Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'B. Nicholson' 'Cameron Evans' 'Gwion J. Harfoot' 'K. M. MacKay' 'C. John McAdam' 'J. Scott McIndoe' 'Brian H. Robinson' 'Martin L. Van Tiel' _publ_contact_author_name 'Prof B Nicholson' _publ_contact_author_address ; Department of Chemistry University of Waikato Private Bag 3105 Hamilton NEW ZEALAND ; _publ_contact_author_email 'B.NICHOLSON@WAIKATO.AC.NZ' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The preparation and characterisation of monomeric and linked metal carbonyl clusters containing the closo-Si2Co4 pseudo-octahedral core ; data_gjhax _database_code_CSD 193182 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H14 Co8 Si4 O22, 1.5(C H2 Cl2)' _chemical_formula_sum 'C41.50 H17 Cl3 Co8 O22 Si4' _chemical_formula_weight 1557.70 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' 'Si' 'Si' 0.0817 0.0704 '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 monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.323(4) _cell_length_b 18.192(7) _cell_length_c 16.890(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.340(5) _cell_angle_gamma 90.00 _cell_volume 2787.1(19) _cell_formula_units_Z 2 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'thin plates' _exptl_crystal_colour 'red-black' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1530 _exptl_absorpt_coefficient_mu 2.623 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34955 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.1092 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.37 _reflns_number_total 11041 _reflns_number_gt 6524 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0420P)^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 0.05(2) _refine_ls_number_reflns 11041 _refine_ls_number_parameters 716 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _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 0.48782(14) 0.47553(7) 0.63531(7) 0.0281(3) Uani 1 1 d . . . Co2 Co 0.58643(13) 0.34982(6) 0.70172(7) 0.0277(3) Uani 1 1 d . . . Co3 Co 0.32365(14) 0.28683(7) 0.63338(7) 0.0307(3) Uani 1 1 d . . . Co4 Co 0.23503(13) 0.42003(7) 0.56867(7) 0.0302(3) Uani 1 1 d . . . Co5 Co 0.00764(14) 0.40626(7) 1.10129(7) 0.0324(3) Uani 1 1 d . . . Co6 Co 0.25836(13) 0.46455(7) 1.16704(7) 0.0308(3) Uani 1 1 d . . . Co7 Co 0.16571(13) 0.59680(6) 1.10532(7) 0.0277(3) Uani 1 1 d . . . Co8 Co -0.09678(13) 0.53205(7) 1.03643(7) 0.0287(3) Uani 1 1 d . . . Si1 Si 0.4566(3) 0.36401(14) 0.56737(15) 0.0254(6) Uani 1 1 d . . . Si2 Si 0.3571(3) 0.39845(14) 