) 0.005(3) C43 0.068(4) 0.059(4) 0.036(3) 0.010(3) 0.005(3) -0.003(3) C44 0.047(3) 0.068(4) 0.057(4) 0.014(3) 0.004(3) -0.004(3) C45 0.039(3) 0.061(4) 0.051(3) 0.009(3) 0.015(2) -0.006(2) C46 0.032(2) 0.030(2) 0.031(2) 0.0009(18) 0.0180(19) -0.0007(17) C47 0.034(2) 0.025(2) 0.030(2) 0.0011(17) 0.0174(19) -0.0013(17) C48 0.035(2) 0.040(3) 0.033(2) -0.004(2) 0.017(2) -0.007(2) C49 0.054(3) 0.035(3) 0.042(3) -0.004(2) 0.032(2) -0.002(2) C50 0.051(3) 0.035(3) 0.030(2) -0.003(2) 0.017(2) -0.006(2) C51 0.039(2) 0.042(3) 0.034(3) -0.002(2) 0.013(2) -0.003(2) C52 0.041(2) 0.041(3) 0.033(2) -0.001(2) 0.020(2) 0.004(2) C53 0.036(2) 0.035(2) 0.034(2) -0.0065(19) 0.022(2) -0.0006(19) C54 0.038(2) 0.042(3) 0.031(2) -0.002(2) 0.018(2) -0.002(2) C55 0.044(3) 0.048(3) 0.049(3) -0.010(2) 0.032(2) -0.013(2) C56 0.042(3) 0.063(4) 0.068(4) -0.009(3) 0.036(3) 0.001(3) C57 0.045(3) 0.043(3) 0.087(4) 0.007(3) 0.038(3) 0.012(2) C58 0.047(3) 0.038(3) 0.064(4) 0.002(2) 0.035(3) 0.001(2) C59 0.033(2) 0.032(2) 0.027(2) -0.0010(18) 0.0146(18) 0.0030(18) C60 0.038(2) 0.031(2) 0.038(3) 0.002(2) 0.019(2) -0.0010(19) C61 0.039(2) 0.043(3) 0.044(3) 0.003(2) 0.023(2) -0.004(2) C62 0.031(2) 0.052(3) 0.044(3) 0.001(2) 0.017(2) 0.001(2) C63 0.033(2) 0.046(3) 0.035(3) 0.002(2) 0.013(2) 0.006(2) C64 0.039(2) 0.037(3) 0.031(2) 0.000(2) 0.016(2) 0.001(2) C65 0.033(2) 0.030(2) 0.033(2) 0.0011(18) 0.0206(19) 0.0002(18) C66 0.039(2) 0.033(2) 0.040(3) 0.002(2) 0.021(2) -0.0015(19) C67 0.043(3) 0.034(3) 0.050(3) 0.009(2) 0.024(2) 0.004(2) C68 0.061(3) 0.030(3) 0.063(4) 0.003(2) 0.042(3) 0.006(2) C69 0.067(3) 0.034(3) 0.044(3) -0.008(2) 0.033(3) -0.003(2) C70 0.047(3) 0.034(3) 0.033(3) 0.000(2) 0.018(2) -0.002(2) O101 0.068(2) 0.052(2) 0.090(3) 0.024(2) 0.054(2) -0.0007(19) C101 0.039(3) 0.049(3) 0.057(3) 0.004(3) 0.032(2) 0.002(2) O102 0.080(3) 0.093(4) 0.057(3) -0.024(3) 0.033(2) -0.015(3) C102 0.051(3) 0.052(3) 0.050(3) -0.005(3) 0.028(3) -0.013(3) O201 0.0361(19) 0.063(3) 0.077(3) -0.004(2) 0.0227(19) -0.0072(18) C201 0.040(3) 0.049(3) 0.039(3) 0.006(2) 0.019(2) 0.007(2) O202 0.075(3) 0.054(2) 0.051(2) 0.025(2) 0.034(2) 0.009(2) C202 0.042(3) 0.048(3) 0.041(3) 0.003(2) 0.024(2) 0.007(2) O301 0.054(2) 0.070(3) 0.045(2) 0.012(2) 0.0123(19) 0.028(2) C301 0.044(3) 0.045(3) 0.038(3) -0.003(2) 0.025(2) 0.003(2) O302 0.073(3) 0.042(2) 0.062(3) 0.002(2) 0.004(2) -0.012(2) C302 0.043(3) 0.028(2) 0.041(3) 0.010(2) 0.014(2) 0.003(2) O401 0.062(2) 0.073(3) 0.032(2) 0.012(2) 0.0059(18) -0.009(2) C401 0.053(3) 0.047(3) 0.037(3) -0.006(2) 0.027(3) -0.015(2) O402 0.123(4) 0.055(3) 0.157(5) -0.042(3) 0.119(4) -0.024(3) C402 0.068(3) 0.044(3) 0.063(4) -0.009(3) 0.049(3) -0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C102 1.776(6) . ? Co1 C101 1.783(5) . ? Co1 C5 1.967(4) . ? Co1 C4 1.972(4) . ? Co1 P2 2.2307(13) . ? Co1 Co2 2.4752(9) . ? P1 C28 1.831(4) . ? P1 C22 1.832(5) . ? P1 C21 1.847(4) . ? P1 Co2 2.2331(13) . ? O1 C1 1.441(6) . ? C1 C2 1.472(7) . ? C1 C19 1.528(9) . ? C1 C20 1.536(9) . ? C01 Cl11 1.741(7) . ? C01 Cl11 1.741(7) 2_556 ? Co2 C201 1.781(5) . ? Co2 C202 1.807(5) . ? Co2 C4 1.958(4) . ? Co2 C5 1.976(5) . ? P2 C40 1.834(5) . ? P2 C34 1.837(5) . ? P2 C21 1.836(5) . ? O2 C16 1.430(7) . ? C2 C3 1.198(6) . ? C02 Cl21 1.545(10) . ? C02 Cl22 1.720(8) . ? C02 Cl23 1.751(10) . ? Co3 C302 1.769(5) . ? Co3 C301 1.789(5) . ? Co3 C12 1.965(4) . ? Co3 C13 1.974(4) . ? Co3 P3 2.2512(13) . ? Co3 Co4 2.4749(8) . ? P3 C53 1.829(4) . ? P3 C46 1.834(4) . ? P3 C47 1.837(4) . ? C3 C4 1.398(6) . ? Co4 C402 1.773(6) . ? Co4 C401 1.800(6) . ? Co4 C12 1.956(4) . ? Co4 C13 1.962(4) . ? Co4 P4 2.2005(12) . ? P4 C65 1.824(4) . ? P4 C59 1.830(4) . ? P4 C46 1.844(4) . ? C4 C5 1.363(7) . ? C5 C6 1.509(7) . ? C6 C9 1.503(7) . ? C6 C8 1.524(7) . ? C6 C7 1.604(8) . ? C9 C10 1.510(7) . ? C10 C11 1.327(7) . ? C10 C12 1.479(7) . ? C12 C13 1.367(6) . ? C13 C14 1.405(6) . ? C14 C15 1.197(6) . ? C15 C16 1.491(6) . ? C16 C17 1.514(7) . ? C16 C18 1.520(7) . ? C22 C27 1.385(7) . ? C22 C23 1.390(7) . ? C23 C24 1.382(7) . ? C24 C25 1.372(8) . ? C25 C26 1.375(9) . ? C26 C27 1.382(8) . ? C28 C29 1.388(7) . ? C28 C33 1.400(7) . ? C29 C30 1.393(6) . ? C30 C31 1.381(7) . ? C31 C32 1.389(7) . ? C32 C33 1.382(6) . ? C34 C39 1.382(8) . ? C34 C35 1.391(8) . ? C35 C36 1.398(7) . ? C36 C37 1.364(10) . ? C37 C38 1.354(10) . ? C38 C39 1.400(8) . ? C40 C45 1.393(7) . ? C40 C41 1.399(7) . ? C41 C42 1.368(8) . ? C42 C43 1.375(9) . ? C43 C44 1.354(9) . ? C44 C45 1.398(8) . ? C47 C48 1.389(6) . ? C47 C52 1.400(6) . ? C48 C49 1.384(7) . ? C49 C50 1.374(7) . ? C50 C51 1.401(7) . ? C51 C52 1.381(7) . ? C53 C58 1.379(7) . ? C53 C54 1.400(7) . ? C54 C55 1.395(6) . ? C55 C56 1.381(8) . ? C56 C57 1.370(8) . ? C57 C58 1.399(7) . ? C59 C60 1.390(6) . ? C59 C64 1.396(6) . ? C60 C61 1.380(6) . ? C61 C62 1.392(7) . ? C62 C63 1.375(7) . ? C63 C64 1.390(6) . ? C65 C66 1.393(6) . ? C65 C70 1.394(6) . ? C66 C67 1.378(7) . ? C67 C68 1.380(7) . ? C68 C69 1.382(8) . ? C69 C70 1.379(7) . ? O101 C101 1.141(6) . ? O102 C102 1.153(7) . ? O201 C201 1.148(6) . ? O202 C202 1.135(6) . ? O301 C301 1.147(6) . ? O302 C302 1.147(6) . ? O401 C401 1.139(6) . ? O402 C402 1.138(7) . ? 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 C102 Co1 C101 102.5(3) . . ? C102 Co1 C5 100.9(2) . . ? C101 Co1 C5 102.9(2) . . ? C102 Co1 C4 102.0(2) . . ? C101 Co1 C4 139.4(2) . . ? C5 Co1 C4 40.48(19) . . ? C102 Co1 P2 97.63(19) . . ? C101 Co1 P2 108.20(16) . . ? C5 Co1 P2 139.14(14) . . ? C4 Co1 P2 100.10(14) . . ? C102 Co1 Co2 150.09(17) . . ? C101 Co1 Co2 95.53(18) . . ? C5 Co1 Co2 51.29(14) . . ? C4 Co1 Co2 50.71(13) . . ? P2 Co1 Co2 99.20(4) . . ? C28 P1 C22 101.7(2) . . ? C28 P1 C21 101.56(19) . . ? C22 P1 C21 102.4(2) . . ? C28 P1 Co2 119.15(15) . . ? C22 P1 Co2 119.49(15) . . ? C21 P1 Co2 109.98(15) . . ? O1 C1 C2 109.4(4) . . ? O1 C1 C19 108.6(5) . . ? C2 C1 C19 110.3(5) . . ? O1 C1 C20 104.6(5) . . ? C2 C1 C20 110.9(5) . . ? C19 C1 C20 113.0(6) . . ? Cl11 C01 Cl11 111.7(7) . 2_556 ? C201 Co2 C202 100.5(2) . . ? C201 Co2 C4 98.4(2) . . ? C202 Co2 C4 142.5(2) . . ? C201 Co2 C5 104.4(2) . . ? C202 Co2 C5 103.0(2) . . ? C4 Co2 C5 40.53(19) . . ? C201 Co2 P1 96.43(17) . . ? C202 Co2 P1 110.00(16) . . ? C4 Co2 P1 99.62(14) . . ? C5 Co2 P1 136.69(14) . . ? C201 Co2 Co1 149.26(17) . . ? C202 Co2 Co1 102.91(17) . . ? C4 Co2 Co1 51.23(13) . . ? C5 Co2 Co1 50.95(13) . . ? P1 Co2 Co1 93.94(4) . . ? C40 P2 C34 101.3(2) . . ? C40 P2 C21 103.6(2) . . ? C34 P2 C21 104.6(2) . . ? C40 P2 Co1 115.88(17) . . ? C34 P2 Co1 122.01(17) . . ? C21 P2 Co1 107.58(14) . . ? C3 C2 C1 179.4(6) . . ? Cl21 C02 Cl22 106.4(6) . . ? Cl21 C02 Cl23 104.7(5) . . ? Cl22 C02 Cl23 114.5(5) . . ? C302 Co3 C301 102.1(2) . . ? C302 Co3 C12 101.7(2) . . ? C301 Co3 C12 104.9(2) . . ? C302 Co3 C13 100.0(2) . . ? C301 Co3 C13 142.5(2) . . ? C12 Co3 C13 40.60(18) . . ? C302 Co3 P3 97.74(17) . . ? C301 Co3 P3 106.63(16) . . ? C12 Co3 P3 138.26(13) . . ? C13 Co3 P3 99.89(13) . . ? C302 Co3 Co4 149.14(17) . . ? C301 Co3 Co4 99.09(16) . . ? C12 Co3 Co4 50.71(13) . . ? C13 Co3 Co4 50.82(13) . . ? P3 Co3 Co4 97.45(4) . . ? C53 P3 C46 105.6(2) . . ? C53 P3 C47 100.81(19) . . ? C46 P3 C47 103.09(19) . . ? C53 P3 Co3 121.61(16) . . ? C46 P3 Co3 107.67(14) . . ? C47 P3 Co3 116.18(14) . . ? C2 C3 C4 174.6(5) . . ? C402 Co4 C401 101.3(3) . . ? C402 Co4 C12 104.7(2) . . ? C401 Co4 C12 97.7(2) . . ? C402 Co4 C13 100.0(2) . . ? C401 Co4 C13 137.3(2) . . ? C12 Co4 C13 40.82(18) . . ? C402 Co4 P4 96.19(17) . . ? C401 Co4 P4 113.23(15) . . ? C12 Co4 P4 138.29(14) . . ? C13 Co4 P4 100.68(13) . . ? C402 Co4 Co3 150.62(19) . . ? C401 Co4 Co3 98.66(17) . . ? C12 Co4 Co3 51.03(13) . . ? C13 Co4 Co3 51.25(12) . . ? P4 Co4 Co3 95.45(4) . . ? C65 P4 C59 103.3(2) . . ? C65 P4 C46 105.0(2) . . ? C59 P4 C46 102.43(19) . . ? C65 P4 Co4 113.79(14) . . ? C59 P4 Co4 120.89(15) . . ? C46 P4 Co4 109.82(14) . . ? C5 C4 C3 142.6(4) . . ? C5 C4 Co2 70.5(3) . . ? C3 C4 Co2 129.2(3) . . ? C5 C4 Co1 69.5(3) . . ? C3 C4 Co1 138.5(3) . . ? Co2 C4 Co1 78.06(15) . . ? C4 C5 C6 139.8(4) . . ? C4 C5 Co1 70.0(3) . . ? C6 C5 Co1 133.4(3) . . ? C4 C5 Co2 69.0(3) . . ? C6 C5 Co2 138.1(4) . . ? Co1 C5 Co2 77.76(16) . . ? C9 C6 C5 109.2(4) . . ? C9 C6 C8 113.8(5) . . ? C5 C6 C8 110.9(4) . . ? C9 C6 C7 105.4(4) . . ? C5 C6 C7 108.4(4) . . ? C8 C6 C7 108.8(5) . . ? C6 C9 C10 117.9(4) . . ? C11 C10 C12 120.6(4) . . ? C11 C10 C9 123.4(5) . . ? C12 C10 C9 115.6(4) . . ? C13 C12 C10 144.5(4) . . ? C13 C12 Co4 69.8(3) . . ? C10 C12 Co4 122.8(4) . . ? C13 C12 Co3 70.0(3) . . ? C10 C12 Co3 141.4(3) . . ? Co4 C12 Co3 78.27(15) . . ? C12 C13 C14 141.8(4) . . ? C12 C13 Co4 69.4(3) . . ? C14 C13 Co4 134.9(3) . . ? C12 C13 Co3 69.4(2) . . ? C14 C13 Co3 134.8(3) . . ? Co4 C13 Co3 77.94(15) . . ? C15 C14 C13 177.0(5) . . ? C14 C15 C16 174.2(5) . . ? O2 C16 C15 110.3(4) . . ? O2 C16 C17 105.3(5) . . ? C15 C16 C17 110.0(4) . . ? O2 C16 C18 110.4(4) . . ? C15 C16 C18 109.1(4) . . ? C17 C16 C18 111.7(5) . . ? P2 C21 P1 108.5(2) . . ? C27 C22 C23 117.7(5) . . ? C27 C22 P1 123.9(4) . . ? C23 C22 P1 118.4(4) . . ? C24 C23 C22 121.2(5) . . ? C25 C24 C23 120.1(5) . . ? C24 C25 C26 119.7(5) . . ? C25 C26 C27 120.2(6) . . ? C26 C27 C22 121.1(5) . . ? C29 C28 C33 118.6(4) . . ? C29 C28 P1 120.0(3) . . ? C33 C28 P1 121.2(3) . . ? C28 C29 C30 120.6(4) . . ? C31 C30 C29 120.1(5) . . ? C30 C31 C32 119.9(4) . . ? C33 C32 C31 120.1(5) . . ? C32 C33 C28 120.7(5) . . ? C39 C34 C35 119.1(5) . . ? C39 C34 P2 122.5(4) . . ? C35 C34 P2 118.3(4) . . ? C34 C35 C36 119.5(6) . . ? C37 C36 C35 120.4(6) . . ? C38 C37 C36 120.8(6) . . ? C37 C38 C39 120.0(7) . . ? C34 C39 C38 120.2(6) . . ? C45 C40 C41 118.3(5) . . ? C45 C40 P2 123.0(4) . . ? C41 C40 P2 118.6(4) . . ? C42 C41 C40 120.5(5) . . ? C41 C42 C43 120.7(6) . . ? C44 C43 C42 120.1(5) . . ? C43 C44 C45 120.4(5) . . ? C40 C45 C44 120.0(5) . . ? P3 C46 P4 108.2(2) . . ? C48 C47 C52 118.4(4) . . ? C48 C47 P3 123.1(3) . . ? C52 C47 P3 118.5(3) . . ? C49 C48 C47 120.8(4) . . ? C50 C49 C48 120.7(4) . . ? C49 C50 C51 119.3(4) . . ? C52 C51 C50 119.9(4) . . ? C51 C52 C47 120.8(4) . . ? C58 C53 C54 118.5(4) . . ? C58 C53 P3 118.4(4) . . ? C54 C53 P3 122.9(4) . . ? C55 C54 C53 120.2(5) . . ? C56 C55 C54 120.4(5) . . ? C57 C56 C55 119.8(5) . . ? C56 C57 C58 120.1(5) . . ? C53 C58 C57 121.0(5) . . ? C60 C59 C64 118.9(4) . . ? C60 C59 P4 121.6(3) . . ? C64 C59 P4 119.3(3) . . ? C61 C60 C59 120.9(4) . . ? C60 C61 C62 119.5(5) . . ? C63 C62 C61 120.5(4) . . ? C62 C63 C64 119.9(4) . . ? C63 C64 C59 120.3(4) . . ? C66 C65 C70 117.9(4) . . ? C66 C65 P4 123.6(3) . . ? C70 C65 P4 118.0(3) . . ? C67 C66 C65 120.8(5) . . ? C66 C67 C68 120.6(5) . . ? C69 C68 C67 119.5(5) . . ? C68 C69 C70 120.0(5) . . ? C69 C70 C65 121.2(5) . . ? O101 C101 Co1 175.5(5) . . ? O102 C102 Co1 178.1(6) . . ? O201 C201 Co2 178.5(5) . . ? O202 C202 Co2 177.1(5) . . ? O301 C301 Co3 177.7(4) . . ? O302 C302 Co3 177.6(5) . . ? O401 C401 Co4 172.0(4) . . ? O402 C402 Co4 177.3(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.431 _refine_diff_density_min -1.413 _refine_diff_density_rms 0.147 #===END data_mm0207i_COMPOUND_17 _database_code_depnum_ccdc_archive 'CCDC 228899' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Cl1.50 Co4 O13 S2' _chemical_formula_weight 997.