0.70278(15) 0.0247(6) Uani 1 1 d . . . Si3 Si 0.1340(3) 0.48680(14) 1.03378(15) 0.0264(6) Uani 1 1 d . . . Si4 Si 0.0340(3) 0.51807(14) 1.16950(15) 0.0260(6) Uani 1 1 d . . . C1 C 0.5943(11) 0.5099(6) 0.5679(6) 0.044(3) Uani 1 1 d . . . C2 C 0.5024(10) 0.5495(6) 0.7080(6) 0.037(3) Uani 1 1 d . . . C3 C 0.6027(10) 0.3139(6) 0.8007(6) 0.036(3) Uani 1 1 d . . . C4 C 0.6938(11) 0.4314(6) 0.7243(6) 0.038(3) Uani 1 1 d . . . C5 C 0.7194(11) 0.2975(6) 0.6655(6) 0.045(3) Uani 1 1 d . . . C6 C 0.1530(13) 0.2788(6) 0.5638(7) 0.051(3) Uani 1 1 d . . . C7 C 0.2769(10) 0.2479(5) 0.7233(6) 0.033(2) Uani 1 1 d . . . C8 C 0.4272(12) 0.2110(6) 0.6029(6) 0.040(3) Uani 1 1 d . . . C9 C 0.1659(10) 0.4075(6) 0.4554(7) 0.036(2) Uani 1 1 d . . . C10 C 0.0666(11) 0.4394(6) 0.5986(6) 0.043(3) Uani 1 1 d . . . C11 C 0.3010(10) 0.5197(6) 0.5671(6) 0.045(3) Uani 1 1 d . . . C12 C 0.0027(11) 0.3319(5) 1.0273(7) 0.042(3) Uani 1 1 d . . . C13 C -0.1038(11) 0.3677(5) 1.1678(6) 0.037(2) Uani 1 1 d . . . C14 C 0.1960(12) 0.3674(6) 1.1711(6) 0.043(3) Uani 1 1 d . . . C15 C 0.4265(12) 0.4409(5) 1.1359(6) 0.038(3) Uani 1 1 d . . . C16 C 0.3267(10) 0.4749(6) 1.2754(6) 0.036(2) Uani 1 1 d . . . C17 C 0.0864(10) 0.6723(6) 1.1505(6) 0.037(3) Uani 1 1 d . . . C18 C 0.3459(11) 0.6018(6) 1.1686(6) 0.039(2) Uani 1 1 d . . . C19 C 0.1888(11) 0.6362(5) 1.0126(6) 0.037(2) Uani 1 1 d . . . C20 C -0.1168(11) 0.5744(6) 0.9365(7) 0.040(3) Uani 1 1 d . . . C21 C -0.2337(11) 0.5837(6) 1.0743(5) 0.033(2) Uani 1 1 d . . . C22 C -0.2016(11) 0.4474(6) 1.0092(6) 0.043(3) Uani 1 1 d . . . C23 C 0.5225(10) 0.3341(5) 0.4759(5) 0.028(2) Uani 1 1 d . . . C24 C 0.6554(11) 0.3575(6) 0.4600(6) 0.047(3) Uani 1 1 d . . . H24 H 0.7158 0.3900 0.4975 0.056 Uiso 1 1 calc R . . C25 C 0.7055(13) 0.3347(7) 0.3893(6) 0.063(4) Uani 1 1 d . . . H25 H 0.7971 0.3508 0.3800 0.075 Uiso 1 1 calc R . . C26 C 0.6127(15) 0.2876(9) 0.3352(7) 0.069(4) Uani 1 1 d . . . H26 H 0.6435 0.2702 0.2887 0.083 Uiso 1 1 calc R . . C27 C 0.4820(11) 0.2662(7) 0.3469(6) 0.050(3) Uani 1 1 d . . . H27 H 0.4200 0.2353 0.3082 0.060 Uiso 1 1 calc R . . C28 C 0.4368(11) 0.2894(6) 0.4160(6) 0.039(3) Uani 1 1 d . . . H28 H 0.3429 0.2740 0.4226 0.047 Uiso 1 1 calc R . . C29 C 0.2940(10) 0.4239(5) 0.7956(5) 0.027(2) Uani 1 1 d . . . C30 C 0.3823(9) 0.4638(5) 0.8579(5) 0.027(2) Uani 1 1 d . . . H30 H 0.4777 0.4782 0.8530 0.032 Uiso 1 1 calc R . . C31 C 0.3360(10) 0.4834(5) 0.9276(5) 0.031(2) Uani 1 1 d . . . H31 H 0.4007 0.5103 0.9692 0.037 Uiso 1 1 calc R . . C32 C 0.1953(9) 0.4640(5) 0.9376(5) 0.025(2) Uani 1 1 d . . . C33 C 0.1030(10) 0.4254(5) 0.8732(5) 0.031(2) Uani 1 1 d . . . H33 H 0.0057 0.4132 0.8769 0.037 Uiso 1 1 calc R . . C34 C 0.1512(9) 0.4044(5) 0.8037(5) 0.027(2) Uani 1 1 d . . . H34 H 0.0878 0.3770 0.7619 0.032 Uiso 1 1 calc R . . C35 C -0.0349(10) 0.5419(5) 1.2632(5) 0.031(2) Uani 1 1 d . . . C36 C -0.1682(9) 0.5187(5) 1.2742(6) 0.030(2) Uani 1 1 d . . . H36 H -0.2311 0.4896 1.2339 0.036 Uiso 1 1 calc R . . C37 C -0.2099(10) 0.5381(5) 1.3440(6) 0.037(2) Uani 1 1 d . . . H37 H -0.3017 0.5211 1.3523 0.044 Uiso 1 1 calc R . . C38 C -0.1211(11) 0.5821(6) 1.4033(6) 0.039(3) Uani 1 1 d . . . H38 H -0.1527 0.5951 1.4510 0.046 Uiso 1 1 calc R . . C39 C 0.0129(10) 0.6068(5) 1.3921(5) 0.035(2) Uani 1 1 d . . . H39 H 0.0737 0.6365 1.4327 0.042 Uiso 1 1 calc R . . C40 C 0.0595(9) 0.5887(5) 1.3225(5) 0.028(2) Uani 1 1 d . . . H40 H 0.1505 0.6065 1.3139 0.033 Uiso 1 1 calc R . . O1 O 0.6538(9) 0.5366(5) 0.5222(5) 0.069(3) Uani 1 1 d . . . O2 O 0.5146(9) 0.6029(5) 0.7501(5) 0.062(2) Uani 1 1 d . . . O3 O 0.6156(9) 0.2853(5) 0.8630(4) 0.052(2) Uani 1 1 d . . . O4 O 0.7915(7) 0.4670(4) 0.7553(4) 0.052(2) Uani 1 1 d . . . O5 O 0.8030(9) 0.2611(5) 0.6425(4) 0.075(3) Uani 1 1 d . . . O6 O 0.0417(10) 0.2646(5) 0.5196(6) 0.078(3) Uani 1 1 d . . . O7 O 0.2517(8) 0.2212(4) 0.7785(4) 0.056(2) Uani 1 1 d . . . O8 O 0.4931(9) 0.1626(4) 0.5876(4) 0.058(2) Uani 1 1 d . . . O9 O 0.1167(8) 0.3998(4) 0.3895(4) 0.047(2) Uani 1 1 d . . . O10 O -0.0433(8) 0.4531(5) 0.6123(5) 0.067(3) Uani 1 1 d . . . O11 O 0.2678(9) 0.5774(5) 0.5456(5) 0.080(3) Uani 1 1 d . . . O12 O -0.0072(9) 0.2852(5) 0.9851(5) 0.066(2) Uani 1 1 d . . . O13 O -0.1671(9) 0.3389(4) 1.2085(5) 0.069(2) Uani 1 1 d . . . O14 O 0.2328(9) 0.3081(5) 1.2001(5) 0.070(2) Uani 1 1 d . . . O15 O 0.5393(8) 0.4275(5) 1.1218(4) 0.066(3) Uani 1 1 d . . . O16 O 0.3796(7) 0.4822(4) 1.3452(4) 0.048(2) Uani 1 1 d . . . O17 O 0.0412(7) 0.7209(4) 1.1792(4) 0.0431(18) Uani 1 1 d . . . O18 O 0.4604(7) 0.6174(4) 1.2100(4) 0.051(2) Uani 1 1 d . . . O19 O 0.1954(9) 0.6654(4) 0.9528(5) 0.063(2) Uani 1 1 d . . . O20 O -0.1340(9) 0.6027(5) 0.8742(5) 0.065(2) Uani 1 1 d . . . O21 O -0.3305(7) 0.6108(4) 1.0933(4) 0.052(2) Uani 1 1 d . . . O22 O -0.2946(7) 0.4099(5) 0.9764(5) 0.062(2) Uani 1 1 d . . . Cl91 Cl 0.3374(4) 0.2923(2) 0.9806(2) 0.0823(11) Uani 1 1 d . . . Cl92 Cl 0.4898(4) 0.1975(2) 1.1085(2) 0.0945(13) Uani 1 1 d . . . C91 C 0.4904(13) 0.2499(6) 1.0242(7) 0.069(3) Uani 1 1 d . . . H91A H 0.5687 0.2874 1.0397 0.083 Uiso 1 1 calc R . . H91B H 0.5185 0.2177 0.9830 0.083 Uiso 1 1 calc R . . Cl93 Cl 0.8578(5) 0.1073(3) 0.2528(3) 0.0492(15) Uani 0.50 1 d P . . Cl94 Cl 0.1237(9) 0.1569(5) 0.3576(5) 0.138(4) Uani 0.50 1 d P . . C92 C 1.035(3) 0.1660(19) 0.294(2) 0.123(12) Uiso 0.50 1 d P . . H92A H 1.0916 0.1641 0.2512 0.147 Uiso 0.50 1 calc PR . . H92B H 1.0003 0.2174 0.2951 0.147 Uiso 0.50 1 calc PR . . 