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.4650(4) _cell_length_b 12.9587(5) _cell_length_c 13.8733(4) _cell_angle_alpha 69.498(2) _cell_angle_beta 73.291(2) _cell_angle_gamma 81.816(2) _cell_volume 2008.22(12) _cell_formula_units_Z 2 _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 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1003 _exptl_absorpt_coefficient_mu 1.887 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8052 _exptl_absorpt_correction_T_max 0.8337 _exptl_absorpt_process_details ? _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18407 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9128 _reflns_number_gt 5755 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+2.9100P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9128 _refine_ls_number_parameters 488 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1477 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C0 C 0.9689(17) -0.8867(14) 0.8476(11) 0.1298(10) Uiso 0.50 1 d PD A 1 H0 H 1.0446 -0.9216 0.8534 0.156 Uiso 0.50 1 calc PR A 1 Co1 Co 0.93637(5) -0.32990(5) 0.63720(5) 0.02979(17) Uani 1 1 d . . . S1 S 0.28177(12) 0.05752(13) 0.75165(12) 0.0529(4) Uani 1 1 d . . . O1 O 0.4331(4) -0.2365(4) 0.7581(4) 0.0856(16) Uani 1 1 d . . . C1 C 0.8472(4) -0.3583(4) 0.7858(3) 0.0283(10) Uani 1 1 d . . . Cl1 Cl 0.9002(5) -0.8775(5) 0.9653(4) 0.1298(10) Uiso 0.50 1 d PD A 1 Co2 Co 0.98738(5) -0.30091(5) 0.78386(4) 0.02867(16) Uani 1 1 d . . . S2 S 0.66732(12) -0.47687(11) 0.81102(12) 0.0473(3) Uani 1 1 d . . . C2 C 0.8505(3) -0.2492(4) 0.7325(3) 0.0250(9) Uani 1 1 d . . . Cl2 Cl 0.9889(5) -0.7635(5) 0.7468(4) 0.1298(10) Uiso 0.50 1 d PD A 1 Co3 Co 0.51256(5) 0.25688(5) 0.57257(4) 0.02370(15) Uani 1 1 d . . . C3 C 0.7828(3) -0.1457(3) 0.7194(3) 0.0245(9) Uani 1 1 d . . . Cl3 Cl 0.9014(5) -0.9739(5) 0.8118(5) 0.1298(10) Uiso 0.50 1 d PD A 1 Co4 Co 0.56459(5) 0.28341(5) 0.72046(4) 0.02626(16) Uani 1 1 d . . . C4 C 0.7268(4) -0.1122(4) 0.8072(3) 0.0358(12) Uani 1 1 d . . . H4 H 0.7359 -0.1559 0.8757 0.043 Uiso 1 1 calc R . . C5 C 0.6589(4) -0.0177(4) 0.7970(3) 0.0368(12) Uani 1 1 d . . . H5 H 0.6226 0.0030 0.8582 0.044 Uiso 1 1 calc R . . C6 C 0.6424(4) 0.0483(3) 0.6980(3) 0.0244(9) Uani 1 1 d . . . C7 C 0.6998(4) 0.0170(3) 0.6105(3) 0.0259(9) Uani 1 1 d . . . H7 H 0.6913 0.0613 0.5420 0.031 Uiso 1 1 calc R . . C8 C 0.7693(4) -0.0769(4) 0.6204(3) 0.0277(10) Uani 1 1 d . . . H8 H 0.8087 -0.0952 0.5585 0.033 Uiso 1 1 calc R . . C9 C 0.5647(4) 0.1446(3) 0.6891(3) 0.0243(9) Uani 1 1 d . . . C10 C 0.4587(4) 0.1791(3) 0.7261(3) 0.0262(10) Uani 1 1 d . . . C11 C 0.3476(4) 0.1410(4) 0.8002(3) 0.0326(11) Uani 1 1 d . . . C12 C 0.2618(4) 0.2381(5) 0.8016(5) 0.0566(17) Uani 1 1 d . . . H12C H 0.2846 0.2856 0.8332 0.085 Uiso 1 1 calc R . . H12B H 0.1879 0.2102 0.8439 0.085 Uiso 1 1 calc R . . H12A H 0.2582 0.2808 0.7286 0.085 Uiso 1 1 calc R . . C13 C 0.3603(5) 0.0771(5) 0.9122(4) 0.0620(18) Uani 1 1 d . . . H13C H 0.3893 0.1253 0.9389 0.093 Uiso 1 1 calc R . . H13B H 0.4127 0.0134 0.9103 0.093 Uiso 1 1 calc R . . H13A H 0.2871 0.0517 0.9594 0.093 Uiso 1 1 calc R . . C14 C 0.3799(6) -0.0521(6) 0.7308(8) 0.106(3) Uani 1 1 d . . . H14B H 0.3872 -0.0527 0.6580 0.127 Uiso 1 1 calc R . . H14A H 0.4537 -0.0339 0.7323 0.127 Uiso 1 1 calc R . . C15 C 0.3582(6) -0.1599(6) 0.8012(5) 0.084(3) Uani 1 1 d . . . H15B H 0.2797 -0.1761 0.8115 0.101 Uiso 1 1 calc R . . H15A H 0.3689 -0.1669 0.8713 0.101 Uiso 1 1 calc R . . C16 C 0.4919(5) -0.3144(5) 0.8239(5) 0.0559(16) Uani 1 1 d . . . H16B H 0.4458 -0.3789 0.8684 0.067 Uiso 1 1 calc R . . H16A H 0.5116 -0.2825 0.8714 0.067 Uiso 1 1 calc R . . C17 C 0.5957(5) -0.3485(4) 0.7536(4) 0.0461(13) Uani 1 1 d . . . H17B H 0.6493 -0.2891 0.7269 0.055 Uiso 1 1 calc R . . H17A H 0.5757 -0.3532 0.6912 0.055 Uiso 1 1 calc R . . C18 C 0.7690(4) -0.4441(4) 0.8684(4) 0.0385(12) Uani 1 1 d . . . C19 C 0.7028(5) -0.4041(5) 0.9617(4) 0.0537(15) Uani 1 1 d . . . H19C H 0.7550 -0.3907 0.9966 0.081 Uiso 1 1 calc R . . H19B H 0.6513 -0.4605 1.0130 0.081 Uiso 1 1 calc R . . H19A H 0.6599 -0.3356 0.9349 0.081 Uiso 1 1 calc R . . C20 C 0.8321(5) -0.5535(4) 0.9090(5) 0.0606(17) Uani 1 1 d . . . H20C H 0.8836 -0.5441 0.9468 0.091 Uiso 1 1 calc R . . H20B H 0.8748 -0.5775 0.8487 0.091 Uiso 1 1 calc R . . H20A H 0.7784 -0.6091 0.9577 0.091 Uiso 1 1 calc R . . C51 C 0.8968(13) -0.8545(12) 0.8080(10) 0.082(2) Uiso 0.50 1 d PD B 2 H51A H 0.8946 -0.7938 0.8354 0.122 Uiso 0.50 1 calc PR B 2 H51B H 0.8203 -0.8688 0.8119 0.122 Uiso 0.50 1 calc PR B 2 H51C H 0.9413 -0.8343 0.7338 0.122 Uiso 0.50 1 calc PR B 2 C52 C 0.9506(13) -0.9591(12) 0.8757(10) 0.082(2) Uiso 0.50 1 d PD B 2 H52A H 0.8984 -1.0192 0.8992 0.098 Uiso 0.50 1 calc PR B 2 H52B H 1.0195 -0.9796 0.8278 0.098 Uiso 0.50 1 calc PR B 2 C53 C 0.9787(13) -0.9590(10) 0.9626(9) 0.082(2) Uiso 0.50 1 d PD . 2 H53A H 0.9099 -0.9306 1.0043 0.098 Uiso 0.50 1 calc PR . 2 H53B H 1.0327 -0.8998 0.9350 0.098 Uiso 0.50 1 calc PR . 2 O101 O 0.7761(4) -0.3270(4) 0.5178(3) 0.0651(12) Uani 1 1 d . . . C101 C 0.8366(4) -0.3310(4) 0.5664(4) 0.0407(12) Uani 1 1 d . . . O102 O 1.0747(4) -0.1582(4) 0.4638(3) 0.0659(12) Uani 1 1 d . . . C102 C 1.0230(4) -0.2252(5) 0.5289(4) 0.0407(12) Uani 1 1 d . . . O103 O 1.0578(5) -0.5414(4) 0.6315(4) 0.0946(18) Uani 1 1 d . . . C103 C 1.0115(5) -0.4602(5) 0.6341(4) 0.0530(15) Uani 1 1 d . . . O201 O 0.9343(4) -0.2793(4) 0.9953(3) 0.0659(12) Uani 1 1 d . . . C201 C 0.9546(4) -0.2871(4) 0.9122(4) 0.0409(12) Uani 1 1 d . . . C202 C 1.0709(4) -0.1800(5) 0.7098(4) 0.0415(12) Uani 1 1 d . . . O202 O 1.1207(4) -0.1036(4) 0.6623(3) 0.0651(12) Uani 1 1 d . . . O203 O 1.1492(3) -0.4917(4) 0.8180(3) 0.0656(13) Uani 1 1 d . . . C203 C 1.0876(4) -0.4178(5) 0.8044(4) 0.0414(12) Uani 1 1 d . . . O301 O 0.7231(3) 0.3164(3) 0.4048(3) 0.0536(11) Uani 1 1 d . . . C301 C 0.6422(4) 0.2951(4) 0.4675(3) 0.0339(11) Uani 1 1 d . . . O302 O 0.3632(3) 0.4562(3) 0.5316(3) 0.0468(9) Uani 1 1 d . . . C302 C 0.4196(4) 0.3790(4) 0.5459(3) 0.0308(10) Uani 1 1 d . . . O303 O 0.4264(3) 0.1217(3) 0.4826(3) 0.0550(10) Uani 1 1 d . . . C303 C 0.4584(4) 0.1739(4) 0.5180(4) 0.0364(11) Uani 1 1 d . . . O401 O 0.4258(3) 0.4851(3) 0.7338(3) 0.0506(10) Uani 1 1 d . . . C401 C 0.4783(4) 0.4073(4) 0.7284(4) 0.0359(11) Uani 1 1 d . . . O402 O 0.7916(3) 0.3654(3) 0.6046(3) 0.0544(10) Uani 1 1 d . . . C402 C 0.7040(5) 0.3343(4) 0.6490(4) 0.0380(12) Uani 1 1 d . . . O403 O 0.5961(5) 0.2039(4) 0.9359(3) 0.0772(15) Uani 1 1 d . . . C403 C 0.5838(5) 0.2340(4) 0.8521(4) 0.0452(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0292(3) 0.0295(4) 0.0331(3) -0.0162(3) -0.0075(3) 0.0056(3) S1 0.0412(8) 0.0544(9) 0.0645(9) -0.0336(7) 0.0106(7) -0.0199(7) O1 0.093(4) 0.080(4) 0.094(3) -0.040(3) -0.049(3) 0.047(3) C1 0.026(2) 0.025(2) 0.032(2) -0.0078(18) -0.0082(19) 0.0050(19) Co2 0.0269(3) 0.0286(3) 0.0302(3) -0.0107(3) -0.0086(3) 0.0050(3) S2 0.0477(8) 0.0315(7) 0.0642(9) -0.0175(6) -0.0128(7) -0.0047(6) C2 0.023(2) 0.027(2) 0.026(2) -0.0107(18) -0.0065(17) 0.0021(18) Co3 0.0253(3) 0.0212(3) 0.0228(3) -0.0056(2) -0.0067(2) 0.0017(2) C3 0.021(2) 0.025(2) 0.028(2) -0.0107(17) -0.0044(17) -0.0001(18) Co4 0.0307(3) 0.0220(3) 0.0275(3) -0.0090(2) -0.0101(3) 0.0026(3) C4 0.047(3) 0.035(3) 0.022(2) -0.0095(19) -0.010(2) 0.013(2) C5 0.046(3) 0.041(3) 0.019(2) -0.0139(19) -0.006(2) 0.016(2) C6 0.025(2) 0.020(2) 0.028(2) -0.0075(17) -0.0065(18) 0.0015(18) C7 0.030(2) 0.020(2) 0.024(2) -0.0036(16) -0.0058(18) 0.0001(19) C8 0.032(2) 0.027(2) 0.023(2) -0.0092(18) -0.0052(18) 0.002(2) C9 0.032(2) 0.018(2) 0.022(2) -0.0049(16) -0.0081(18) 0.0009(18) C10 0.032(2) 0.022(2) 0.024(2) -0.0079(17) -0.0058(18) 0.0001(19) C11 0.032(3) 0.026(2) 0.033(2) -0.0114(19) 0.002(2) 0.000(2) C12 0.032(3) 0.046(3) 0.079(4) -0.031(3) 0.017(3) -0.003(3) C13 0.058(4) 0.075(4) 0.031(3) -0.001(3) 0.011(3) -0.023(3) C14 0.064(5) 0.057(5) 0.179(8) -0.078(5) 0.057(5) -0.030(4) C15 0.082(5) 0.072(5) 0.067(4) -0.009(4) -0.009(4) 0.041(4) C16 0.057(4) 0.040(3) 0.063(4) -0.012(3) -0.012(3) 0.002(3) C17 0.053(3) 0.031(3) 0.054(3) -0.010(2) -0.016(3) -0.006(3) C18 0.040(3) 0.028(3) 0.044(3) -0.005(2) -0.012(2) -0.002(2) C19 0.057(4) 0.048(3) 0.041(3) -0.013(3) 0.013(3) -0.011(3) C20 0.058(4) 0.028(3) 0.073(4) 0.007(3) -0.013(3) -0.001(3) O101 0.053(3) 0.097(4) 0.068(3) -0.051(3) -0.025(2) 0.004(2) C101 0.039(3) 0.046(3) 0.042(3) -0.027(2) -0.003(2) 0.001(2) O102 0.070(3) 0.070(3) 0.048(2) -0.013(2) 0.004(2) -0.026(2) C102 0.037(3) 0.050(3) 0.037(3) -0.021(2) -0.005(2) -0.002(3) O103 0.119(4) 0.063(3) 0.099(4) -0.046(3) -0.026(3) 0.052(3) C103 0.062(4) 0.045(3) 0.057(3) -0.028(3) -0.018(3) 0.018(3) O201 0.074(3) 0.086(3) 0.045(2) -0.036(2) -0.008(2) -0.005(2) C201 0.038(3) 0.042(3) 0.043(3) -0.016(2) -0.012(2) 0.004(2) C202 0.039(3) 0.049(3) 0.040(3) -0.018(2) -0.009(2) -0.004(3) O202 0.069(3) 0.064(3) 0.061(3) -0.014(2) -0.008(2) -0.030(2) O203 0.055(3) 0.056(3) 0.070(3) -0.011(2) -0.019(2) 0.029(2) C203 0.035(3) 0.045(3) 0.040(3) -0.011(2) -0.012(2) 0.006(3) O301 0.038(2) 0.057(3) 0.044(2) -0.0070(18) 0.0083(18) 0.0019(19) C301 0.039(3) 0.032(3) 0.027(2) -0.0084(19) -0.008(2) 0.007(2) O302 0.049(2) 0.0259(19) 0.068(2) -0.0121(17) -0.0279(19) 0.0107(17) C302 0.031(3) 0.027(3) 0.035(2) -0.0082(19) -0.010(2) -0.001(2) O303 0.071(3) 0.059(3) 0.051(2) -0.031(2) -0.019(2) -0.009(2) C303 0.040(3) 0.034(3) 0.034(3) -0.010(2) -0.013(2) 0.003(2) O401 0.050(2) 0.035(2) 0.078(3) -0.0324(19) -0.023(2) 0.0121(18) C401 0.035(3) 0.032(3) 0.043(3) -0.015(2) -0.011(2) -0.001(2) O402 0.034(2) 0.063(3) 0.063(2) -0.021(2) -0.0065(19) -0.006(2) C402 0.041(3) 0.036(3) 0.042(3) -0.018(2) -0.016(2) 0.007(2) O403 0.134(4) 0.064(3) 0.046(2) -0.010(2) -0.052(3) -0.006(3) C403 0.064(4) 0.036(3) 0.043(3) -0.015(2) -0.024(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C0 Cl1 1.648(15) . ? C0 Cl2 1.707(15) . ? C0 Cl3 1.771(15) . ? Co1 C101 1.797(6) . ? Co1 C103 1.818(5) . ? Co1 C102 1.822(6) . ? Co1 C2 1.956(4) . ? Co1 C1 1.972(4) . ? Co1 Co2 2.4561(9) . ? S1 C14 1.785(6) . ? S1 C11 1.838(5) . ? O1 C16 1.385(7) . ? O1 C15 1.430(7) . ? C1 C2 1.347(6) . ? C1 C18 1.507(7) . ? C1 Co2 1.984(5) . ? Co2 C201 1.776(5) . ? Co2 C203 1.817(5) . ? Co2 C202 1.821(6) . ? Co2 C2 1.977(4) . ? S2 C17 1.805(5) . ? S2 C18 1.841(5) . ? C2 C3 1.462(6) . ? Co3 C303 1.805(6) . ? Co3 C302 1.815(5) . ? Co3 C301 1.830(5) . ? Co3 C9 1.959(4) . ? Co3 C10 1.968(4) . ? Co3 Co4 2.4638(8) . ? C3 C8 1.393(6) . ? C3 C4 1.398(6) . ? Co4 C403 1.787(5) . ? Co4 C401 1.819(5) . ? Co4 C402 1.821(6) . ? Co4 C10 1.987(5) . ? Co4 C9 1.994(4) . ? C4 C5 1.374(6) . ? C5 C6 1.396(6) . ? C6 C7 1.383(6) . ? C6 C9 1.459(6) . ? C7 C8 1.379(6) . ? C9 C10 1.347(6) . ? C10 C11 1.497(6) . ? C11 C13 1.525(7) . ? C11 C12 1.533(7) . ? C14 C15 1.407(10) . ? C16 C17 1.494(7) . ? C18 C20 1.525(7) . ? C18 C19 1.535(7) . ? C51 C52 1.543(14) . ? C52 C53 1.350(14) . ? C53 C53 1.368(15) 2_737 ? O101 C101 1.132(6) . ? O102 C102 1.123(6) . ? O103 C103 1.133(6) . ? O201 C201 1.145(6) . ? C202 O202 1.132(6) . ? O203 C203 1.136(6) . ? O301 C301 1.121(5) . ? O302 C302 1.130(5) . ? O303 C303 1.131(6) . ? O401 C401 1.135(5) . ? O402 C402 1.139(6) . ? O403 C403 1.138(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 C0 Cl2 114.8(11) . . ? Cl1 C0 Cl3 110.9(10) . . ? Cl2 C0 Cl3 108.8(9) . . ? C101 Co1 C103 98.3(3) . . ? C101 Co1 C102 96.2(2) . . ? C103 Co1 C102 104.7(3) . . ? C101 Co1 C2 101.50(19) . . ? C103 Co1 C2 143.5(2) . . ? C102 Co1 C2 103.3(2) . . ? C101 Co1 C1 104.3(2) . . ? C103 Co1 C1 105.1(2) . . ? C102 Co1 C1 140.5(2) . . ? C2 Co1 C1 40.11(17) . . ? C101 Co1 Co2 152.33(15) . . ? C103 Co1 Co2 101.60(18) . . ? C102 Co1 Co2 97.11(17) . . ? C2 Co1 Co2 51.75(12) . . ? C1 Co1 Co2 51.83(14) . . ? C14 S1 C11 107.4(3) . . ? C16 O1 C15 117.5(5) . . ? C2 C1 C18 141.3(4) . . ? C2 C1 Co1 69.3(2) . . ? C18 C1 Co1 137.4(4) . . ? C2 C1 Co2 69.9(3) . . ? C18 C1 Co2 133.2(3) . . ? Co1 C1 Co2 76.76(16) . . ? C201 Co2 C203 98.5(2) . . ? C201 Co2 C202 98.4(2) . . ? C203 Co2 C202 105.7(2) . . ? C201 Co2 C2 105.7(2) . . ? C203 Co2 C2 141.6(2) . . ? C202 Co2 C2 99.9(2) . . ? C201 Co2 C1 102.0(2) . . ? C203 Co2 C1 106.6(2) . . ? C202 Co2 C1 138.5(2) . . ? C2 Co2 C1 39.77(17) . . ? C201 Co2 Co1 152.62(18) . . ? C203 Co2 Co1 96.13(17) . . ? C202 Co2 Co1 99.79(16) . . ? C2 Co2 Co1 50.96(12) . . ? C1 Co2 Co1 51.41(12) . . ? C17 S2 C18 106.8(2) . . ? C1 C2 C3 143.0(4) . . ? C1 C2 Co1 70.6(2) . . ? C3 C2 Co1 135.1(3) . . ? C1 C2 Co2 70.4(3) . . ? C3 C2 Co2 132.3(3) . . ? Co1 C2 Co2 77.29(15) . . ? C303 Co3 C302 100.0(2) . . ? C303 Co3 C301 98.1(2) . . ? C302 Co3 C301 104.4(2) . . ? C303 Co3 C9 102.00(19) . . ? C302 Co3 C9 141.69(18) . . ? C301 Co3 C9 103.12(19) . . ? C303 Co3 C10 101.0(2) . . ? C302 Co3 C10 104.89(18) . . ? C301 Co3 C10 141.40(19) . . ? C9 Co3 C10 40.11(17) . . ? C303 Co3 Co4 151.22(15) . . ? C302 Co3 Co4 96.92(15) . . ? C301 Co3 Co4 100.05(15) . . ? C9 Co3 Co4 52.07(12) . . ? C10 Co3 Co4 51.83(13) . . ? C8 C3 C4 116.8(4) . . ? C8 C3 C2 122.3(4) . . ? C4 C3 C2 120.9(4) . . ? C403 Co4 C401 98.6(2) . . ? C403 Co4 C402 98.2(2) . . ? C401 Co4 C402 103.9(2) . . ? C403 Co4 C10 103.1(2) . . ? C401 Co4 C10 104.6(2) . . ? C402 Co4 C10 141.16(19) . . ? C403 Co4 C9 102.8(2) . . ? C401 Co4 C9 141.6(2) . . ? C402 Co4 C9 104.2(2) . . ? C10 Co4 C9 39.54(17) . . ? C403 Co4 Co3 151.74(18) . . ? C401 Co4 Co3 99.34(16) . . ? C402 Co4 Co3 98.46(15) . . ? C10 Co4 Co3 51.11(11) . . ? C9 Co4 Co3 50.83(11) . . ? C5 C4 C3 121.6(4) . . ? C4 C5 C6 121.0(4) . . ? C7 C6 C5 117.6(4) . . ? C7 C6 C9 121.9(4) . . ? C5 C6 C9 120.5(4) . . ? C8 C7 C6 121.4(4) . . ? C7 C8 C3 121.4(4) . . ? C10 C9 C6 143.9(4) . . ? C10 C9 Co3 70.3(2) . . ? C6 C9 Co3 135.4(3) . . ? C10 C9 Co4 70.0(3) . . ? C6 C9 Co4 131.7(3) . . ? Co3 C9 Co4 77.10(14) . . ? C9 C10 C11 143.5(4) . . ? C9 C10 Co3 69.6(2) . . ? C11 C10 Co3 135.1(3) . . ? C9 C10 Co4 70.5(3) . . ? C11 C10 Co4 132.6(3) . . ? Co3 C10 Co4 77.06(16) . . ? C10 C11 C13 110.5(4) . . ? C10 C11 C12 111.2(4) . . ? C13 C11 C12 110.6(4) . . ? C10 C11 S1 111.4(3) . . ? C13 C11 S1 110.9(4) . . ? C12 C11 S1 101.9(4) . . ? C15 C14 S1 118.7(5) . . ? C14 C15 O1 109.3(6) . . ? O1 C16 C17 107.1(5) . . ? C16 C17 S2 117.4(4) . . ? C1 C18 C20 111.4(4) . . ? C1 C18 C19 111.3(4) . . ? C20 C18 C19 110.3(5) . . ? C1 C18 S2 111.1(3) . . ? C20 C18 S2 104.6(4) . . ? C19 C18 S2 107.9(4) . . ? C53 C52 C51 120.3(12) . . ? C52 C53 C53 131.5(17) . 2_737 ? O101 C101 Co1 176.5(5) . . ? O102 C102 Co1 177.7(5) . . ? O103 C103 Co1 179.3(6) . . ? O201 C201 Co2 179.2(5) . . ? O202 C202 Co2 178.1(5) . . ? O203 C203 Co2 179.1(5) . . ? O301 C301 Co3 178.2(4) . . ? O302 C302 Co3 177.5(4) . . ? O303 C303 Co3 178.7(5) . . ? O401 C401 Co4 178.9(5) . . ? O402 C402 Co4 179.5(5) . . ? O403 C403 Co4 179.1(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.950 _refine_diff_density_min -1.253 _refine_diff_density_rms 0.104 #===END data_mm0213_COMPOUND_6 _database_code_depnum_ccdc_archive 'CCDC 228900' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H70 Cl2 Co4 O8 P4' _chemical_formula_weight 1529.81 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' Co Co 0.3494 0.9721 '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 TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.35510(10) _cell_length_b 13.8087(2) _cell_length_c 23.8944(3) _cell_angle_alpha 73.855(2) _cell_angle_beta 80.770(2) _cell_angle_gamma 82.120(2) _cell_volume 3535.32(7) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 36278 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1572 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.917 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43652 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.45 _reflns_number_total 16067 _reflns_number_gt 12229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+9.3725P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16067 _refine_ls_number_parameters 804 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 5.301 _refine_ls_shift/su_mean 0.014 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.93139(4) -0.11000(4) 0.22407(2) 0.02214(12) Uani 1 1 d . . . P1 P 1.09928(9) -0.21368(7) 0.22438(4) 0.02334(19) Uani 1 1 d . . . C1 C 0.9880(3) -0.0099(3) 0.25573(14) 0.0223(7) Uani 1 1 d . . . C70 C 1.1647(6) 0.0845(5) -0.0002(3) 0.0661(15) Uiso 1 1 d . . . H70A H 1.1147 0.0340 -0.0041 0.079 Uiso 1 1 calc R . . H70B H 1.1932 0.0600 0.0388 0.079 Uiso 1 1 calc R . . Cl1 Cl 1.0786(2) 0.1986(2) -0.00445(12) 0.1196(8) Uiso 1 1 d . . . Co2 Co 0.91579(4) -0.10116(4) 0.32707(2) 0.02309(12) Uani 1 1 d . . . P2 P 1.06913(9) -0.21627(7) 0.35127(4) 0.0236(2) Uani 1 1 d . . . C2 C 0.8663(3) 0.0038(3) 0.25803(14) 0.0210(7) Uani 1 1 d . . . Cl2 Cl 1.28758(17) 0.09497(15) -0.05471(8) 0.0841(5) Uiso 1 1 d . . . C67 C 0.7958(9) 0.4803(8) -0.0757(5) 0.131(3) Uiso 1 1 d D . . H67B H 0.8045 0.4466 -0.1074 0.196 Uiso 1 1 calc R . . H67A H 0.7688 0.5521 -0.0906 0.196 Uiso 1 1 calc R . . H67C H 0.7366 0.4485 -0.0436 0.196 Uiso 1 1 calc R . . Co3 Co 0.68344(4) 0.16417(4) 0.302869(19) 0.02176(12) Uani 1 1 d . A . P3 P 0.52076(8) 0.27285(7) 0.30639(4) 0.02206(19) Uani 1 1 d . . . C3 C 0.7688(3) 0.0812(3) 0.25092(14) 0.0211(7) Uani 1 1 d . A . C68 C 0.9107(15) 0.4708(15) -0.0541(8) 0.259(9) Uiso 1 1 d D . . H68A H 0.9349 0.3970 -0.0436 0.311 Uiso 1 1 calc R . . H68B H 0.9660 0.4997 -0.0895 0.311 Uiso 1 1 calc R . . Co4 Co 0.73150(4) 0.21166(4) 0.194375(19) 0.02081(11) Uani 1 1 d . A . P4 P 0.56992(8) 0.32051(7) 0.17530(4) 0.02235(19) Uani 1 1 d . . . C4 C 0.6501(3) 0.0961(3) 0.24657(15) 0.0234(7) Uani 1 1 d . . . C69 C 0.9445(9) 0.5029(11) -0.0114(6) 0.171(5) Uiso 1 1 d D . . H69A H 0.8891 0.4732 0.0238 0.205 Uiso 1 1 calc R . . H69B H 0.9183 0.5764 -0.0218 0.205 Uiso 1 1 calc R . . C5 C 0.5595(4) 0.0356(3) 0.23923(18) 0.0310(8) Uani 1 1 d . A . C6 C 0.5831(5) 0.0005(4) 0.1838(2) 0.0481(12) Uani 1 1 d . . . H6A H 0.5185 -0.0390 0.1827 0.072 Uiso 1 1 calc R A . H6B H 0.6598 -0.0419 0.1831 0.072 Uiso 1 1 calc R . . H6C H 0.5865 0.0594 0.1496 0.072 Uiso 1 1 calc R . . C7 C 0.4669(4) 0.0100(4) 0.2790(2) 0.0482(12) Uani 1 1 d . . . H7A H 0.4563 0.0306 0.3144 0.058 Uiso 1 1 calc R A . H7B H 0.4106 -0.0293 0.2723 0.058 Uiso 1 1 calc R . . C8 C 1.1583(4) 0.0661(4) 0.2724(2) 0.0457(11) Uani 1 1 d . . . H8A H 1.1465 0.0316 0.3130 0.055 Uiso 1 1 calc R . . H8B H 1.2212 0.1089 0.2577 0.055 Uiso 1 1 calc R . . C9 C 1.1024(4) 0.1089(3) 0.17203(19) 0.0411(10) Uani 1 1 d . . . H9A H 1.1703 0.1499 0.1634 0.062 Uiso 1 1 calc R . . H9B H 1.0293 0.1531 0.1621 0.062 Uiso 1 1 calc R . . H9C H 1.1178 0.0592 0.1487 0.062 Uiso 1 1 calc R . . C10 C 1.0868(3) 0.0547(3) 0.23631(17) 0.0295(8) Uani 1 1 d . . . C11 C 1.2121(3) -0.1816(3) 0.15943(15) 0.0268(8) Uani 1 1 d . . . C12 C 1.3010(4) -0.1195(3) 0.15513(18) 0.0381(10) Uani 1 1 d . . . H12A H 1.3085 -0.0952 0.1878 0.046 Uiso 1 1 calc R . . C13 C 1.3792(4) -0.0925(4) 0.1036(2) 0.0461(11) Uani 1 1 d . . . H13A H 1.4391 -0.0492 0.1012 0.055 Uiso 1 1 calc R . . C14 C 1.3707(5) -0.1281(4) 0.0560(2) 0.0482(12) Uani 1 1 d . . . H14A H 1.4257 -0.1110 0.0212 0.058 Uiso 1 1 calc R . . C15 C 1.2822(5) -0.1882(4) 0.05940(19) 0.0524(13) Uani 1 1 d . . . H15A H 1.2751 -0.2120 0.0265 0.063 Uiso 1 1 calc R . . C16 C 1.2024(4) -0.2149(4) 0.11056(18) 0.0429(11) Uani 1 1 d . . . H16A H 1.1407 -0.2560 0.1122 0.052 Uiso 1 1 calc R . . C17 C 1.0907(4) -0.3484(3) 0.23200(17) 0.0283(8) Uani 1 1 d . . . C18 C 0.9952(4) -0.3766(3) 0.2114(2) 0.0376(10) Uani 1 1 d . . . H18A H 0.9380 -0.3262 0.1927 0.045 Uiso 1 1 calc R . . C19 C 0.9842(4) -0.4785(4) 0.2185(2) 0.0460(11) Uani 1 1 d . . . H19A H 0.9202 -0.4974 0.2038 0.055 Uiso 1 1 calc R . . C20 C 1.0649(4) -0.5521(3) 0.2464(2) 0.0426(11) Uani 1 1 d . . . H20A H 1.0556 -0.6217 0.2521 0.051 Uiso 1 1 calc R . . C21 C 1.1602(4) -0.5245(3) 0.2663(2) 0.0364(9) Uani 1 1 d . . . H21A H 1.2163 -0.5752 0.2856 0.044 Uiso 1 1 calc R . . C22 C 1.1737(4) -0.4232(3) 0.25814(17) 0.0312(8) Uani 1 1 d . . . H22A H 1.2408 -0.4049 0.2707 0.037 Uiso 1 1 calc R . . C23 C 1.1791(3) -0.2122(3) 0.28524(15) 0.0251(7) Uani 1 1 d . . . H23A H 1.2208 -0.1499 0.2751 0.030 Uiso 1 1 calc R . . H23B H 1.2398 -0.2715 0.2927 0.030 Uiso 1 1 calc R . . C24 C 1.0458(4) -0.3508(3) 0.38056(16) 0.0288(8) Uani 1 1 d . . . C25 C 0.9485(4) -0.3868(3) 0.36662(19) 0.0383(10) Uani 1 1 d . . . H25A H 0.8921 -0.3407 0.3446 0.046 Uiso 1 1 calc R . . C26 C 0.9332(5) -0.4898(4) 0.3848(2) 0.0484(12) Uani 1 1 d . . . H26A H 0.8675 -0.5141 0.3745 0.058 Uiso 1 1 calc R . . C27 C 1.0136(5) -0.5560(4) 0.4175(2) 0.0554(14) Uani 1 1 d . . . H27A H 1.0031 -0.6263 0.4300 0.066 Uiso 1 1 calc R . . C28 C 1.1095(5) -0.5214(4) 0.4326(2) 0.0505(12) Uani 1 1 d . . . H28A H 1.1646 -0.5676 0.4554 0.061 Uiso 1 1 calc R . . C29 C 1.1250(4) -0.4191(3) 0.41427(18) 0.0368(9) Uani 1 1 d . . . H29A H 1.1906 -0.3953 0.4250 0.044 Uiso 1 1 calc R . . C30 C 1.1566(4) -0.1948(3) 0.40389(17) 0.0309(8) Uani 1 1 d . . . C31 C 1.0979(5) -0.2002(4) 0.46059(19) 0.0435(11) Uani 1 1 d . . . H31A H 1.0190 -0.2205 0.4708 0.052 Uiso 1 1 calc R . . C32 C 1.1527(6) -0.1764(4) 0.5020(2) 0.0597(15) Uani 1 1 d . . . H32A H 1.1122 -0.1811 0.5405 0.072 Uiso 1 1 calc R . . C33 C 1.2659(7) -0.1459(5) 0.4870(3) 0.0688(18) Uani 1 1 d . . . H33A H 1.3029 -0.1274 0.5149 0.083 Uiso 1 1 calc R . . C34 C 1.3272(6) -0.1418(5) 0.4314(3) 0.0676(17) Uani 1 1 d . . . H34A H 1.4061 -0.1215 0.4215 0.081 Uiso 1 1 calc R . . C35 C 1.2720(5) -0.1676(4) 0.3901(2) 0.0477(12) Uani 1 1 d . . . H35A H 1.3144 -0.1664 0.3523 0.057 Uiso 1 1 calc R . . C36 C 0.3984(4) 0.2310(3) 0.36446(16) 0.0299(8) Uani 1 1 d . . . C37 C 0.2905(4) 0.2073(3) 0.3548(2) 0.0416(10) Uani 1 1 d . . . H37A H 0.2742 0.2173 0.3157 0.050 Uiso 1 1 calc R . . C38 C 0.2052(5) 0.1689(4) 0.4016(3) 0.0624(16) Uani 1 1 d . . . H38A H 0.1311 0.1528 0.3946 0.075 Uiso 1 1 calc R . . C39 C 0.2293(6) 0.1543(4) 0.4585(3) 0.071(2) Uani 1 1 d . . . H39A H 0.1724 0.1262 0.4907 0.085 Uiso 1 1 calc R . . C40 C 0.3342(6) 0.1798(5) 0.4688(2) 0.0671(18) Uani 1 1 d . . . H40A H 0.3484 0.1720 0.5080 0.080 Uiso 1 1 calc R . . C41 C 0.4203(5) 0.2174(4) 0.42214(18) 0.0472(12) Uani 1 1 d . . . H41A H 0.4939 0.2337 0.4295 0.057 Uiso 1 1 calc R . . C42 C 0.5328(3) 0.4007(3) 0.31255(15) 0.0250(7) Uani 1 1 d . . . C43 C 0.4365(4) 0.4570(3) 0.33579(17) 0.0298(8) Uani 1 1 d . . . H43A H 0.3628 0.4282 0.3508 0.036 Uiso 1 1 calc R . . C44 C 0.4471(4) 0.5555(3) 0.33723(18) 0.0374(10) Uani 1 1 d . . . H44A H 0.3802 0.5941 0.3526 0.045 Uiso 1 1 calc R . . C45 C 0.5549(4) 0.5976(3) 0.3164(2) 0.0409(10) Uani 1 1 d . . . H45A H 0.5623 0.6645 0.3177 0.049 Uiso 1 1 calc R . . C46 C 0.6509(4) 0.5418(3) 0.29370(19) 0.0383(10) Uani 1 1 d . . . H46A H 0.7246 0.5706 0.2791 0.046 Uiso 1 1 calc R . . C47 C 0.6410(4) 0.4437(3) 0.29202(17) 0.0313(8) Uani 1 1 d . . . H47A H 0.7083 0.4055 0.2768 0.038 Uiso 1 1 calc R . . C48 C 0.4527(3) 0.2943(3) 0.23873(14) 0.0236(7) Uani 1 1 d . A . H48A H 0.3902 0.3523 0.2356 0.028 Uiso 1 1 calc R . . H48B H 0.4145 0.2335 0.2395 0.028 Uiso 1 1 calc R . . C49 C 0.5795(3) 0.4568(3) 0.15951(15) 0.0259(8) Uani 1 1 d . A . C50 C 0.4790(4) 0.5233(3) 0.16836(18) 0.0350(9) Uani 1 1 d . . . H50A H 0.4025 0.4985 0.1804 0.042 Uiso 1 1 calc R A . C51 C 0.4892(4) 0.6256(3) 0.15984(19) 0.0411(10) Uani 1 1 d . A . H51A H 0.4201 0.6701 0.1666 0.049 Uiso 1 1 calc R . . C52 C 0.6006(5) 0.6629(3) 0.14137(19) 0.0427(11) Uani 1 1 d . . . H52A H 0.6082 0.7325 0.1365 0.051 Uiso 1 1 calc R A . C53 