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 0.0294(8) 0.0317(8) 0.0244(8) 0.0000(6) 0.0089(6) -0.0018(6) Co2 0.0262(7) 0.0355(8) 0.0225(7) 0.0031(6) 0.0081(6) 0.0056(6) Co3 0.0346(8) 0.0314(8) 0.0292(8) 0.0010(6) 0.0138(6) -0.0017(6) Co4 0.0254(7) 0.0407(9) 0.0239(7) 0.0007(6) 0.0042(6) 0.0023(6) Co5 0.0378(8) 0.0334(8) 0.0300(8) -0.0031(6) 0.0160(6) -0.0051(7) Co6 0.0249(7) 0.0428(8) 0.0250(7) -0.0004(6) 0.0062(5) 0.0048(6) Co7 0.0296(7) 0.0316(8) 0.0246(7) -0.0023(6) 0.0117(6) -0.0033(6) Co8 0.0250(7) 0.0399(8) 0.0221(7) -0.0023(6) 0.0075(5) 0.0031(6) Si1 0.0276(14) 0.0296(15) 0.0210(14) 0.0001(12) 0.0095(11) 0.0005(12) Si2 0.0228(13) 0.0298(16) 0.0222(14) 0.0012(12) 0.0067(11) 0.0055(11) Si3 0.0239(14) 0.0373(17) 0.0205(14) -0.0043(12) 0.0102(11) 0.0000(12) Si4 0.0244(14) 0.0376(16) 0.0178(14) -0.0031(12) 0.0086(11) -0.0040(12) C1 0.035(6) 0.054(7) 0.040(7) 0.002(5) 0.004(5) 0.006(5) C2 0.025(5) 0.048(7) 0.036(6) 0.005(5) 0.002(5) -0.004(5) C3 0.042(6) 0.044(7) 0.022(6) 0.001(5) 0.011(5) -0.003(5) C4 0.034(6) 0.045(7) 0.036(6) 0.001(5) 0.012(5) 0.003(5) C5 0.046(7) 0.054(8) 0.033(6) 0.013(5) 0.004(5) 0.023(6) C6 0.052(8) 0.044(7) 0.053(8) 0.006(6) 0.003(6) -0.004(6) C7 0.024(5) 0.050(7) 0.031(6) 0.007(5) 0.016(4) -0.001(5) C8 0.062(7) 0.026(6) 0.036(6) -0.009(5) 0.023(5) -0.021(5) C9 0.028(6) 0.035(6) 0.048(7) 0.005(6) 0.013(5) 0.000(5) C10 0.024(6) 0.066(8) 0.040(7) -0.002(5) 0.008(5) 0.002(5) C11 0.025(6) 0.052(8) 0.053(8) -0.008(6) -0.003(5) 0.005(5) C12 0.043(6) 0.021(6) 0.067(8) 0.003(6) 0.026(6) -0.008(5) C13 0.045(6) 0.026(6) 0.043(7) 0.003(5) 0.017(5) -0.002(5) C14 0.059(7) 0.040(7) 0.030(6) 0.000(5) 0.011(5) -0.005(6) C15 0.041(7) 0.043(7) 0.024(6) -0.009(5) -0.007(5) -0.002(5) C16 0.031(5) 0.041(6) 0.040(7) 0.014(6) 0.018(5) 0.014(5) C17 0.022(5) 0.062(8) 0.026(6) 0.016(5) 0.005(4) 0.000(5) C18 0.041(6) 0.035(6) 0.045(7) 0.004(5) 0.016(5) -0.004(5) C19 0.045(6) 0.022(6) 0.044(7) -0.011(5) 0.013(5) -0.007(4) C20 0.024(6) 0.047(7) 0.049(8) 0.002(6) 0.008(5) 0.009(5) C21 0.039(6) 0.044(7) 0.019(5) 0.001(5) 0.011(4) 0.002(5) C22 0.030(6) 0.051(7) 0.052(7) -0.013(6) 0.017(5) -0.009(5) C23 0.031(5) 0.037(6) 0.022(5) 0.003(4) 0.017(4) -0.008(4) C24 0.041(6) 0.066(8) 0.032(6) -0.014(6) 0.006(5) 0.002(6) C25 0.061(8) 0.101(11) 0.034(7) 0.001(7) 0.027(6) -0.003(7) C26 0.088(11) 0.104(12) 0.023(7) -0.001(7) 0.027(7) 0.015(9) C27 0.036(6) 0.083(9) 0.032(6) -0.005(6) 0.010(5) -0.004(6) C28 0.038(6) 0.047(6) 0.036(6) -0.011(5) 0.015(5) -0.009(5) C29 0.037(5) 0.031(6) 0.010(5) 0.003(4) -0.001(4) 0.009(5) C30 0.016(5) 0.031(6) 0.033(6) 0.005(5) 0.006(4) 0.003(4) C31 0.030(5) 0.040(6) 0.024(5) -0.012(5) 0.010(4) -0.002(5) C32 0.025(5) 0.026(5) 0.029(5) -0.004(4) 0.015(4) 0.000(4) C33 0.030(5) 0.039(6) 0.025(6) 0.001(5) 0.007(4) 0.004(5) C34 0.025(5) 0.036(6) 0.020(5) -0.004(4) 0.006(4) -0.007(4) C35 0.038(6) 0.034(6) 0.018(5) 0.000(4) 0.003(4) 0.012(5) C36 0.016(5) 0.039(6) 0.037(6) 0.004(5) 0.008(4) -0.003(4) C37 0.032(6) 0.040(6) 0.042(6) -0.008(5) 0.017(5) -0.004(5) C38 0.043(7) 0.039(7) 0.044(7) 0.003(5) 0.029(6) 0.014(5) C39 0.036(6) 0.038(6) 0.027(6) -0.019(5) -0.001(4) 0.018(5) C40 0.030(5) 0.035(6) 0.021(5) -0.002(5) 0.009(4) 0.008(4) O1 0.066(6) 0.077(6) 0.077(6) 0.032(5) 0.040(5) -0.003(5) O2 0.085(6) 0.051(6) 0.053(5) -0.016(4) 0.021(4) -0.005(5) O3 0.065(6) 0.061(5) 0.029(5) 0.007(4) 0.011(4) 0.013(5) O4 0.033(4) 0.052(5) 0.066(5) 0.008(4) 0.002(4) -0.006(4) O5 0.079(6) 0.106(7) 0.050(5) 0.012(5) 0.033(5) 0.056(5) O6 0.062(6) 0.071(7) 0.093(8) 0.025(5) -0.001(5) -0.022(5) O7 0.073(5) 0.062(5) 0.046(5) 0.008(4) 0.040(4) -0.002(4) O8 0.081(6) 0.033(4) 0.071(6) 0.005(4) 0.039(4) 0.007(4) O9 0.056(5) 0.060(6) 0.019(4) 0.000(4) -0.004(4) -0.004(4) O10 0.027(4) 0.116(8) 0.056(5) 0.003(5) 0.007(4) 0.021(5) O11 0.069(6) 0.042(6) 0.101(7) 0.023(5) -0.036(5) 0.007(4) O12 0.100(7) 0.038(5) 0.067(6) -0.030(5) 0.032(5) -0.027(5) O13 0.079(6) 0.062(6) 0.080(6) 0.014(5) 0.048(5) -0.015(5) O14 0.076(6) 0.048(6) 0.083(6) 0.012(5) 0.012(5) 0.012(5) O15 0.036(5) 0.107(7) 0.057(5) -0.029(5) 0.016(4) 0.015(5) O16 0.042(4) 0.075(6) 0.025(4) 0.006(4) 0.003(3) 0.010(4) O17 0.043(4) 0.048(5) 0.037(4) 0.001(4) 0.008(3) 0.014(4) O18 0.036(4) 0.055(5) 0.059(5) -0.004(4) 0.005(4) -0.010(4) O19 0.084(6) 0.058(5) 0.061(6) 0.004(4) 0.046(5) -0.005(4) O20 0.072(6) 0.077(6) 0.052(5) 0.020(5) 0.025(4) 0.012(5) O21 0.039(4) 0.065(5) 0.058(5) -0.001(4) 0.020(4) 0.025(4) O22 0.032(4) 0.065(6) 0.080(6) -0.008(5) -0.007(4) -0.010(4) Cl91 0.088(3) 0.083(2) 0.074(2) 0.0111(19) 0.0140(19) 0.043(2) Cl92 0.091(3) 0.131(3) 0.068(2) 0.048(2) 0.032(2) 0.007(2) C91 0.075(8) 0.057(8) 0.076(9) 0.025(6) 0.020(7) 0.017(6) Cl93 0.033(3) 0.081(4) 