C 0.6995(4) 0.5986(3) 0.1301(2) 0.0413(10) Uani 1 1 d . A . H53A H 0.7751 0.6245 0.1159 0.050 Uiso 1 1 calc R . . C54 C 0.6897(4) 0.4959(3) 0.13948(17) 0.0333(9) Uani 1 1 d . . . H54A H 0.7590 0.4520 0.1321 0.040 Uiso 1 1 calc R A . C55 C 0.4882(12) 0.3072(10) 0.1149(6) 0.024(4) Uiso 0.50 1 d P A 1 C55' C 0.5021(12) 0.3182(11) 0.1138(6) 0.025(4) Uiso 0.50 1 d P A 2 C56 C 0.4211(8) 0.2334(7) 0.1211(4) 0.0247(18) Uiso 0.50 1 d P A 1 H56A H 0.4033 0.1886 0.1588 0.030 Uiso 0.50 1 calc PR A 1 C56' C 0.3955(12) 0.2641(10) 0.1222(5) 0.052(3) Uiso 0.50 1 d P A 2 H56B H 0.3579 0.2354 0.1606 0.062 Uiso 0.50 1 calc PR A 2 C57 C 0.3760(9) 0.2200(8) 0.0736(4) 0.0307(19) Uiso 0.50 1 d P A 1 H57A H 0.3227 0.1697 0.0795 0.037 Uiso 0.50 1 calc PR A 1 C57' C 0.3494(12) 0.2549(11) 0.0731(6) 0.059(3) Uiso 0.50 1 d P A 2 H57B H 0.2864 0.2133 0.0785 0.071 Uiso 0.50 1 calc PR A 2 C58 C 0.4078(10) 0.2788(9) 0.0183(5) 0.032(3) Uiso 0.50 1 d P A 1 H58A H 0.3813 0.2662 -0.0146 0.038 Uiso 0.50 1 calc PR A 1 C58' C 0.3946(13) 0.3058(11) 0.0171(6) 0.049(4) Uiso 0.50 1 d P A 2 H58B H 0.3559 0.3073 -0.0156 0.059 Uiso 0.50 1 calc PR A 2 C59 C 0.4729(12) 0.3507(10) 0.0109(6) 0.040(4) Uiso 0.50 1 d P A 1 H59A H 0.4892 0.3931 -0.0277 0.048 Uiso 0.50 1 calc PR A 1 C59' C 0.5020(11) 0.3570(8) 0.0088(5) 0.030(3) Uiso 0.50 1 d P A 2 H59B H 0.5388 0.3886 -0.0293 0.036 Uiso 0.50 1 calc PR A 2 C60 C 0.5244(12) 0.3719(10) 0.0584(5) 0.033(3) Uiso 0.50 1 d P A 1 H60A H 0.5764 0.4233 0.0522 0.040 Uiso 0.50 1 calc PR A 1 C60' C 0.5466(12) 0.3576(9) 0.0571(5) 0.031(3) Uiso 0.50 1 d P A 2 H60B H 0.6182 0.3896 0.0510 0.037 Uiso 0.50 1 calc PR A 2 C66 C 0.276(10) 0.705(12) 0.564(12) 2.0(5) Uiso 0.50 1 d PD B -1 H66C H 0.1965 0.7304 0.5797 3.000 Uiso 0.50 1 calc PR B -1 H66B H 0.3084 0.7570 0.5300 3.000 Uiso 0.50 1 calc PR B -1 H66A H 0.3296 0.6883 0.5943 3.000 Uiso 0.50 1 calc PR B -1 C65 C 0.266(4) 0.611(4) 0.545(5) 0.95(13) Uiso 0.50 1 d PD B -1 H65B H 0.2289 0.5606 0.5789 1.145 Uiso 0.50 1 calc PR B -1 H65A H 0.2120 0.6289 0.5142 1.145 Uiso 0.50 1 calc PR B -1 C64 C 0.3813(10) 0.5625(7) 0.5216(5) 0.054(3) Uiso 0.50 1 d PD B -1 H64A H 0.4411 0.5624 0.5476 0.065 Uiso 0.50 1 calc PR B -1 H64B H 0.4076 0.6072 0.4826 0.065 Uiso 0.50 1 calc PR B -1 C63 C 0.3888(11) 0.4575(8) 0.5146(6) 0.068(3) Uiso 0.50 1 d PD B -1 H63A H 0.3316 0.4199 0.5462 0.082 Uiso 0.50 1 calc PR B -1 H63B H 0.3592 0.4628 0.4769 0.082 Uiso 0.50 1 calc PR B -1 C62 C 0.5017(10) 0.3956(9) 0.5151(6) 0.068(3) Uiso 0.50 1 d PD B -1 H62A H 0.5286 0.3851 0.5539 0.082 Uiso 0.50 1 calc PR B -1 H62C H 0.5610 0.4345 0.4853 0.082 Uiso 0.50 1 calc PR B -1 C61 C 0.506(11) 0.293(14) 0.50(2) 2.0(5) Uiso 0.50 1 d PD B -1 H61C H 0.5876 0.2600 0.5044 3.000 Uiso 0.50 1 calc PR B -1 H62B H 0.4810 0.3018 0.4649 3.000 Uiso 0.50 1 calc PR B -1 H61A H 0.4512 0.2518 0.5339 3.000 Uiso 0.50 1 calc PR B -1 O101 O 0.7252(3) -0.2261(3) 0.24201(17) 0.0564(9) Uani 1 1 d . . . C101 C 0.8076(4) -0.1827(3) 0.23481(19) 0.0349(9) Uani 1 1 d . . . O102 O 0.9600(3) -0.0230(3) 0.09723(12) 0.0488(8) Uani 1 1 d . . . C102 C 0.9463(4) -0.0556(3) 0.14708(17) 0.0300(8) Uani 1 1 d . . . O201 O 0.9289(3) 0.0160(3) 0.40991(14) 0.0490(8) Uani 1 1 d . . . C201 C 0.9225(4) -0.0303(3) 0.37805(16) 0.0325(9) Uani 1 1 d . . . O202 O 0.6944(3) -0.1979(3) 0.37739(16) 0.0586(10) Uani 1 1 d . . . C202 C 0.7820(4) -0.1631(3) 0.35852(18) 0.0359(9) Uani 1 1 d . . . O301 O 0.6139(3) 0.0140(2) 0.41200(13) 0.0519(9) Uani 1 1 d . A . C301 C 0.6411(4) 0.0726(3) 0.36957(17) 0.0328(9) Uani 1 1 d . . . O302 O 0.8767(3) 0.2474(3) 0.33776(16) 0.0545(9) Uani 1 1 d . A . C302 C 0.8010(4) 0.2166(3) 0.32434(17) 0.0319(9) Uani 1 1 d . . . O401 O 0.9391(3) 0.3188(3) 0.18873(17) 0.0537(9) Uani 1 1 d . A . C401 C 0.8561(4) 0.2799(3) 0.19050(17) 0.0309(8) Uani 1 1 d . . . O402 O 0.7815(3) 0.1690(3) 0.07948(13) 0.0556(9) Uani 1 1 d . A . C402 C 0.7622(4) 0.1840(3) 0.12467(17) 0.0306(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0234(3) 0.0213(2) 0.0225(2) -0.00755(18) -0.00271(18) -0.00138(19) P1 0.0243(5) 0.0246(5) 0.0227(4) -0.0101(4) -0.0037(3) 0.0012(4) C1 0.0234(18) 0.0253(18) 0.0191(16) -0.0067(13) -0.0036(13) -0.0027(14) Co2 0.0257(3) 0.0223(2) 0.0193(2) -0.00480(18) -0.00098(18) 0.0005(2) P2 0.0269(5) 0.0230(5) 0.0201(4) -0.0054(3) -0.0038(3) 0.0006(4) C2 0.0289(19) 0.0182(16) 0.0160(15) -0.0051(12) -0.0014(13) -0.0029(14) Co3 0.0253(3) 0.0218(2) 0.0174(2) -0.00503(18) -0.00355(18) 0.00125(19) P3 0.0240(5) 0.0228(4) 0.0175(4) -0.0042(3) -0.0015(3) 0.0002(4) C3 0.0253(18) 0.0198(17) 0.0179(15) -0.0049(13) -0.0006(13) -0.0036(14) Co4 0.0231(3) 0.0206(2) 0.0178(2) -0.00408(17) -0.00163(18) -0.00185(19) P4 0.0241(5) 0.0234(5) 0.0173(4) -0.0027(3) -0.0025(3) -0.0003(4) C4 0.0263(19) 0.0239(18) 0.0199(16) -0.0061(13) -0.0010(13) -0.0034(15) C5 0.031(2) 0.0256(19) 0.037(2) -0.0076(16) -0.0065(16) -0.0042(16) C6 0.053(3) 0.049(3) 0.052(3) -0.022(2) -0.012(2) -0.016(2) C7 0.036(3) 0.054(3) 0.058(3) -0.017(2) 0.004(2) -0.022(2) C8 0.043(3) 0.050(3) 0.051(3) -0.014(2) -0.012(2) -0.019(2) C9 0.042(3) 0.038(2) 0.041(2) -0.0078(19) 0.0079(19) -0.017(2) C10 0.026(2) 0.028(2) 0.035(2) -0.0104(16) -0.0008(16) -0.0022(16) C11 0.0257(19) 0.032(2) 0.0219(17) -0.0094(15) -0.0033(14) 0.0045(16) C12 0.039(2) 0.043(2) 0.031(2) -0.0115(18) 0.0014(17) -0.006(2) C13 0.040(3) 0.057(3) 0.038(2) -0.011(2) 0.0061(19) -0.010(2) C14 0.045(3) 0.060(3) 0.031(2) -0.009(2) 0.0065(19) 0.003(2) C15 0.063(3) 0.071(3) 0.026(2) -0.023(2) -0.003(2) 0.003(3) C16 0.048(3) 0.055(3) 0.030(2) -0.018(2) -0.0032(19) -0.008(2) C17 0.032(2) 0.0244(19) 0.0308(19) -0.0122(15) -0.0026(15) -0.0005(16) C18 0.037(2) 0.032(2) 0.052(3) -0.0208(19) -0.015(2) 0.0032(18) C19 0.042(3) 0.040(3) 0.068(3) -0.029(2) -0.018(2) -0.002(2) C20 0.046(3) 0.028(2) 0.060(3) -0.019(2) -0.011(2) -0.0033(19) C21 0.036(2) 0.026(2) 0.048(2) -0.0135(18) -0.0115(19) 0.0058(17) C22 0.027(2) 0.033(2) 0.037(2) -0.0157(17) -0.0056(16) 0.0016(16) C23 0.0259(19) 0.0258(18) 0.0251(17) -0.0098(14) -0.0041(14) 0.0000(15) C24 0.034(2) 0.0238(19) 0.0257(18) -0.0047(14) -0.0004(15) -0.0007(16) C25 0.036(2) 0.032(2) 0.043(2) -0.0071(18) -0.0040(19) -0.0015(19) C26 0.054(3) 0.035(2) 0.056(3) -0.010(2) -0.003(2) -0.012(2) C27 0.072(4) 0.027(2) 0.061(3) -0.001(2) -0.002(3) -0.010(2) C28 0.060(3) 0.032(2) 0.048(3) 0.004(2) -0.009(2) 0.006(2) C29 0.040(2) 0.031(2) 0.035(2) -0.0026(17) -0.0061(18) 0.0001(18) C30 0.040(2) 0.027(2) 0.0273(19) -0.0085(15) -0.0116(16) 0.0041(17) C31 0.047(3) 0.052(3) 0.033(2) -0.017(2) -0.0101(19) 0.010(2) C32 0.081(4) 0.068(4) 0.037(3) -0.024(2) -0.026(3) 0.012(3) C33 0.103(5) 0.068(4) 0.052(3) -0.026(3) -0.044(3) -0.003(4) C34 0.076(4) 0.075(4) 0.062(4) -0.009(3) -0.033(3) -0.032(3) C35 0.055(3) 0.058(3) 0.033(2) -0.006(2) -0.015(2) -0.020(2) C36 0.032(2) 0.0263(19) 0.0250(18) -0.0028(14) 0.0055(15) 0.0021(16) C37 0.042(3) 0.040(2) 0.041(2) -0.0147(19) 0.0122(19) -0.010(2) C38 0.052(3) 0.055(3) 0.073(4) -0.017(3) 0.030(3) -0.023(3) C39 0.075(4) 0.053(3) 0.053(3) 0.010(3) 0.039(3) -0.002(3) C40 0.078(4) 0.070(4) 0.027(2) 0.007(2) 0.017(2) 0.016(3) C41 0.047(3) 0.057(3) 0.025(2) -0.0026(19) -0.0004(18) 0.014(2) C42 0.030(2) 0.0233(18) 0.0219(17) -0.0075(14) -0.0049(14) 0.0015(15) C43 0.028(2) 0.030(2) 0.032(2) -0.0094(16) -0.0037(15) 0.0000(16) C44 0.039(2) 0.033(2) 0.037(2) -0.0139(18) -0.0019(18) 0.0089(19) C45 0.051(3) 0.027(2) 0.045(2) -0.0135(18) -0.005(2) -0.001(2) C46 0.040(2) 0.032(2) 0.043(2) -0.0102(18) -0.0026(19) -0.0076(19) C47 0.030(2) 0.029(2) 0.033(2) -0.0086(16) -0.0016(16) 0.0025(16) C48 0.0234(18) 0.0252(18) 0.0193(16) -0.0028(13) -0.0007(13) -0.0018(15) C49 0.029(2) 0.0252(18) 0.0186(16) -0.0001(13) -0.0026(14) 0.0006(15) C50 0.032(2) 0.031(2) 0.034(2) -0.0007(16) -0.0007(17) 0.0031(17) C51 0.050(3) 0.026(2) 0.039(2) -0.0029(17) -0.002(2) 0.0083(19) C52 0.063(3) 0.024(2) 0.037(2) 0.0003(17) -0.009(2) -0.004(2) C53 0.044(3) 0.032(2) 0.042(2) 0.0016(18) -0.006(2) -0.009(2) C54 0.031(2) 0.027(2) 0.034(2) 0.0017(16) 0.0006(16) 0.0004(17) O101 0.046(2) 0.046(2) 0.083(3) -0.0208(18) -0.0033(18) -0.0235(17) C101 0.039(2) 0.028(2) 0.040(2) -0.0124(17) -0.0031(18) -0.0055(18) O102 0.060(2) 0.060(2) 0.0230(15) -0.0060(14) -0.0059(14) -0.0039(17) C102 0.029(2) 0.033(2) 0.029(2) -0.0116(16) -0.0051(15) 0.0007(17) O201 0.068(2) 0.0481(19) 0.0366(17) -0.0245(15) -0.0130(15) 0.0088(17) C201 0.038(2) 0.031(2) 0.0247(18) -0.0064(16) -0.0056(16) 0.0078(17) O202 0.046(2) 0.064(2) 0.061(2) -0.0157(18) 0.0195(17) -0.0226(18) C202 0.038(2) 0.033(2) 0.033(2) -0.0064(17) 0.0021(18) -0.0029(19) O301 0.067(2) 0.0436(19) 0.0276(16) 0.0087(14) 0.0052(15) 0.0037(17) C301 0.036(2) 0.031(2) 0.030(2) -0.0113(17) -0.0038(16) 0.0094(17) O302 0.060(2) 0.057(2) 0.057(2) -0.0139(17) -0.0294(18) -0.0168(18) C302 0.040(2) 0.028(2) 0.0291(19) -0.0077(16) -0.0115(17) 0.0001(18) O401 0.045(2) 0.045(2) 0.076(2) -0.0165(17) -0.0104(17) -0.0180(16) C401 0.032(2) 0.0249(19) 0.034(2) -0.0054(16) -0.0042(16) -0.0036(17) O402 0.070(2) 0.069(2) 0.0271(16) -0.0220(16) -0.0041(15) 0.0121(19) C402 0.032(2) 0.029(2) 0.0265(19) -0.0033(15) -0.0011(15) 0.0010(16) _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 Co1 C102 1.773(4) . ? Co1 C101 1.783(4) . ? Co1 C2 1.968(3) . ? Co1 C1 1.969(4) . ? Co1 P1 2.2213(11) . ? Co1 Co2 2.4746(7) . ? P1 C17 1.833(4) . ? P1 C11 1.839(4) . ? P1 C23 1.839(4) . ? C1 C2 1.363(5) . ? C1 C10 1.465(5) . ? C1 Co2 1.951(3) . ? C70 Cl1 1.723(7) . ? C70 Cl2 1.741(6) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? Co2 C201 1.777(4) . ? Co2 C202 1.799(4) . ? Co2 C2 1.970(3) . ? Co2 P2 2.2239(11) . ? P2 C30 1.828(4) . ? P2 C24 1.834(4) . ? P2 C23 1.841(4) . ? C2 C3 1.425(5) . ? C67 C68 1.455(12) . ? C67 H67B 0.9800 . ? C67 H67A 0.9800 . ? C67 H67C 0.9800 . ? Co3 C301 1.781(4) . ? Co3 C302 1.805(4) . ? Co3 C4 1.949(4) . ? Co3 C3 1.973(3) . ? Co3 P3 2.2208(10) . ? Co3 Co4 2.4794(6) . ? P3 C36 1.829(4) . ? P3 C48 1.836(4) . ? P3 C42 1.837(4) . ? C3 C4 1.352(5) . ? C3 Co4 1.967(3) . ? C68 C69 1.345(13) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? Co4 C402 1.781(4) . ? Co4 C401 1.781(4) . ? Co4 C4 1.971(3) . ? Co4 P4 2.2280(10) . ? P4 C55' 1.775(13) . ? P4 C49 1.828(4) . ? P4 C48 1.839(4) . ? P4 C55 1.898(13) . ? C4 C5 1.470(5) . ? C69 C69 1.435(14) 2_765 ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C5 C7 1.314(6) . ? C5 C6 1.506(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9500 . ? C7 H7B 0.9500 . ? C8 C10 1.329(6) . ? C8 H8A 0.9500 . ? C8 H8B 0.9500 . ? C9 C10 1.504(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.386(6) . ? C11 C16 1.393(5) . ? C12 C13 1.388(6) . ? C12 H12A 0.9500 . ? C13 C14 1.380(7) . ? C13 H13A 0.9500 . ? C14 C15 1.368(7) . ? C14 H14A 0.9500 . ? C15 C16 1.392(7) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C22 1.381(6) . ? C17 C18 1.402(6) . ? C18 C19 1.391(6) . ? C18 H18A 0.9500 . ? C19 C20 1.373(7) . ? C19 H19A 0.9500 . ? C20 C21 1.385(6) . ? C20 H20A 0.9500 . ? C21 C22 1.384(6) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.386(6) . ? C24 C25 1.393(6) . ? C25 C26 1.393(6) . ? C25 H25A 0.9500 . ? C26 C27 1.373(7) . ? C26 H26A 0.9500 . ? C27 C28 1.381(8) . ? C27 H27A 0.9500 . ? C28 C29 1.386(6) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C35 1.377(6) . ? C30 C31 1.398(6) . ? C31 C32 1.381(7) . ? C31 H31A 0.9500 . ? C32 C33 1.370(9) . ? C32 H32A 0.9500 . ? C33 C34 1.386(9) . ? C33 H33A 0.9500 . ? C34 C35 1.397(7) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.381(6) . ? C36 C41 1.396(6) . ? C37 C38 1.390(6) . ? C37 H37A 0.9500 . ? C38 C39 1.385(9) . ? C38 H38A 0.9500 . ? C39 C40 1.363(9) . ? C39 H39A 0.9500 . ? C40 C41 1.391(7) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 C43 1.386(5) . ? C42 C47 1.396(6) . ? C43 C44 1.392(6) . ? C43 H43A 0.9500 . ? C44 C45 1.386(6) . ? C44 H44A 0.9500 . ? C45 C46 1.374(6) . ? C45 H45A 0.9500 . ? C46 C47 1.386(6) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.390(6) . ? C49 C54 1.392(5) . ? C50 C51 1.389(6) . ? C50 H50A 0.9500 . ? C51 C52 1.390(7) . ? C51 H51A 0.9500 . ? C52 C53 1.372(7) . ? C52 H52A 0.9500 . ? C53 C54 1.391(6) . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? C55 C56 1.317(17) . ? C55 C60 1.429(18) . ? C55' C60' 1.353(18) . ? C55' C56' 1.467(18) . ? C56 C57 1.383(12) . ? C56 H56A 0.9500 . ? C56' C57' 1.399(17) . ? C56' H56B 0.9500 . ? C57 C58 1.366(14) . ? C57 H57A 0.9500 . ? C57' C58' 1.380(18) . ? C57' H57B 0.9500 . ? C58 C59 1.274(18) . ? C58 H58A 0.9500 . ? C58' C59' 1.450(18) . ? C58' H58B 0.9500 . ? C59 C60 1.470(18) . ? C59 H59A 0.9500 . ? C59' C60' 1.337(16) . ? C59' H59B 0.9500 . ? C60 H60A 0.9500 . ? C60' H60B 0.9500 . ? C66 C65 1.51(2) . ? C66 H66C 0.9800 . ? C66 H66B 0.9800 . ? C66 H66A 0.9800 . ? C65 C64 1.48(2) . ? C65 H65B 0.9900 . ? C65 H65A 0.9900 . ? C64 C63 1.496(12) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C63 C62 1.439(12) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C62 C61 1.50(2) . ? C62 H62A 0.9900 . ? C62 H62C 0.9900 . ? C61 H61C 0.9800 . ? C61 H62B 0.9800 . ? C61 H61A 0.9800 . ? O101 C101 1.143(5) . ? O102 C102 1.143(5) . ? O201 C201 1.139(5) . ? O202 C202 1.136(5) . ? O301 C301 1.135(5) . ? O302 C302 1.135(5) . ? O401 C401 1.137(5) . ? O402 C402 1.137(5) . ? 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 C102 Co1 C101 101.73(19) . . ? C102 Co1 C2 104.45(16) . . ? C101 Co1 C2 104.21(17) . . ? C102 Co1 C1 104.34(16) . . ? C101 Co1 C1 140.52(17) . . ? C2 Co1 C1 40.49(15) . . ? C102 Co1 P1 96.30(13) . . ? C101 Co1 P1 108.46(14) . . ? C2 Co1 P1 136.46(11) . . ? C1 Co1 P1 97.61(11) . . ? C102 Co1 Co2 153.03(13) . . ? C101 Co1 Co2 96.27(14) . . ? C2 Co1 Co2 51.11(10) . . ? C1 Co1 Co2 50.53(10) . . ? P1 Co1 Co2 96.84(3) . . ? C17 P1 C11 101.57(18) . . ? C17 P1 C23 104.44(17) . . ? C11 P1 C23 103.40(17) . . ? C17 P1 Co1 119.29(13) . . ? C11 P1 Co1 116.26(12) . . ? C23 P1 Co1 110.11(12) . . ? C2 C1 C10 136.3(3) . . ? C2 C1 Co2 70.4(2) . . ? C10 C1 Co2 139.6(3) . . ? C2 C1 Co1 69.7(2) . . ? C10 C1 Co1 133.6(3) . . ? Co2 C1 Co1 78.28(13) . . ? Cl1 C70 Cl2 111.8(4) . . ? Cl1 C70 H70A 109.3 . . ? Cl2 C70 H70A 109.3 . . ? Cl1 C70 H70B 109.3 . . ? Cl2 C70 H70B 109.3 . . ? H70A C70 H70B 107.9 . . ? C201 Co2 C202 101.2(2) . . ? C201 Co2 C1 99.21(17) . . ? C202 Co2 C1 142.38(17) . . ? C201 Co2 C2 102.90(16) . . ? C202 Co2 C2 103.60(17) . . ? C1 Co2 C2 40.66(15) . . ? C201 Co2 P2 97.76(13) . . ? C202 Co2 P2 106.33(14) . . ? C1 Co2 P2 101.74(11) . . ? C2 Co2 P2 139.22(11) . . ? C201 Co2 Co1 149.44(13) . . ? C202 Co2 Co1 100.73(14) . . ? C1 Co2 Co1 51.18(10) . . ? C2 Co2 Co1 51.04(10) . . ? P2 Co2 Co1 96.16(3) . . ? C30 P2 C24 102.58(18) . . ? C30 P2 C23 103.36(18) . . ? C24 P2 C23 104.16(17) . . ? C30 P2 Co2 115.89(13) . . ? C24 P2 Co2 120.56(14) . . ? C23 P2 Co2 108.46(12) . . ? C1 C2 C3 141.8(3) . . ? C1 C2 Co1 69.8(2) . . ? C3 C2 Co1 137.1(3) . . ? C1 C2 Co2 68.9(2) . . ? C3 C2 Co2 132.5(2) . . ? Co1 C2 Co2 77.85(13) . . ? C68 C67 H67B 109.5 . . ? C68 C67 H67A 109.5 . . ? H67B C67 H67A 109.5 . . ? C68 C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? C301 Co3 C302 100.34(19) . . ? C301 Co3 C4 99.64(17) . . ? C302 Co3 C4 142.97(17) . . ? C301 Co3 C3 103.42(16) . . ? C302 Co3 C3 104.38(17) . . ? C4 Co3 C3 40.33(15) . . ? C301 Co3 P3 97.23(13) . . ? C302 Co3 P3 106.64(13) . . ? C4 Co3 P3 101.36(11) . . ? C3 Co3 P3 138.63(11) . . ? C301 Co3 Co4 149.89(13) . . ? C302 Co3 Co4 101.48(13) . . ? C4 Co3 Co4 51.15(10) . . ? C3 Co3 Co4 50.91(10) . . ? P3 Co3 Co4 96.11(3) . . ? C36 P3 C48 103.31(18) . . ? C36 P3 C42 101.98(18) . . ? C48 P3 C42 104.40(16) . . ? C36 P3 Co3 116.49(13) . . ? C48 P3 Co3 108.63(12) . . ? C42 P3 Co3 120.19(13) . . ? C4 C3 C2 141.9(3) . . ? C4 C3 Co4 70.1(2) . . ? C2 C3 Co4 137.1(3) . . ? C4 C3 Co3 68.9(2) . . ? C2 C3 Co3 132.3(2) . . ? Co4 C3 Co3 77.99(13) . . ? C69 C68 C67 132.2(15) . . ? C69 C68 H68A 104.2 . . ? C67 C68 H68A 104.2 . . ? C69 C68 H68B 104.2 . . ? C67 C68 H68B 104.2 . . ? H68A C68 H68B 105.5 . . ? C402 Co4 C401 100.01(19) . . ? C402 Co4 C3 104.38(16) . . ? C401 Co4 C3 103.47(16) . . ? C402 Co4 C4 104.76(16) . . ? C401 Co4 C4 140.05(16) . . ? C3 Co4 C4 40.16(15) . . ? C402 Co4 P4 96.78(13) . . ? C401 Co4 P4 109.40(13) . . ? C3 Co4 P4 136.81(11) . . ? C4 Co4 P4 98.32(11) . . ? C402 Co4 Co3 153.18(13) . . ? C401 Co4 Co3 96.96(13) . . ? C3 Co4 Co3 51.11(10) . . ? C4 Co4 Co3 50.39(10) . . ? P4 Co4 Co3 96.97(3) . . ? C55' P4 C49 99.5(5) . . ? C55' P4 C48 105.7(5) . . ? C49 P4 C48 103.93(17) . . ? C55' P4 C55 6.0(7) . . ? C49 P4 C55 104.2(4) . . ? C48 P4 C55 100.8(4) . . ? C55' P4 Co4 116.5(5) . . ? C49 P4 Co4 120.33(13) . . ? C48 P4 Co4 109.30(12) . . ? C55 P4 Co4 116.0(4) . . ? C3 C4 C5 135.9(4) . . ? C3 C4 Co3 70.8(2) . . ? C5 C4 Co3 139.4(3) . . ? C3 C4 Co4 69.8(2) . . ? C5 C4 Co4 133.8(3) . . ? Co3 C4 Co4 78.46(13) . . ? C68 C69 C69 134.9(17) . 2_765 ? C68 C69 H69A 103.5 . . ? C69 C69 H69A 103.5 2_765 . ? C68 C69 H69B 103.5 . . ? C69 C69 H69B 103.5 2_765 . ? H69A C69 H69B 105.3 . . ? C7 C5 C4 122.9(4) . . ? C7 C5 C6 121.8(4) . . ? C4 C5 C6 115.2(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 120.0 . . ? C5 C7 H7B 120.0 . . ? H7A C7 H7B 120.0 . . ? C10 C8 H8A 120.0 . . ? C10 C8 H8B 120.0 . . ? H8A C8 H8B 120.0 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 C1 123.1(4) . . ? C8 C10 C9 121.3(4) . . ? C1 C10 C9 115.5(3) . . ? C12 C11 C16 118.3(4) . . ? C12 C11 P1 123.0(3) . . ? C16 C11 P1 118.5(3) . . ? C11 C12 C13 120.7(4) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 120.5(5) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C15 C14 C13 119.4(4) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C14 C15 C16 120.6(4) . . ? C14 C15 H15A 119.7 . . ? C16 C15 H15A 119.7 . . ? C15 C16 C11 120.5(4) . . ? C15 C16 H16A 119.8 . . ? C11 C16 H16A 119.8 . . ? C22 C17 C18 118.8(4) . . ? C22 C17 P1 122.5(3) . . ? C18 C17 P1 118.7(3) . . ? C19 C18 C17 119.9(4) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C20 C19 C18 120.6(4) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C19 C20 C21 119.7(4) . . ? C19 C20 H20A 120.2 . . ? C21 C20 H20A 120.2 . . ? C22 C21 C20 120.2(4) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C17 C22 C21 120.8(4) . . ? C17 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? P1 C23 P2 108.49(19) . . ? P1 C23 H23A 110.0 . . ? P2 C23 H23A 110.0 . . ? P1 C23 H23B 110.0 . . ? P2 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? C29 C24 C25 118.7(4) . . ? C29 C24 P2 122.0(3) . . ? C25 C24 P2 119.2(3) . . ? C24 C25 C26 120.5(4) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C27 C26 C25 119.7(5) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C28 120.5(4) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C27 C28 C29 119.8(4) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C28 C29 C24 120.8(4) . . ? C28 C29 H29A 119.6 . . ? C24 C29 H29A 119.6 . . ? C35 C30 C31 118.8(4) . . ? C35 C30 P2 124.3(3) . . ? C31 C30 P2 116.7(3) . . ? C32 C31 C30 121.1(5) . . ? C32 C31 H31A 119.4 . . ? C30 C31 H31A 119.4 . . ? C33 C32 C31 119.4(5) . . ? C33 C32 H32A 120.3 . . ? C31 C32 H32A 120.3 . . ? C32 C33 C34 120.7(5) . . ? C32 C33 H33A 119.6 . . ? C34 C33 H33A 119.6 . . ? C33 C34 C35 119.6(6) . . ? C33 C34 H34A 120.2 . . ? C35 C34 H34A 120.2 . . ? C30 C35 C34 120.3(5) . . ? C30 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C37 C36 C41 119.0(4) . . ? C37 C36 P3 124.2(3) . . ? C41 C36 P3 116.7(3) . . ? C36 C37 C38 120.8(5) . . ? C36 C37 H37A 119.6 . . ? C38 C37 H37A 119.6 . . ? C39 C38 C37 119.4(6) . . ? C39 C38 H38A 120.3 . . ? C37 C38 H38A 120.3 . . ? C40 C39 C38 120.5(5) . . ? C40 C39 H39A 119.7 . . ? C38 C39 H39A 119.7 . . ? C39 C40 C41 120.3(5) . . ? C39 C40 H40A 119.8 . . ? C41 C40 H40A 119.9 . . ? C40 C41 C36 120.0(5) . . ? C40 C41 H41A 120.0 . . ? C36 C41 H41A 120.0 . . ? C43 C42 C47 118.8(3) . . ? C43 C42 P3 121.9(3) . . ? C47 C42 P3 119.3(3) . . ? C42 C43 C44 120.4(4) . . ? C42 C43 H43A 119.8 . . ? C44 C43 H43A 119.8 . . ? C45 C44 C43 120.2(4) . . ? C45 C44 H44A 119.9 . . ? C43 C44 H44A 119.9 . . ? C46 C45 C44 119.6(4) . . ? C46 C45 H45A 120.2 . . ? C44 C45 H45A 120.2 . . ? C45 C46 C47 120.5(4) . . ? C45 C46 H46A 119.7 . . ? C47 C46 H46A 119.7 . . ? C46 C47 C42 120.5(4) . . ? C46 C47 H47A 119.8 . . ? C42 C47 H47A 119.8 . . ? P3 C48 P4 109.00(19) . . ? P3 C48 H48A 109.9 . . ? P4 C48 H48A 109.9 . . ? P3 C48 H48B 109.9 . . ? P4 C48 H48B 109.9 . . ? H48A C48 H48B 108.3 . . ? C50 C49 C54 118.4(4) . . ? C50 C49 P4 121.6(3) . . ? C54 C49 P4 120.0(3) . . ? C51 C50 C49 120.8(4) . . ? C51 C50 H50A 119.6 . . ? C49 C50 H50A 119.6 . . ? C50 C51 C52 120.0(4) . . ? C50 C51 H51A 120.0 . . ? C52 C51 H51A 120.0 . . ? C53 C52 C51 119.6(4) . . ? C53 C52 H52A 120.2 . . ? C51 C52 H52A 120.2 . . ? C52 C53 C54 120.4(4) . . ? C52 C53 H53A 119.8 . . ? C54 C53 H53A 119.8 . . ? C53 C54 C49 120.7(4) . . ? C53 C54 H54A 119.6 . . ? C49 C54 H54A 119.6 . . ? C56 C55 C60 121.4(11) . . ? C56 C55 P4 123.7(9) . . ? C60 C55 P4 113.8(10) . . ? C60' C55' C56' 115.1(12) . . ? C60' C55' P4 124.5(11) . . ? C56' C55' P4 120.2(9) . . ? C55 C56 C57 121.1(9) . . ? C55 C56 H56A 119.4 . . ? C57 C56 H56A 119.4 . . ? C57' C56' C55' 119.6(12) . . ? C57' C56' H56B 120.2 . . ? C55' C56' H56B 120.2 . . ? C58 C57 C56 120.3(9) . . ? C58 C57 H57A 119.8 . . ? C56 C57 H57A 119.8 . . ? C58' C57' C56' 120.7(13) . . ? C58' C57' H57B 119.6 . . ? C56' C57' H57B 119.7 . . ? C59 C58 C57 119.8(11) . . ? C59 C58 H58A 120.1 . . ? C57 C58 H58A 120.1 . . ? C57' C58' C59' 119.2(12) . . ? C57' C58' H58B 120.4 . . ? C59' C58' H58B 120.4 . . ? C58 C59 C60 124.0(12) . . ? C58 C59 H59A 118.0 . . ? C60 C59 H59A 118.0 . . ? C60' C59' C58' 117.0(11) . . ? C60' C59' H59B 121.5 . . ? C58' C59' H59B 121.5 . . ? C55 C60 C59 113.0(12) . . ? C55 C60 H60A 123.5 . . ? C59 C60 H60A 123.5 . . ? C59' C60' C55' 127.8(13) . . ? C59' C60' H60B 116.1 . . ? C55' C60' H60B 116.1 . . ? C65 C66 H66C 109.5 . . ? C65 C66 H66B 109.3 . . ? H66C C66 H66B 109.5 . . ? C65 C66 H66A 109.6 . . ? H66C C66 H66A 109.5 . . ? H66B C66 H66A 109.5 . . ? C64 C65 C66 115(2) . . ? C64 C65 H65B 108.4 . . ? C66 C65 H65B 108.3 . . ? C64 C65 H65A 108.5 . . ? C66 C65 H65A 108.7 . . ? H65B C65 H65A 107.5 . . ? C65 C64 C63 120(2) . . ? C65 C64 H64A 107.3 . . ? C63 C64 H64A 107.3 . . ? C65 C64 H64B 107.2 . . ? C63 C64 H64B 107.3 . . ? H64A C64 H64B 106.9 . . ? C62 C63 C64 120.2(10) . . ? C62 C63 H63A 107.3 . . ? C64 C63 H63A 107.3 . . ? C62 C63 H63B 107.3 . . ? C64 C63 H63B 107.3 . . ? H63A C63 H63B 106.9 . . ? C63 C62 C61 118(2) . . ? C63 C62 H62A 107.8 . . ? C61 C62 H62A 108.0 . . ? C63 C62 H62C 107.8 . . ? C61 C62 H62C 107.7 . . ? H62A C62 H62C 107.2 . . ? C62 C61 H61C 109.5 . . ? C62 C61 H62B 109.6 . . ? H61C C61 H62B 109.5 . . ? C62 C61 H61A 109.3 . . ? H61C C61 H61A 109.5 . . ? H62B C61 H61A 109.5 . . ? O101 C101 Co1 177.3(4) . . ? O102 C102 Co1 177.3(4) . . ? O201 C201 Co2 178.5(4) . . ? O202 C202 Co2 176.7(4) . . ? O301 C301 Co3 179.8(5) . . ? O302 C302 Co3 178.3(4) . . ? O401 C401 Co4 176.5(4) . . ? O402 C402 Co4 178.2(4) . . ? 