0.026(3) -0.011(3) -0.008(2) -0.027(3) Cl94 0.106(6) 0.151(8) 0.114(7) -0.009(6) -0.060(5) -0.085(6) _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 C1 1.788(11) . ? Co1 C2 1.806(11) . ? Co1 C11 2.020(10) . ? Co1 C4 2.293(10) . ? Co1 Si1 2.316(3) . ? Co1 Si2 2.322(3) . ? Co1 Co4 2.5721(19) . ? Co1 Co2 2.6187(19) . ? Co2 C3 1.768(10) . ? Co2 C5 1.780(11) . ? Co2 C4 1.782(11) . ? Co2 Si2 2.318(3) . ? Co2 Si1 2.327(3) . ? Co2 Co3 2.7097(19) . ? Co3 C6 1.752(12) . ? Co3 C7 1.817(10) . ? Co3 C8 1.825(11) . ? Co3 Si1 2.321(3) . ? Co3 Si2 2.329(3) . ? Co3 Co4 2.708(2) . ? Co4 C10 1.792(11) . ? Co4 C9 1.886(11) . ? Co4 C11 1.916(11) . ? Co4 Si1 2.308(3) . ? Co4 Si2 2.322(3) . ? Co5 C13 1.837(10) . ? Co5 C12 1.836(11) . ? Co5 C14 2.004(11) . ? Co5 C22 2.320(11) . ? Co5 Si4 2.323(3) . ? Co5 Si3 2.335(3) . ? Co5 Co6 2.574(2) . ? Co5 Co8 2.6254(19) . ? Co6 C16 1.804(10) . ? Co6 C15 1.816(11) . ? Co6 C14 1.867(10) . ? Co6 Si4 2.316(3) . ? Co6 Si3 2.317(3) . ? Co6 Co7 2.684(2) . ? Co7 C18 1.773(11) . ? Co7 C19 1.780(11) . ? Co7 C17 1.810(12) . ? Co7 Si4 2.313(3) . ? Co7 Si3 2.321(3) . ? Co7 Co8 2.7232(18) . ? Co8 C21 1.815(10) . ? Co8 C20 1.826(12) . ? Co8 C22 1.825(10) . ? Co8 Si4 2.310(3) . ? Co8 Si3 2.314(3) . ? Si1 C23 1.871(9) . ? Si1 Si2 2.732(3) . ? Si2 C29 1.856(9) . ? Si3 C32 1.889(8) . ? Si3 Si4 2.726(3) . ? Si4 C35 1.891(9) . ? C1 O1 1.155(11) . ? C2 O2 1.194(12) . ? C3 O3 1.155(11) . ? C4 O4 1.141(11) . ? C5 O5 1.156(11) . ? C6 O6 1.159(12) . ? C7 O7 1.124(10) . ? C8 O8 1.136(11) . ? C9 O9 1.111(11) . ? C10 O10 1.130(11) . ? C11 O11 1.130(12) . ? C12 O12 1.098(11) . ? C13 O13 1.132(10) . ? C14 O14 1.201(11) . ? C15 O15 1.157(11) . ? C16 O16 1.176(10) . ? C17 O17 1.136(11) . ? C18 O18 1.168(11) . ? C19 O19 1.156(11) . ? C20 O20 1.148(12) . ? C21 O21 1.138(10) . ? C22 O22 1.141(11) . ? C23 C24 1.394(12) . ? C23 C28 1.397(12) . ? C24 C25 1.440(13) . ? C25 C26 1.398(17) . ? C26 C27 1.336(15) . ? C27 C28 1.394(13) . ? C29 C30 1.382(12) . ? C29 C34 1.415(11) . ? C30 C31 1.390(11) . ? C31 C32 1.406(11) . ? C32 C33 1.409(12) . ? C33 C34 1.403(11) . ? C35 C36 1.364(12) . ? C35 C40 1.448(12) . ? C36 C37 1.372(12) . ? C37 C38 1.395(14) . ? C38 C39 1.381(13) . ? C39 C40 1.383(11) . ? Cl91 C91 1.639(11) . ? Cl92 C91 1.715(11) . ? Cl93 C92 1.95(3) . ? Cl94 C92 1.21(3) 1_455 ? C92 Cl94 1.21(3) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Co1 C2 101.9(5) . . ? C1 Co1 C11 91.7(5) . . ? C2 Co1 C11 90.7(4) . . ? C1 Co1 C4 92.0(4) . . ? C2 Co1 C4 84.0(4) . . ? C11 Co1 C4 174.0(4) . . ? C1 Co1 Si1 90.9(4) . . ? C2 Co1 Si1 166.2(3) . . ? C11 Co1 Si1 94.1(3) . . ? C4 Co1 Si1 90.5(3) . . ? C1 Co1 Si2 162.8(4) . . ? C2 Co1 Si2 94.7(3) . . ? C11 Co1 Si2 92.2(3) . . ? C4 Co1 Si2 85.5(3) . . ? Si1 Co1 Si2 72.18(9) . . ? C1 Co1 Co4 116.5(3) . . ? C2 Co1 Co4 120.5(3) . . ? C11 Co1 Co4 47.5(3) . . ? C4 Co1 Co4 133.9(3) . . ? Si1 Co1 Co4 56.06(7) . . ? Si2 Co1 Co4 56.36(7) . . ? C1 Co1 Co2 112.7(3) . . ? C2 Co1 Co2 113.3(3) . . ? C11 Co1 Co2 139.7(3) . . ? C4 Co1 Co2 41.9(3) . . ? Si1 Co1 Co2 55.86(8) . . ? Si2 Co1 Co2 55.56(7) . . ? Co4 Co1 Co2 92.31(6) . . ? C3 Co2 C5 102.3(4) . . ? C3 Co2 C4 100.6(4) . . ? C5 Co2 C4 96.8(5) . . ? C3 Co2 Si2 90.7(3) . . ? C5 Co2 Si2 157.5(3) . . ? C4 Co2 Si2 98.9(3) . . ? C3 Co2 Si1 151.0(3) . . ? C5 Co2 Si1 88.3(3) . . ? C4 Co2 Si1 104.8(3) . . ? Si2 Co2 Si1 72.06(9) . . ? C3 Co2 Co1 132.3(3) . . ? C5 Co2 Co1 121.5(3) . . ? C4 Co2 Co1 59.2(3) . . ? Si2 Co2 Co1 55.71(7) . . ? Si1 Co2 Co1 55.47(7) . . ? C3 Co2 Co3 96.8(3) . . ? C5 Co2 Co3 105.1(4) . . ? C4 Co2 Co3 148.4(3) . . ? Si2 Co2 Co3 54.53(8) . . ? Si1 Co2 Co3 54.25(7) . . ? Co1 Co2 Co3 89.62(6) . . ? C6 Co3 C7 99.9(5) . . ? C6 Co3 C8 101.9(5) . . ? C7 Co3 C8 100.7(4) . . ? C6 Co3 Si1 103.4(4) . . ? C7 Co3 Si1 153.4(3) . . ? C8 Co3 Si1 86.9(3) . . ? C6 Co3 Si2 113.9(4) . . ? C7 Co3 Si2 87.1(3) . . ? C8 Co3 Si2 141.5(3) . . ? Si1 Co3 Si2 71.94(9) . . ? C6 Co3 Co4 70.0(4) . . ? C7 Co3 Co4 125.2(3) . . ? C8 Co3 Co4 134.0(3) . . ? Si1 Co3 Co4 53.97(7) . . ? Si2 Co3 Co4 54.26(7) . . ? C6 Co3 Co2 155.9(4) . . ? C7 Co3 Co2 100.2(3) . . ? C8 Co3 Co2 87.4(3) . . ? Si1 Co3 Co2 54.43(8) . . ? Si2 Co3 Co2 54.13(7) . . ? Co4 Co3 Co2 87.43(6) . . ? C10 Co4 C9 101.1(4) . . ? C10 Co4 C11 97.1(5) . . ? C9 Co4 C11 97.8(4) . . ? C10 Co4 Si1 159.0(4) . . ? C9 Co4 Si1 91.9(3) . . ? C11 Co4 Si1 97.3(3) . . ? C10 Co4 Si2 91.3(3) . . ? C9 Co4 Si2 160.9(3) . . ? C11 Co4 Si2 95.0(3) . . ? Si1 Co4 Si2 72.32(9) . . ? C10 Co4 Co1 125.0(3) . . ? C9 Co4 Co1 123.8(3) . . ? C11 Co4 Co1 51.0(3) . . ? Si1 Co4 Co1 56.35(8) . . ? Si2 Co4 Co1 56.37(7) . . ? C10 Co4 Co3 105.5(4) . . ? C9 Co4 Co3 107.6(3) . . ? C11 Co4 Co3 141.5(3) . . ? Si1 Co4 Co3 54.43(7) . . ? Si2 Co4 Co3 54.52(7) . . ? Co1 Co4 Co3 90.65(6) . . ? C13 Co5 C12 101.9(4) . . ? C13 Co5 C14 92.8(4) . . ? C12 Co5 C14 91.2(4) . . ? C13 Co5 C22 91.5(4) . . ? C12 Co5 C22 84.1(4) . . ? C14 Co5 C22 174.2(4) . . ? C13 Co5 Si4 92.4(3) . . ? C12 Co5 Si4 165.2(3) . . ? C14 Co5 Si4 92.2(3) . . ? C22 Co5 Si4 91.5(3) . . ? C13 Co5 Si3 163.5(3) . . ? C12 Co5 Si3 93.8(3) . . ? C14 Co5 