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 C102 Co1 P1 C17 -102.38(19) . . . . ? C101 Co1 P1 C17 2.2(2) . . . . ? C2 Co1 P1 C17 138.9(2) . . . . ? C1 Co1 P1 C17 152.18(17) . . . . ? Co2 Co1 P1 C17 101.22(14) . . . . ? C102 Co1 P1 C11 19.86(19) . . . . ? C101 Co1 P1 C11 124.5(2) . . . . ? C2 Co1 P1 C11 -98.9(2) . . . . ? C1 Co1 P1 C11 -85.58(17) . . . . ? Co2 Co1 P1 C11 -136.54(14) . . . . ? C102 Co1 P1 C23 136.97(18) . . . . ? C101 Co1 P1 C23 -118.41(19) . . . . ? C2 Co1 P1 C23 18.2(2) . . . . ? C1 Co1 P1 C23 31.53(16) . . . . ? Co2 Co1 P1 C23 -19.43(13) . . . . ? C102 Co1 C1 C2 95.6(2) . . . . ? C101 Co1 C1 C2 -34.2(3) . . . . ? P1 Co1 C1 C2 -165.88(18) . . . . ? Co2 Co1 C1 C2 -73.26(19) . . . . ? C102 Co1 C1 C10 -39.9(4) . . . . ? C101 Co1 C1 C10 -169.7(3) . . . . ? C2 Co1 C1 C10 -135.5(5) . . . . ? P1 Co1 C1 C10 58.6(4) . . . . ? Co2 Co1 C1 C10 151.2(4) . . . . ? C102 Co1 C1 Co2 168.84(15) . . . . ? C101 Co1 C1 Co2 39.0(3) . . . . ? C2 Co1 C1 Co2 73.26(19) . . . . ? P1 Co1 C1 Co2 -92.62(9) . . . . ? C2 C1 Co2 C201 -99.1(2) . . . . ? C10 C1 Co2 C201 41.0(4) . . . . ? Co1 C1 Co2 C201 -171.53(15) . . . . ? C2 C1 Co2 C202 23.2(4) . . . . ? C10 C1 Co2 C202 163.2(4) . . . . ? Co1 C1 Co2 C202 -49.3(3) . . . . ? C10 C1 Co2 C2 140.1(5) . . . . ? Co1 C1 Co2 C2 -72.42(19) . . . . ? C2 C1 Co2 P2 160.91(18) . . . . ? C10 C1 Co2 P2 -59.0(4) . . . . ? Co1 C1 Co2 P2 88.48(9) . . . . ? C2 C1 Co2 Co1 72.42(19) . . . . ? C10 C1 Co2 Co1 -147.5(5) . . . . ? C102 Co1 Co2 C201 -7.8(4) . . . . ? C101 Co1 Co2 C201 -139.6(3) . . . . ? C2 Co1 Co2 C201 -36.4(3) . . . . ? C1 Co1 Co2 C201 16.6(3) . . . . ? P1 Co1 Co2 C201 110.9(3) . . . . ? C102 Co1 Co2 C202 127.5(3) . . . . ? C101 Co1 Co2 C202 -4.3(2) . . . . ? C2 Co1 Co2 C202 98.89(19) . . . . ? C1 Co1 Co2 C202 151.9(2) . . . . ? P1 Co1 Co2 C202 -113.85(14) . . . . ? C102 Co1 Co2 C1 -24.4(3) . . . . ? C101 Co1 Co2 C1 -156.2(2) . . . . ? C2 Co1 Co2 C1 -53.02(19) . . . . ? P1 Co1 Co2 C1 94.24(14) . . . . ? C102 Co1 Co2 C2 28.6(3) . . . . ? C101 Co1 Co2 C2 -103.22(19) . . . . ? C1 Co1 Co2 C2 53.02(19) . . . . ? P1 Co1 Co2 C2 147.27(14) . . . . ? C102 Co1 Co2 P2 -124.5(3) . . . . ? C101 Co1 Co2 P2 103.63(14) . . . . ? C2 Co1 Co2 P2 -153.15(14) . . . . ? C1 Co1 Co2 P2 -100.13(14) . . . . ? P1 Co1 Co2 P2 -5.88(4) . . . . ? C201 Co2 P2 C30 -6.8(2) . . . . ? C202 Co2 P2 C30 -110.9(2) . . . . ? C1 Co2 P2 C30 94.38(18) . . . . ? C2 Co2 P2 C30 113.4(2) . . . . ? Co1 Co2 P2 C30 145.95(15) . . . . ? C201 Co2 P2 C24 117.8(2) . . . . ? C202 Co2 P2 C24 13.7(2) . . . . ? C1 Co2 P2 C24 -141.03(18) . . . . ? C2 Co2 P2 C24 -122.0(2) . . . . ? Co1 Co2 P2 C24 -89.45(14) . . . . ? C201 Co2 P2 C23 -122.41(19) . . . . ? C202 Co2 P2 C23 133.42(19) . . . . ? C1 Co2 P2 C23 -21.26(17) . . . . ? C2 Co2 P2 C23 -2.2(2) . . . . ? Co1 Co2 P2 C23 30.31(13) . . . . ? C10 C1 C2 C3 -9.9(8) . . . . ? Co2 C1 C2 C3 133.0(5) . . . . ? Co1 C1 C2 C3 -142.7(5) . . . . ? C10 C1 C2 Co1 132.7(5) . . . . ? Co2 C1 C2 Co1 -84.35(10) . . . . ? C10 C1 C2 Co2 -142.9(5) . . . . ? Co1 C1 C2 Co2 84.35(10) . . . . ? C102 Co1 C2 C1 -95.3(2) . . . . ? C101 Co1 C2 C1 158.3(2) . . . . ? P1 Co1 C2 C1 20.5(3) . . . . ? Co2 Co1 C2 C1 71.76(19) . . . . ? C102 Co1 C2 C3 51.3(4) . . . . ? C101 Co1 C2 C3 -55.1(4) . . . . ? C1 Co1 C2 C3 146.6(5) . . . . ? P1 Co1 C2 C3 167.2(3) . . . . ? Co2 Co1 C2 C3 -141.6(4) . . . . ? C102 Co1 C2 Co2 -167.04(15) . . . . ? C101 Co1 C2 Co2 86.59(17) . . . . ? C1 Co1 C2 Co2 -71.76(19) . . . . ? P1 Co1 C2 Co2 -51.21(17) . . . . ? C201 Co2 C2 C1 89.2(2) . . . . ? C202 Co2 C2 C1 -165.7(2) . . . . ? P2 Co2 C2 C1 -29.4(3) . . . . ? Co1 Co2 C2 C1 -72.8(2) . . . . ? C201 Co2 C2 C3 -53.0(4) . . . . ? C202 Co2 C2 C3 52.1(4) . . . . ? C1 Co2 C2 C3 -142.2(5) . . . . ? P2 Co2 C2 C3 -171.5(3) . . . . ? Co1 Co2 C2 C3 145.0(4) . . . . ? C201 Co2 C2 Co1 161.96(16) . . . . ? C202 Co2 C2 Co1 -92.91(17) . . . . ? C1 Co2 C2 Co1 72.8(2) . . . . ? P2 Co2 C2 Co1 43.44(19) . . . . ? C301 Co3 P3 C36 -7.6(2) . . . . ? C302 Co3 P3 C36 -110.7(2) . . . . ? C4 Co3 P3 C36 93.77(19) . . . . ? C3 Co3 P3 C36 112.2(2) . . . . ? Co4 Co3 P3 C36 145.31(15) . . . . ? C301 Co3 P3 C48 -123.71(18) . . . . ? C302 Co3 P3 C48 133.18(18) . . . . ? C4 Co3 P3 C48 -22.30(16) . . . . ? C3 Co3 P3 C48 -3.8(2) . . . . ? Co4 Co3 P3 C48 29.24(13) . . . . ? C301 Co3 P3 C42 116.31(19) . . . . ? C302 Co3 P3 C42 13.20(19) . . . . ? C4 Co3 P3 C42 -142.29(17) . . . . ? C3 Co3 P3 C42 -123.8(2) . . . . ? Co4 Co3 P3 C42 -90.74(13) . . . . ? C1 C2 C3 C4 169.5(5) . . . . ? Co1 C2 C3 C4 46.2(7) . . . . ? Co2 C2 C3 C4 -78.4(6) . . . . ? C1 C2 C3 Co4 45.5(7) . . . . ? Co1 C2 C3 Co4 -77.7(5) . . . . ? Co2 C2 C3 Co4 157.7(2) . . . . ? C1 C2 C3 Co3 -78.7(6) . . . . ? Co1 C2 C3 Co3 158.0(2) . . . . ? Co2 C2 C3 Co3 33.4(5) . . . . ? C301 Co3 C3 C4 89.1(2) . . . . ? C302 Co3 C3 C4 -166.3(2) . . . . ? P3 Co3 C3 C4 -28.7(3) . . . . ? Co4 Co3 C3 C4 -73.0(2) . . . . ? C301 Co3 C3 C2 -53.0(4) . . . . ? C302 Co3 C3 C2 51.6(4) . . . . ? C4 Co3 C3 C2 -142.1(4) . . . . ? P3 Co3 C3 C2 -170.8(3) . . . . ? Co4 Co3 C3 C2 144.9(4) . . . . ? C301 Co3 C3 Co4 162.18(16) . . . . ? C302 Co3 C3 Co4 -93.24(15) . . . . ? C4 Co3 C3 Co4 73.0(2) . . . . ? P3 Co3 C3 Co4 44.36(19) . . . . ? C4 C3 Co4 C402 -96.0(2) . . . . ? C2 C3 Co4 C402 51.0(4) . . . . ? Co3 C3 Co4 C402 -167.65(15) . . . . ? C4 C3 Co4 C401 159.8(2) . . . . ? C2 C3 Co4 C401 -53.2(4) . . . . ? Co3 C3 Co4 C401 88.11(16) . . . . ? C2 C3 Co4 C4 147.0(5) . . . . ? Co3 C3 Co4 C4 -71.7(2) . . . . ? C4 C3 Co4 P4 20.8(3) . . . . ? C2 C3 Co4 P4 167.9(3) . . . . ? Co3 C3 Co4 P4 -50.84(18) . . . . ? C4 C3 Co4 Co3 71.7(2) . . . . ? C2 C3 Co4 Co3 -141.3(4) . . . . ? C301 Co3 Co4 C402 -9.1(4) . . . . ? C302 Co3 Co4 C402 126.6(3) . . . . ? C4 Co3 Co4 C402 -25.3(3) . . . . ? C3 Co3 Co4 C402 27.3(3) . . . . ? P3 Co3 Co4 C402 -125.0(3) . . . . ? C301 Co3 Co4 C401 -138.1(3) . . . . ? C302 Co3 Co4 C401 -2.41(18) . . . . ? C4 Co3 Co4 C401 -154.34(19) . . . . ? C3 Co3 Co4 C401 -101.71(18) . . . . ? P3 Co3 Co4 C401 105.98(13) . . . . ? C301 Co3 Co4 C3 -36.4(3) . . . . ? C302 Co3 Co4 C3 99.29(19) . . . . ? C4 Co3 Co4 C3 -52.63(19) . . . . ? P3 Co3 Co4 C3 -152.31(14) . . . . ? C301 Co3 Co4 C4 16.2(3) . . . . ? C302 Co3 Co4 C4 151.93(19) . . . . ? C3 Co3 Co4 C4 52.63(19) . . . . ? P3 Co3 Co4 C4 -99.68(14) . . . . ? C301 Co3 Co4 P4 111.3(3) . . . . ? C302 Co3 Co4 P4 -113.03(13) . . . . ? C4 Co3 Co4 P4 95.05(14) . . . . ? C3 Co3 Co4 P4 147.68(14) . . . . ? P3 Co3 Co4 P4 -4.63(4) . . . . ? C402 Co4 P4 C55' 16.7(5) . . . . ? C401 Co4 P4 C55' 119.8(5) . . . . ? C3 Co4 P4 C55' -102.8(5) . . . . ? C4 Co4 P4 C55' -89.4(5) . . . . ? Co3 Co4 P4 C55' -140.2(5) . . . . ? C402 Co4 P4 C49 -103.59(19) . . . . ? C401 Co4 P4 C49 -0.44(19) . . . . ? C3 Co4 P4 C49 136.94(19) . . . . ? C4 Co4 P4 C49 150.35(17) . . . . ? Co3 Co4 P4 C49 99.50(13) . . . . ? C402 Co4 P4 C48 136.38(18) . . . . ? C401 Co4 P4 C48 -120.47(19) . . . . ? C3 Co4 P4 C48 16.9(2) . . . . ? C4 Co4 P4 C48 30.32(17) . . . . ? Co3 Co4 P4 C48 -20.53(13) . . . . ? C402 Co4 P4 C55 23.3(5) . . . . ? C401 Co4 P4 C55 126.4(5) . . . . ? C3 Co4 P4 C55 -96.2(5) . . . . ? C4 Co4 P4 C55 -82.8(5) . . . . ? Co3 Co4 P4 C55 -133.6(5) . . . . ? C2 C3 C4 C5 -10.3(8) . . . . ? Co4 C3 C4 C5 132.8(4) . . . . ? Co3 C3 C4 C5 -142.8(5) . . . . ? C2 C3 C4 Co3 132.5(5) . . . . ? Co4 C3 C4 Co3 -84.41(10) . . . . ? C2 C3 C4 Co4 -143.0(5) . . . . ? Co3 C3 C4 Co4 84.41(10) . . . . ? C301 Co3 C4 C3 -99.4(2) . . . . ? C302 Co3 C4 C3 22.4(4) . . . . ? P3 Co3 C4 C3 161.12(18) . . . . ? Co4 Co3 C4 C3 72.40(19) . . . . ? C301 Co3 C4 C5 40.2(4) . . . . ? C302 Co3 C4 C5 162.1(4) . . . . ? C3 Co3 C4 C5 139.7(5) . . . . ? P3 Co3 C4 C5 -59.2(4) . . . . ? Co4 Co3 C4 C5 -147.9(5) . . . . ? C301 Co3 C4 Co4 -171.82(15) . . . . ? C302 Co3 C4 Co4 -50.0(3) . . . . ? C3 Co3 C4 Co4 -72.40(19) . . . . ? P3 Co3 C4 Co4 88.72(10) . . . . ? C402 Co4 C4 C3 94.9(2) . . . . ? C401 Co4 C4 C3 -31.5(4) . . . . ? P4 Co4 C4 C3 -165.75(19) . . . . ? Co3 Co4 C4 C3 -73.6(2) . . . . ? C402 Co4 C4 C5 -40.1(4) . . . . ? C401 Co4 C4 C5 -166.5(4) . . . . ? C3 Co4 C4 C5 -135.0(5) . . . . ? P4 Co4 C4 C5 59.3(4) . . . . ? Co3 Co4 C4 C5 151.4(4) . . . . ? C402 Co4 C4 Co3 168.49(15) . . . . ? C401 Co4 C4 Co3 42.0(3) . . . . ? C3 Co4 C4 Co3 73.6(2) . . . . ? P4 Co4 C4 Co3 -92.19(9) . . . . ? C67 C68 C69 C69 -179(2) . . . 2_765 ? C3 C4 C5 C7 116.6(5) . . . . ? Co3 C4 C5 C7 -2.0(7) . . . . ? Co4 C4 C5 C7 -135.9(4) . . . . ? C3 C4 C5 C6 -60.7(6) . . . . ? Co3 C4 C5 C6 -179.2(3) . . . . ? Co4 C4 C5 C6 46.9(5) . . . . ? C2 C1 C10 C8 116.9(5) . . . . ? Co2 C1 C10 C8 -1.9(7) . . . . ? Co1 C1 C10 C8 -135.3(4) . . . . ? C2 C1 C10 C9 -62.6(6) . . . . ? Co2 C1 C10 C9 178.6(3) . . . . ? Co1 C1 C10 C9 45.2(5) . . . . ? C17 P1 C11 C12 -139.1(4) . . . . ? C23 P1 C11 C12 -31.0(4) . . . . ? Co1 P1 C11 C12 89.8(3) . . . . ? C17 P1 C11 C16 46.0(4) . . . . ? C23 P1 C11 C16 154.1(3) . . . . ? Co1 P1 C11 C16 -85.1(3) . . . . ? C16 C11 C12 C13 -0.9(7) . . . . ? P1 C11 C12 C13 -175.8(4) . . . . ? C11 C12 C13 C14 -0.8(7) . . . . ? C12 C13 C14 C15 1.7(8) . . . . ? C13 C14 C15 C16 -1.0(8) . . . . ? C14 C15 C16 C11 -0.7(8) . . . . ? C12 C11 C16 C15 1.7(7) . . . . ? P1 C11 C16 C15 176.8(4) . . . . ? C11 P1 C17 C22 80.5(4) . . . . ? C23 P1 C17 C22 -26.8(4) . . . . ? Co1 P1 C17 C22 -150.2(3) . . . . ? C11 P1 C17 C18 -100.7(3) . . . . ? C23 P1 C17 C18 152.1(3) . . . . ? Co1 P1 C17 C18 28.6(4) . . . . ? C22 C17 C18 C19 1.1(6) . . . . ? P1 C17 C18 C19 -177.8(4) . . . . ? C17 C18 C19 C20 1.3(8) . . . . ? C18 C19 C20 C21 -1.9(8) . . . . ? C19 C20 C21 C22 0.1(7) . . . . ? C18 C17 C22 C21 -2.8(6) . . . . ? P1 C17 C22 C21 176.0(3) . . . . ? C20 C21 C22 C17 2.2(7) . . . . ? C17 P1 C23 P2 -85.9(2) . . . . ? C11 P1 C23 P2 168.13(19) . . . . ? Co1 P1 C23 P2 43.3(2) . . . . ? C30 P2 C23 P1 -171.64(19) . . . . ? C24 P2 C23 P1 81.5(2) . . . . ? Co2 P2 C23 P1 -48.1(2) . . . . ? C30 P2 C24 C29 -26.7(4) . . . . ? C23 P2 C24 C29 80.8(4) . . . . ? Co2 P2 C24 C29 -157.3(3) . . . . ? C30 P2 C24 C25 156.0(3) . . . . ? C23 P2 C24 C25 -96.5(3) . . . . ? Co2 P2 C24 C25 25.4(4) . . . . ? C29 C24 C25 C26 -1.9(6) . . . . ? P2 C24 C25 C26 175.5(4) . . . . ? C24 C25 C26 C27 1.2(7) . . . . ? C25 C26 C27 C28 -0.1(8) . . . . ? C26 C27 C28 C29 -0.2(8) . . . . ? C27 C28 C29 C24 -0.5(7) . . . . ? C25 C24 C29 C28 1.6(6) . . . . ? P2 C24 C29 C28 -175.7(4) . . . . ? C24 P2 C30 C35 116.5(4) . . . . ? C23 P2 C30 C35 8.4(4) . . . . ? Co2 P2 C30 C35 -110.0(4) . . . . ? C24 P2 C30 C31 -68.0(4) . . . . ? C23 P2 C30 C31 -176.1(3) . . . . ? Co2 P2 C30 C31 65.5(4) . . . . ? C35 C30 C31 C32 1.5(7) . . . . ? P2 C30 C31 C32 -174.2(4) . . . . ? C30 C31 C32 C33 0.8(8) . . . . ? C31 C32 C33 C34 -2.0(9) . . . . ? C32 C33 C34 C35 0.9(10) . . . . ? C31 C30 C35 C34 -2.6(7) . . . . ? P2 C30 C35 C34 172.8(4) . . . . ? C33 C34 C35 C30 1.5(9) . . . . ? C48 P3 C36 C37 9.3(4) . . . . ? C42 P3 C36 C37 117.5(4) . . . . ? Co3 P3 C36 C37 -109.6(3) . . . . ? C48 P3 C36 C41 -174.3(3) . . . . ? C42 P3 C36 C41 -66.2(4) . . . . ? Co3 P3 C36 C41 66.7(4) . . . . ? C41 C36 C37 C38 -1.0(7) . . . . ? P3 C36 C37 C38 175.2(4) . . . . ? C36 C37 C38 C39 -0.1(8) . . . . ? C37 C38 C39 C40 1.8(9) . . . . ? C38 C39 C40 C41 -2.5(9) . . . . ? C39 C40 C41 C36 1.4(8) . . . . ? C37 C36 C41 C40 0.4(7) . . . . ? P3 C36 C41 C40 -176.2(4) . . . . ? C36 P3 C42 C43 -25.4(3) . . . . ? C48 P3 C42 C43 81.9(3) . . . . ? Co3 P3 C42 C43 -156.1(3) . . . . ? C36 P3 C42 C47 156.1(3) . . . . ? C48 P3 C42 C47 -96.6(3) . . . . ? Co3 P3 C42 C47 25.5(3) . . . . ? C47 C42 C43 C44 1.5(6) . . . . ? P3 C42 C43 C44 -176.9(3) . . . . ? C42 C43 C44 C45 -1.2(6) . . . . ? C43 C44 C45 C46 0.7(7) . . . . ? C44 C45 C46 C47 -0.6(7) . . . . ? C45 C46 C47 C42 0.9(6) . . . . ? C43 C42 C47 C46 -1.4(6) . . . . ? P3 C42 C47 C46 177.1(3) . . . . ? C36 P3 C48 P4 -172.42(19) . . . . ? C42 P3 C48 P4 81.3(2) . . . . ? Co3 P3 C48 P4 -48.1(2) . . . . ? C55' P4 C48 P3 170.1(5) . . . . ? C49 P4 C48 P3 -85.6(2) . . . . ? C55 P4 C48 P3 166.6(4) . . . . ? Co4 P4 C48 P3 44.0(2) . . . . ? C55' P4 C49 C50 75.4(5) . . . . ? C48 P4 C49 C50 -33.6(3) . . . . ? C55 P4 C49 C50 71.6(5) . . . . ? Co4 P4 C49 C50 -156.2(3) . . . . ? C55' P4 C49 C54 -106.2(5) . . . . ? C48 P4 C49 C54 144.8(3) . . . . ? C55 P4 C49 C54 -110.0(5) . . . . ? Co4 P4 C49 C54 22.1(4) . . . . ? C54 C49 C50 C51 -2.7(6) . . . . ? P4 C49 C50 C51 175.7(3) . . . . ? C49 C50 C51 C52 1.0(7) . . . . ? C50 C51 C52 C53 1.7(7) . . . . ? C51 C52 C53 C54 -2.7(7) . . . . ? C52 C53 C54 C49 0.9(7) . . . . ? C50 C49 C54 C53 1.8(6) . . . . ? P4 C49 C54 C53 -176.7(3) . . . . ? C55' P4 C55 C56 170(9) . . . . ? C49 P4 C55 C56 -151.5(11) . . . . ? C48 P4 C55 C56 -44.0(12) . . . . ? Co4 P4 C55 C56 73.9(12) . . . . ? C55' P4 C55 C60 2(7) . . . . ? C49 P4 C55 C60 40.4(10) . . . . ? C48 P4 C55 C60 147.9(9) . . . . ? Co4 P4 C55 C60 -94.2(10) . . . . ? C49 P4 C55' C60' 55.5(13) . . . . ? C48 P4 C55' C60' 163.0(11) . . . . ? C55 P4 C55' C60' -162(9) . . . . ? Co4 P4 C55' C60' -75.4(13) . . . . ? C49 P4 C55' C56' -129.5(10) . . . . ? C48 P4 C55' C56' -22.1(12) . . . . ? C55 P4 C55' C56' 13(7) . . . . ? Co4 P4 C55' C56' 99.5(11) . . . . ? C60 C55 C56 C57 -4.5(19) . . . . ? P4 C55 C56 C57 -171.7(8) . . . . ? C60' C55' C56' C57' 1.3(19) . . . . ? P4 C55' C56' C57' -174.2(11) . . . . ? C55 C56 C57 C58 4.9(17) . . . . ? C55' C56' C57' C58' -7(2) . . . . ? C56 C57 C58 C59 -4.6(18) . . . . ? C56' C57' C58' C59' 9(2) . . . . ? C57 C58 C59 C60 4(2) . . . . ? C57' C58' C59' C60' -4.6(18) . . . . ? C56 C55 C60 C59 3.6(18) . . . . ? P4 C55 C60 C59 172.0(9) . . . . ? C58 C59 C60 C55 -3(2) . . . . ? C58' C59' C60' C55' -2(2) . . . . ? C56' C55' C60' C59' 3(2) . . . . ? P4 C55' C60' C59' 178.6(11) . . . . ? C66 C65 C64 C63 166(13) . . . . ? C65 C64 C63 C62 -155(6) . . . . ? C64 C63 C62 C61 -176(21) . . . . ? C102 Co1 C101 O101 -90(9) . . . . ? C2 Co1 C101 O101 18(9) . . . . ? C1 Co1 C101 O101 41(9) . . . . ? P1 Co1 C101 O101 169(9) . . . . ? Co2 Co1 C101 O101 70(9) . . . . ? C101 Co1 C102 O102 -109(8) . . . . ? C2 Co1 C102 O102 143(8) . . . . ? C1 Co1 C102 O102 101(8) . . . . ? P1 Co1 C102 O102 2(8) . . . . ? Co2 Co1 C102 O102 120(8) . . . . ? C202 Co2 C201 O201 -172(100) . . . . ? C1 Co2 C201 O201 -24(15) . . . . ? C2 Co2 C201 O201 -65(15) . . . . ? P2 Co2 C201 O201 79(15) . . . . ? Co1 Co2 C201 O201 -37(15) . . . . ? C201 Co2 C202 O202 76(7) . . . . ? C1 Co2 C202 O202 -46(7) . . . . ? C2 Co2 C202 O202 -31(7) . . . . ? P2 Co2 C202 O202 177(100) . . . . ? Co1 Co2 C202 O202 -83(7) . . . . ? C302 Co3 C301 O301 -166(100) . . . . ? C4 Co3 C301 O301 -18(100) . . . . ? C3 Co3 C301 O301 -59(100) . . . . ? P3 Co3 C301 O301 85(100) . . . . ? Co4 Co3 C301 O301 -30(100) . . . . ? C301 Co3 C302 O302 75(13) . . . . ? C4 Co3 C302 O302 -47(13) . . . . ? C3 Co3 C302 O302 -32(13) . . . . ? P3 Co3 C302 O302 176(100) . . . . ? Co4 Co3 C302 O302 -84(13) . . . . ? C402 Co4 C401 O401 -80(6) . . . . ? C3 Co4 C401 O401 28(6) . . . . ? C4 Co4 C401 O401 48(7) . . . . ? P4 Co4 C401 O401 180(100) . . . . ? Co3 Co4 C401 O401 80(6) . . . . ? C401 Co4 C402 O402 -62(13) . . . . ? C3 Co4 C402 O402 -169(13) . . . . ? C4 Co4 C402 O402 150(13) . . . . ? P4 Co4 C402 O402 49(13) . . . . ? Co3 Co4 C402 O402 170(13) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.658 _refine_diff_density_min -2.589 _refine_diff_density_rms 0.102 #===END data_mm0129_COMPOUND_8 _database_code_depnum_ccdc_archive 'CCDC 228901' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H44 Co2 O8 P4' _chemical_formula_weight 1086.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 9.0167(6) _cell_length_b 10.6153(8) _cell_length_c 14.1165(12) _cell_angle_alpha 80.777(3) _cell_angle_beta 72.910(5) _cell_angle_gamma 89.329(4) _cell_volume 1273.91(17) _cell_formula_units_Z 1 _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 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8318 _exptl_absorpt_correction_T_max 0.9441 _exptl_absorpt_process_details ? _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10504 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.1195 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 26.80 _reflns_number_total 5310 _reflns_number_gt 3214 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5310 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1118 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.39550(5) 0.43188(4) 0.57784(4) 0.02779(16) Uani 1 1 d . . . P1 P 0.22799(10) 0.31971(8) 0.70848(7) 0.0253(2) Uani 1 1 d . . . O1 O -0.0823(2) 0.0948(2) 0.85044(17) 0.0310(6) Uani 1 1 d . . . C1 C 0.0656(4) 0.4076(3) 0.7724(3) 0.0271(8) Uani 1 1 d . . . P2 P 0.03410(10) 0.05429(8) 0.76410(7) 0.0264(2) Uani 1 1 d . . . C2 C -0.0879(4) 0.3869(3) 0.7746(3) 0.0351(9) Uani 1 1 d . . . H2 H -0.1118 0.3251 0.7390 0.042 Uiso 1 1 calc R . . C3 C -0.2057(4) 0.4552(3) 0.8283(3) 0.0448(11) Uani 1 1 d . . . H3 H -0.3097 0.4406 0.8288 0.054 Uiso 1 1 calc R . . C4 C -0.1729(4) 0.5445(4) 0.8809(3) 0.0485(11) Uani 1 1 d . . . H4 H -0.2544 0.5897 0.9191 0.058 Uiso 1 1 calc R . . C5 C -0.0214(4) 0.5682(3) 0.8780(3) 0.0411(10) Uani 1 1 d . . . H5 H 0.0017 0.6306 0.9133 0.049 Uiso 1 1 calc R . . C6 C 0.0959(4) 0.5016(3) 0.8240(3) 0.0339(9) Uani 1 1 d . . . H6 H 0.2000 0.5196 0.8215 0.041 Uiso 1 1 calc R . . C7 C 0.3061(4) 0.2487(3) 0.8102(3) 0.0241(8) Uani 1 1 d . . . C8 C 0.4612(4) 0.2170(3) 0.7880(3) 0.0351(9) Uani 1 1 d . . . H8 H 0.5259 0.2312 0.7204 0.042 Uiso 1 1 calc R . . C9 C 0.5215(4) 0.1642(3) 0.8654(3) 0.0423(10) Uani 1 1 d . . . H9 H 0.6272 0.1418 0.8506 0.051 Uiso 1 1 calc R . . C10 C 0.4285(4) 0.1450(3) 0.9622(3) 0.0372(10) Uani 1 1 d . . . H10 H 0.4706 0.1105 1.0147 0.045 Uiso 1 1 calc R . . C11 C 0.2739(4) 0.1748(3) 0.9852(3) 0.0356(9) Uani 1 1 d . . . H11 H 0.2097 0.1599 1.0530 0.043 Uiso 1 1 calc R . . C12 C 0.2134(4) 0.2267(3) 0.9085(3) 0.0301(8) Uani 1 1 d . . . H12 H 0.1070 0.2473 0.9239 0.036 Uiso 1 1 calc R . . C13 C 0.1759(4) -0.0494(3) 0.7985(3) 0.0268(8) Uani 1 1 d . . . C14 C 0.3019(4) -0.0908(3) 0.7279(3) 0.0392(10) Uani 1 1 d . . . H14 H 0.3205 -0.0589 0.6584 0.047 Uiso 1 1 calc R . . C15 C 0.3998(4) -0.1783(4) 0.7590(3) 0.0460(11) Uani 1 1 d . . . H15 H 0.4858 -0.2063 0.7107 0.055 Uiso 1 1 calc R . . C16 C 0.3736(4) -0.2250(4) 0.8594(3) 0.0439(11) Uani 1 1 d . . . H16 H 0.4404 -0.2862 0.8799 0.053 Uiso 1 1 calc R . . C17 C 0.2507(4) -0.1835(3) 0.9304(3) 0.0410(10) Uani 1 1 d . . . H17 H 0.2334 -0.2149 0.9998 0.049 Uiso 1 1 calc R . . C18 C 0.1527(4) -0.0954(3) 0.8995(3) 0.0299(8) Uani 1 1 d . . . H18 H 0.0685 -0.0662 0.9483 0.036 Uiso 1 1 calc R . . C19 C -0.0507(4) -0.0325(3) 0.6906(3) 0.0305(9) Uani 1 1 d . . . C20 C -0.0313(4) -0.1620(3) 0.6903(3) 0.0445(11) Uani 1 1 d . . . H20 H 0.0351 -0.2059 0.7247 0.053 Uiso 1 1 calc R . . C21 C -0.1080(5) -0.2283(4) 0.6403(3) 0.0520(12) Uani 1 1 d . . . H21 H -0.0944 -0.3173 0.6411 0.062 Uiso 1 1 calc R . . C22 C -0.2018(4) -0.1665(4) 0.5905(3) 0.0476(11) Uani 1 1 d . . . H22 H -0.2538 -0.2125 0.5565 0.057 Uiso 1 1 calc R . . C23 C -0.2227(4) -0.0383(4) 0.5888(3) 0.0533(12) Uani 1 1 d . . . H23 H -0.2885 0.0042 0.5533 0.064 Uiso 1 1 calc R . . C24 C -0.1472(4) 0.0305(4) 0.6392(3) 0.0439(11) Uani 1 1 d . . . H24 H -0.1619 0.1194 0.6383 0.053 Uiso 1 1 calc R . . C25 C 0.1431(4) 0.1863(3) 0.6708(3) 0.0283(8) Uani 1 1 d . . . H25B H 0.0732 0.2236 0.6320 0.034 Uiso 1 1 calc R . . H25A H 0.2290 0.1487 0.6235 0.034 Uiso 1 1 calc R . . O101 O 0.1580(3) 0.5641(3) 0.4988(2) 0.0656(9) Uani 1 1 d . . . C101 C 0.2511(4) 0.5116(4) 0.5296(3) 0.0395(10) Uani 1 1 d . . . O102 O 0.5421(3) 0.5532(2) 0.7017(2) 0.0495(8) Uani 1 1 d . . . C102 C 0.4832(4) 0.5081(3) 0.6524(3) 0.0344(9) Uani 1 1 d . . . O103 O 0.5401(3) 0.2065(3) 0.5013(2) 0.0477(7) Uani 1 1 d . . . C103 C 0.4844(4) 0.2973(4) 0.5295(3) 0.0340(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0289(3) 0.0245(3) 0.0271(3) 0.0011(2) -0.0065(2) -0.00569(19) P1 0.0294(5) 0.0204(5) 0.0245(6) -0.0007(4) -0.0072(4) -0.0043(4) O1 0.0308(13) 0.0306(14) 0.0268(15) -0.0018(11) -0.0025(12) 0.0008(10) C1 0.0345(19) 0.0220(19) 0.021(2) 0.0028(16) -0.0059(17) -0.0032(15) P2 0.0290(5) 0.0220(5) 0.0248(6) -0.0010(4) -0.0039(4) -0.0046(4) C2 0.036(2) 0.029(2) 0.042(3) -0.0045(18) -0.015(2) -0.0009(16) C3 0.034(2) 0.034(2) 0.068(3) -0.008(2) -0.019(2) 0.0111(18) C4 0.046(3) 0.038(2) 0.054(3) -0.008(2) -0.004(2) 0.0142(19) C5 0.051(3) 0.035(2) 0.041(3) -0.016(2) -0.014(2) 0.0070(19) C6 0.033(2) 0.031(2) 0.039(3) -0.0079(19) -0.0111(19) 0.0027(16) C7 0.0274(19) 0.0149(18) 0.031(2) -0.0041(16) -0.0101(18) 0.0039(14) C8 0.039(2) 0.034(2) 0.029(2) -0.0012(18) -0.0067(19) -0.0003(17) C9 0.039(2) 0.043(2) 0.046(3) -0.003(2) -0.017(2) 0.0044(18) C10 0.047(2) 0.028(2) 0.041(3) 0.0013(19) -0.023(2) 0.0011(17) C11 0.048(2) 0.030(2) 0.029(2) -0.0025(17) -0.013(2) -0.0048(17) C12 0.031(2) 0.031(2) 0.026(2) -0.0036(17) -0.0053(18) -0.0033(15) C13 0.0302(19) 0.0219(19) 0.026(2) -0.0054(16) -0.0046(18) -0.0066(15) C14 0.040(2) 0.036(2) 0.034(2) -0.0037(19) 0.001(2) 0.0021(18) C15 0.037(2) 0.042(3) 0.054(3) -0.015(2) -0.001(2) 0.0061(19) C16 0.042(2) 0.037(2) 0.060(3) -0.015(2) -0.024(2) 0.0139(18) C17 0.048(2) 0.039(2) 0.039(3) -0.004(2) -0.018(2) 0.0014(19) C18 0.0295(19) 0.030(2) 0.031(2) -0.0109(17) -0.0069(18) 0.0030(15) C19 0.0285(19) 0.036(2) 0.022(2) 0.0007(17) -0.0034(17) -0.0114(16) C20 0.062(3) 0.027(2) 0.051(3) 0.000(2) -0.030(2) -0.0101(18) C21 0.071(3) 0.036(2) 0.053(3) -0.007(2) -0.024(3) -0.015(2) C22 0.044(2) 0.059(3) 0.038(3) -0.011(2) -0.007(2) -0.020(2) C23 0.041(2) 0.064(3) 0.059(3) -0.008(3) -0.023(2) -0.001(2) C24 0.041(2) 0.035(2) 0.061(3) -0.007(2) -0.024(2) 0.0010(18) C25 0.0334(19) 0.0237(19) 0.027(2) -0.0035(16) -0.0080(17) -0.0052(15) O101 0.0415(17) 0.080(2) 0.070(2) 0.0148(18) -0.0229(17) 0.0026(16) C101 0.035(2) 0.043(2) 0.034(2) 0.0048(19) -0.006(2) -0.0110(18) O102 0.0584(18) 0.0450(17) 0.052(2) -0.0085(15) -0.0260(16) -0.0098(14) C102 0.039(2) 0.023(2) 0.035(2) 0.0041(18) -0.0061(19) -0.0058(16) O103 0.0568(18) 0.0352(17) 0.0447(19) -0.0089(15) -0.0039(15) 0.0021(14) C103 0.034(2) 0.036(2) 0.029(2) 0.0006(19) -0.0063(18) -0.0073(18) _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 Co1 C103 1.765(4) . ? Co1 C102 1.778(4) . ? Co1 C101 1.785(4) . ? Co1 P1 2.1912(10) . ? Co1 Co1 2.6615(9) 2_666 ? P1 C1 1.814(4) . ? P1 C7 1.833(3) . ? P1 C25 1.839(3) . ? O1 P2 1.476(2) . ? C1 C2 1.394(4) . ? C1 C6 1.398(4) . ? P2 C13 1.801(3) . ? P2 C19 1.816(3) . ? P2 C25 1.829(3) . ? C2 C3 1.383(5) . ? C3 C4 1.378(5) . ? C4 C5 1.379(5) . ? C5 C6 1.372(5) . ? C7 C12 1.378(5) . ? C7 C8 1.390(4) . ? C8 C9 1.397(4) . ? C9 C10 1.360(5) . ? C10 C11 1.380(5) . ? C11 C12 1.387(4) . ? C13 C18 1.385(5) . ? C13 C14 1.393(5) . ? C14 C15 1.384(5) . ? C15 C16 1.375(5) . ? C16 C17 1.380(5) . ? C17 C18 1.386(4) . ? C19 C20 1.384(5) . ? C19 C24 1.390(4) . ? C20 C21 1.389(5) . ? C21 C22 1.352(5) . ? C22 C23 1.369(5) . ? C23 C24 1.402(5) . ? O101 C101 1.153(4) . ? O102 C102 1.151(4) . ? O103 C103 1.154(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 C103 Co1 C102 118.25(15) . . ? C103 Co1 C101 120.43(16) . . ? C102 Co1 C101 119.69(17) . . ? C103 Co1 P1 94.58(12) . . ? C102 Co1 P1 93.57(11) . . ? C101 Co1 P1 94.64(12) . . ? C103 Co1 Co1 85.42(12) . 2_666 ? C102 Co1 Co1 85.04(11) . 2_666 ? C101 Co1 Co1 86.73(12) . 2_666 ? P1 Co1 Co1 178.40(3) . 2_666 ? C1 P1 C7 102.94(15) . . ? C1 P1 C25 106.07(15) . . ? C7 P1 C25 106.12(14) . . ? C1 P1 Co1 114.97(11) . . ? C7 P1 Co1 115.54(11) . . ? C25 P1 Co1 110.34(12) . . ? C2 C1 C6 117.7(3) . . ? C2 C1 P1 124.4(3) . . ? C6 C1 P1 117.9(2) . . ? O1 P2 C13 113.89(15) . . ? O1 P2 C19 113.20(14) . . ? C13 P2 C19 105.24(16) . . ? O1 P2 C25 114.18(15) . . ? C13 P2 C25 106.41(15) . . ? C19 P2 C25 102.89(15) . . ? C3 C2 C1 120.7(3) . . ? C4 C3 C2 120.3(3) . . ? C3 C4 C5 119.8(4) . . ? C6 C5 C4 120.0(4) . . ? C5 C6 C1 121.4(3) . . ? C12 C7 C8 119.5(3) . . ? C12 C7 P1 120.9(2) . . ? C8 C7 P1 119.6(3) . . ? C7 C8 C9 119.7(4) . . ? C10 C9 C8 119.9(3) . . ? C9 C10 C11 121.1(3) . . ? C10 C11 C12 119.3(4) . . ? C7 C12 C11 120.6(3) . . ? C18 C13 C14 119.0(3) . . ? C18 C13 P2 118.1(3) . . ? C14 C13 P2 122.8(3) . . ? C15 C14 C13 120.0(4) . . ? C16 C15 C14 120.4(4) . . ? C15 C16 C17 120.4(4) . . ? C16 C17 C18 119.4(4) . . ? C13 C18 C17 120.9(4) . . ? C20 C19 C24 118.9(3) . . ? C20 C19 P2 121.8(2) . . ? C24 C19 P2 119.1(3) . . ? C19 C20 C21 120.6(3) . . ? C22 C21 C20 120.2(4) . . ? C21 C22 C23 120.6(3) . . ? C22 C23 C24 120.2(3) . . ? C19 C24 C23 119.5(4) . . ? P2 C25 P1 121.20(18) . . ? O101 C101 Co1 179.3(4) . . ? O102 C102 Co1 177.5(3) . . ? O103 C103 Co1 177.5(3) . . ? 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 C103 Co1 P1 C1 -164.29(15) . . . . ? C102 Co1 P1 C1 76.98(16) . . . . ? C101 Co1 P1 C1 -43.21(17) . . . . ? Co1 Co1 P1 C1 106.0(15) 2_666 . . . ? C103 Co1 P1 C7 75.95(16) . . . . ? C102 Co1 P1 C7 -42.78(16) . . . . ? C101 Co1 P1 C7 -162.97(17) . . . . ? Co1 Co1 P1 C7 -13.8(15) 2_666 . . . ? C103 Co1 P1 C25 -44.40(16) . . . . ? C102 Co1 P1 C25 -163.13(16) . . . . ? C101 Co1 P1 C25 76.67(17) . . . . ? Co1 Co1 P1 C25 -134.1(15) 2_666 . . . ? C7 P1 C1 C2 -121.1(3) . . . . ? C25 P1 C1 C2 -9.8(3) . . . . ? Co1 P1 C1 C2 112.4(3) . . . . ? C7 P1 C1 C6 58.1(3) . . . . ? C25 P1 C1 C6 169.4(3) . . . . ? Co1 P1 C1 C6 -68.4(3) . . . . ? C6 C1 C2 C3 -1.5(5) . . . . ? P1 C1 C2 C3 177.7(3) . . . . ? C1 C2 C3 C4 -0.4(6) . . . . ? C2 C3 C4 C5 1.7(6) . . . . ? C3 C4 C5 C6 -1.0(6) . . . . ? C4 C5 C6 C1 -1.0(6) . . . . ? C2 C1 C6 C5 2.3(5) . . . . ? P1 C1 C6 C5 -177.0(3) . . . . ? C1 P1 C7 C12 24.9(3) . . . . ? C25 P1 C7 C12 -86.4(3) . . . . ? Co1 P1 C7 C12 151.0(2) . . . . ? C1 P1 C7 C8 -154.9(3) . . . . ? C25 P1 C7 C8 93.9(3) . . . . ? Co1 P1 C7 C8 -28.7(3) . . . . ? C12 C7 C8 C9 -0.4(5) . . . . ? P1 C7 C8 C9 179.3(3) . . . . ? C7 C8 C9 C10 -0.5(5) . . . . ? C8 C9 C10 C11 1.1(6) . . . . ? C9 C10 C11 C12 -0.8(5) . . . . ? C8 C7 C12 C11 0.7(5) . . . . ? P1 C7 C12 C11 -179.0(2) . . . . ? C10 C11 C12 C7 -0.1(5) . . . . ? O1 P2 C13 C18 8.6(3) . . . . ? C19 P2 C13 C18 -115.9(3) . . . . ? C25 P2 C13 C18 135.3(2) . . . . ? O1 P2 C13 C14 -175.3(3) . . . . ? C19 P2 C13 C14 60.1(3) . . . . ? C25 P2 C13 C14 -48.6(3) . . . . ? C18 C13 C14 C15 1.2(5) . . . . ? P2 C13 C14 C15 -174.9(3) . . . . ? C13 C14 C15 C16 0.1(5) . . . . ? C14 C15 C16 C17 -1.1(6) . . . . ? C15 C16 C17 C18 0.8(5) . . . . ? C14 C13 C18 C17 -1.4(5) . . . . ? P2 C13 C18 C17 174.8(2) . . . . ? C16 C17 C18 C13 0.4(5) . . . . ? O1 P2 C19 C20 -109.9(3) . . . . ? C13 P2 C19 C20 15.1(4) . . . . ? C25 P2 C19 C20 126.4(3) . . . . ? O1 P2 C19 C24 65.2(3) . . . . ? C13 P2 C19 C24 -169.8(3) . . . . ? C25 P2 C19 C24 -58.5(3) . . . . ? C24 C19 C20 C21 -0.6(6) . . . . ? P2 C19 C20 C21 174.5(3) . . . . ? C19 C20 C21 C22 0.5(6) . . . . ? C20 C21 C22 C23 -0.1(6) . . . . ? C21 C22 C23 C24 -0.3(6) . . . . ? C20 C19 C24 C23 0.2(6) . . . . ? P2 C19 C24 C23 -175.1(3) . . . . ? C22 C23 C24 C19 0.3(6) . . . . ? O1 P2 C25 P1 47.2(2) . . . . ? C13 P2 C25 P1 -79.4(2) . . . . ? C19 P2 C25 P1 170.3(2) . . . . ? C1 P1 C25 P2 -69.0(2) . . . . ? C7 P1 C25 P2 40.0(2) . . . . ? Co1 P1 C25 P2 165.83(15) . . . . ? C103 Co1 C101 O101 -161(34) . . . . ? C102 Co1 C101 O101 4(34) . . . . ? P1 Co1 C101 O101 100(34) . . . . ? Co1 Co1 C101 O101 -79(34) 2_666 . . . ? C103 Co1 C102 O102 -28(8) . . . . ? C101 Co1 C102 O102 166(8) . . . . ? P1 Co1 C102 O102 69(8) . . . . ? Co1 Co1 C102 O102 -110(8) 2_666 . . . ? C102 Co1 C103 O103 80(7) . . . . ? C101 Co1 C103 O103 -114(7) . . . . ? P1 Co1 C103 O103 -16(7) . . . . ? Co1 Co1 C103 O103 162(7) 2_666 . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.80 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.569 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.090 #===END data_mm0140_compound_11 _database_code_depnum_ccdc_archive 'CCDC 228902' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H18 Co4 O14' _chemical_formula_weight 814.14 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' O O 0.0106 0.0060 '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' H H 0.0000 0.0000 '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 7.9541(6) _cell_length_b 8.0955(6) _cell_length_c 12.4315(12) _cell_angle_alpha 86.127(5) _cell_angle_beta 85.621(4) _cell_angle_gamma 77.462(5) _cell_volume 778.05(11) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 17128 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 406 _exptl_absorpt_coefficient_mu 2.163 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.929 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9736 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3544 _reflns_number_gt 2810 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; Collect (Nonius B.V. 1998) HKL Scalepack (Otwinowski & Minor 1997) ; _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+0.8839P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3544 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.88186(6) 0.30284(6) 0.70051(4) 0.02733(16) Uani 1 1 d . . . Co2 Co 0.73467(6) 0.06717(6) 0.68561(4) 0.02687(16) Uani 1 1 d . . . O103 O 0.7664(4) 0.5286(4) 0.5119(3) 0.0554(9) Uani 1 1 d . . . C103 C 0.8080(5) 0.4420(5) 0.5842(3) 0.0349(8) Uani 1 1 d . . . O102 O 1.2326(4) 0.1171(4) 0.6355(3) 0.0535(8) Uani 1 1 d . . . C102 C 1.0984(5) 0.1922(5) 0.6585(3) 0.0353(9) Uani 1 1 d . . . O101 O 0.9551(5) 0.5493(5) 0.8427(3) 0.0636(10) Uani 1 1 d . . . C101 C 0.9270(5) 0.4562(5) 0.7869(4) 0.0409(10) Uani 1 1 d . . . O203 O 0.5575(4) 0.1992(4) 0.4870(2) 0.0468(7) Uani 1 1 d . . . C203 C 0.6229(5) 0.1480(5) 0.5633(3) 0.0317(8) Uani 1 1 d . . . O202 O 1.0276(5) -0.1982(4) 0.6089(3) 0.0570(9) Uani 1 1 d . . . C202 C 0.9147(5) -0.0954(5) 0.6369(3) 0.0356(8) Uani 1 1 d . . . O201 O 0.5104(5) -0.1485(4) 0.7877(3) 0.0651(10) Uani 1 1 d . . . C201 C 0.5967(6) -0.0660(5) 0.7466(3) 0.0401(9) Uani 1 1 d . . . O1 O 0.5665(4) 0.4844(4) 0.8937(2) 0.0438(7) Uani 1 1 d . . . H7 H 0.5166 0.4813 0.9555 0.066 Uiso 1 1 calc R . . C7 C 0.4059(5) 0.4705(5) 0.7396(3) 0.0385(9) Uani 1 1 d . . . H7C H 0.4766 0.5371 0.6948 0.058 Uiso 1 1 calc R . . H7B H 0.3050 0.5468 0.7723 0.058 Uiso 1 1 calc R . . H7A H 0.3677 0.3925 0.6946 0.058 Uiso 1 1 calc R . . C6 C 0.5113(5) 0.3705(5) 0.8274(3) 0.0314(8) Uani 1 1 d . . . C1 C 0.6740(4) 0.2574(4) 0.7828(3) 0.0251(7) Uani 1 1 d . . . C2 C 0.8151(5) 0.1436(4) 0.8153(3) 0.0272(7) Uani 1 1 d . . . C3 C 0.9075(5) 0.0678(4) 0.9098(3) 0.0294(8) Uani 1 1 d . . . C4 C 0.8656(5) 0.1408(5) 1.0093(3) 0.0377(9) Uani 1 1 d . . . H4 H 0.7739 0.2374 1.0163 0.045 Uiso 1 1 calc R . . C5 C 0.9572(6) 0.0729(5) 1.0980(3) 0.0379(9) Uani 1 1 d . . . H5 H 0.9271 0.1235 1.1655 0.057 Uiso 1 1 calc R . . C8 C 0.4034(6) 0.2651(5) 0.8992(3) 0.0415(10) Uani 1 1 d . . . H8C H 0.4745 0.1992 0.9547 0.062 Uiso 1 1 calc R . . H8B H 0.3628 0.1880 0.8548 0.062 Uiso 1 1 calc R . . H8A H 0.3040 0.3409 0.9339 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0304(3) 0.0249(3) 0.0267(3) 0.00114(19) -0.0040(2) -0.0059(2) Co2 0.0338(3) 0.0234(3) 0.0236(3) -0.00209(18) -0.0060(2) -0.0048(2) O103 0.061(2) 0.0528(19) 0.0454(19) 0.0198(16) -0.0081(16) -0.0020(16) C103 0.036(2) 0.0318(19) 0.035(2) 0.0021(16) 0.0005(16) -0.0042(16) O102 0.0348(17) 0.0463(18) 0.077(2) -0.0132(16) 0.0034(15) -0.0025(14) C102 0.035(2) 0.034(2) 0.039(2) -0.0013(16) -0.0051(17) -0.0092(17) O101 0.065(2) 0.059(2) 0.076(3) -0.0334(19) 0.0043(19) -0.0302(18) C101 0.041(2) 0.034(2) 0.049(3) -0.0036(18) -0.0006(19) -0.0106(18) O203 0.0519(18) 0.0500(18) 0.0353(17) -0.0012(13) -0.0140(14) -0.0002(14) C203 0.0327(19) 0.0312(18) 0.030(2) -0.0060(15) -0.0036(16) -0.0019(15) O202 0.060(2) 0.0463(18) 0.057(2) -0.0161(15) -0.0004(16) 0.0094(16) C202 0.042(2) 0.032(2) 0.033(2) -0.0050(16) -0.0081(17) -0.0061(17) O201 0.085(3) 0.0456(19) 0.073(2) -0.0010(17) 0.008(2) -0.0364(19) C201 0.055(3) 0.0292(19) 0.038(2) -0.0039(16) -0.0049(19) -0.0120(19) O1 0.063(2) 0.0381(15) 0.0348(16) -0.0160(12) 0.0008(14) -0.0166(14) C7 0.037(2) 0.033(2) 0.041(2) -0.0032(17) -0.0048(17) 0.0029(16) C6 0.038(2) 0.0281(18) 0.0290(19) -0.0082(14) -0.0011(15) -0.0075(15) C1 0.0306(18) 0.0237(16) 0.0222(17) -0.0012(13) -0.0035(13) -0.0078(14) C2 0.0349(19) 0.0267(17) 0.0226(17) -0.0001(13) -0.0060(14) -0.0110(15) C3 0.041(2) 0.0244(17) 0.0249(18) 0.0025(13) -0.0101(15) -0.0100(15) C4 0.048(2) 0.032(2) 0.029(2) -0.0041(15) -0.0099(17) 0.0026(17) C5 0.053(2) 0.034(2) 0.0252(19) -0.0040(15) -0.0116(17) -0.0007(18) C8 0.048(2) 0.041(2) 0.037(2) -0.0035(17) 0.0034(18) -0.0130(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C101 1.804(4) . ? Co1 C102 1.816(4) . ? Co1 C103 1.824(4) . ? Co1 C1 1.968(3) . ? Co1 C2 1.978(3) . ? Co1 Co2 2.4689(6) . ? Co2 C201 1.794(4) . ? Co2 C202 1.819(4) . ? Co2 C203 1.830(4) . ? Co2 C2 1.963(3) . ? Co2 C1 1.976(3) . ? O103 C103 1.127(5) . ? O102 C102 1.134(5) . ? O101 C101 1.126(5) . ? O203 C203 1.128(5) . ? O202 C202 1.134(5) . ? O201 C201 1.130(5) . ? O1 C6 1.434(4) . ? C7 C6 1.509(5) . ? C6 C1 1.505(5) . ? C6 C8 1.536(5) . ? C1 C2 1.357(5) . ? C2 C3 1.461(5) . ? C3 C5 1.390(5) 2_757 ? C3 C4 1.393(5) . ? C4 C5 1.384(5) . ? C5 C3 1.390(5) 2_757 ? 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 C101 Co1 C102 101.29(18) . . ? C101 Co1 C103 99.85(19) . . ? C102 Co1 C103 104.85(18) . . ? C101 Co1 C1 97.69(17) . . ? C102 Co1 C1 139.52(16) . . ? C103 Co1 C1 106.65(16) . . ? C101 Co1 C2 97.75(17) . . ? C102 Co1 C2 101.51(16) . . ? C103 Co1 C2 144.55(16) . . ? C1 Co1 C2 40.24(14) . . ? C101 Co1 Co2 146.33(13) . . ? C102 Co1 Co2 97.64(12) . . ? C103 Co1 Co2 101.87(13) . . ? C1 Co1 Co2 51.39(10) . . ? C2 Co1 Co2 50.95(10) . . ? C201 Co2 C202 99.25(18) . . ? C201 Co2 C203 100.74(18) . . ? C202 Co2 C203 103.42(17) . . ? C201 Co2 C2 100.25(16) . . ? C202 Co2 C2 104.38(16) . . ? C203 Co2 C2 141.68(15) . . ? C201 Co2 C1 99.85(16) . . ? C202 Co2 C1 142.46(16) . . ? C203 Co2 C1 104.35(15) . . ? C2 Co2 C1 40.30(14) . . ? C201 Co2 Co1 148.92(13) . . ? C202 Co2 Co1 100.46(12) . . ? C203 Co2 Co1 97.77(12) . . ? C2 Co2 Co1 51.49(10) . . ? C1 Co2 Co1 51.09(10) . . ? O103 C103 Co1 178.3(4) . . ? O102 C102 Co1 176.8(4) . . ? O101 C101 Co1 178.4(4) . . ? O203 C203 Co2 178.3(3) . . ? O202 C202 Co2 178.4(4) . . ? O201 C201 Co2 178.2(4) . . ? O1 C6 C1 105.7(3) . . ? O1 C6 C7 109.6(3) . . ? C1 C6 C7 112.3(3) . . ? O1 C6 C8 108.5(3) . . ? C1 C6 C8 110.0(3) . . ? C7 C6 C8 110.6(3) . . ? C2 C1 C6 141.2(3) . . ? C2 C1 Co1 70.3(2) . . ? C6 C1 Co1 133.1(2) . . ? C2 C1 Co2 69.3(2) . . ? C6 C1 Co2 136.8(3) . . ? Co1 C1 Co2 77.52(13) . . ? C1 C2 C3 143.9(3) . . ? C1 C2 Co2 70.3(2) . . ? C3 C2 Co2 137.9(3) . . ? C1 C2 Co1 69.5(2) . . ? C3 C2 Co1 128.8(2) . . ? Co2 C2 Co1 77.57(13) . . ? C5 C3 C4 118.6(3) 2_757 . ? C5 C3 C2 121.3(3) 2_757 . ? C4 C3 C2 120.1(3) . . ? C5 C4 C3 120.1(4) . . ? C4 C5 C3 121.3(4) . 2_757 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.938 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.111 #===END