Si3 92.1(3) . . ? C22 Co5 Si3 84.9(3) . . ? Si4 Co5 Si3 71.64(9) . . ? C13 Co5 Co6 118.6(3) . . ? C12 Co5 Co6 118.4(3) . . ? C14 Co5 Co6 46.1(3) . . ? C22 Co5 Co6 134.1(3) . . ? Si4 Co5 Co6 56.18(7) . . ? Si3 Co5 Co6 56.08(8) . . ? C13 Co5 Co8 112.4(3) . . ? C12 Co5 Co8 114.2(3) . . ? C14 Co5 Co8 138.0(3) . . ? C22 Co5 Co8 42.8(3) . . ? Si4 Co5 Co8 55.26(8) . . ? Si3 Co5 Co8 55.22(7) . . ? Co6 Co5 Co8 91.91(6) . . ? C16 Co6 C15 101.1(4) . . ? C16 Co6 C14 95.8(5) . . ? C15 Co6 C14 94.8(5) . . ? C16 Co6 Si4 92.7(3) . . ? C15 Co6 Si4 161.4(3) . . ? C14 Co6 Si4 96.2(3) . . ? C16 Co6 Si3 161.4(3) . . ? C15 Co6 Si3 91.8(3) . . ? C14 Co6 Si3 96.3(3) . . ? Si4 Co6 Si3 72.09(9) . . ? C16 Co6 Co5 123.6(3) . . ? C15 Co6 Co5 122.4(3) . . ? C14 Co6 Co5 50.7(3) . . ? Si4 Co6 Co5 56.42(8) . . ? Si3 Co6 Co5 56.75(7) . . ? C16 Co6 Co7 107.9(3) . . ? C15 Co6 Co7 108.7(3) . . ? C14 Co6 Co7 142.0(3) . . ? Si4 Co6 Co7 54.49(7) . . ? Si3 Co6 Co7 54.70(7) . . ? Co5 Co6 Co7 91.31(6) . . ? C18 Co7 C19 102.7(5) . . ? C18 Co7 C17 97.4(4) . . ? C19 Co7 C17 102.1(4) . . ? C18 Co7 Si4 106.3(3) . . ? C19 Co7 Si4 147.9(3) . . ? C17 Co7 Si4 87.7(3) . . ? C18 Co7 Si3 110.3(3) . . ? C19 Co7 Si3 85.2(3) . . ? C17 Co7 Si3 149.1(3) . . ? Si4 Co7 Si3 72.08(9) . . ? C18 Co7 Co6 68.7(3) . . ? C19 Co7 Co6 127.6(3) . . ? C17 Co7 Co6 130.0(3) . . ? Si4 Co7 Co6 54.61(8) . . ? Si3 Co7 Co6 54.57(8) . . ? C18 Co7 Co8 155.9(3) . . ? C19 Co7 Co8 94.4(3) . . ? C17 Co7 Co8 95.4(3) . . ? Si4 Co7 Co8 53.87(8) . . ? Si3 Co7 Co8 53.89(7) . . ? Co6 Co7 Co8 87.43(5) . . ? C21 Co8 C20 100.2(4) . . ? C21 Co8 C22 98.4(4) . . ? C20 Co8 C22 100.9(5) . . ? C21 Co8 Si4 88.3(3) . . ? C20 Co8 Si4 149.8(3) . . ? C22 Co8 Si4 106.5(3) . . ? C21 Co8 Si3 157.4(3) . . ? C20 Co8 Si3 91.7(3) . . ? C22 Co8 Si3 98.1(3) . . ? Si4 Co8 Si3 72.26(9) . . ? C21 Co8 Co5 121.8(3) . . ? C20 Co8 Co5 134.6(3) . . ? C22 Co8 Co5 59.7(3) . . ? Si4 Co8 Co5 55.70(8) . . ? Si3 Co8 Co5 56.01(7) . . ? C21 Co8 Co7 105.1(3) . . ? C20 Co8 Co7 95.9(3) . . ? C22 Co8 Co7 148.1(3) . . ? Si4 Co8 Co7 53.95(7) . . ? Si3 Co8 Co7 54.14(8) . . ? Co5 Co8 Co7 89.35(6) . . ? C23 Si1 Co4 127.0(3) . . ? C23 Si1 Co1 129.5(3) . . ? Co4 Si1 Co1 67.60(8) . . ? C23 Si1 Co3 122.3(3) . . ? Co4 Si1 Co3 71.60(9) . . ? Co1 Si1 Co3 108.17(11) . . ? C23 Si1 Co2 125.3(3) . . ? Co4 Si1 Co2 107.76(11) . . ? Co1 Si1 Co2 68.67(8) . . ? Co3 Si1 Co2 71.32(9) . . ? C23 Si1 Si2 176.3(3) . . ? Co4 Si1 Si2 54.07(8) . . ? Co1 Si1 Si2 54.01(8) . . ? Co3 Si1 Si2 54.16(8) . . ? Co2 Si1 Si2 53.82(8) . . ? C29 Si2 Co2 125.1(3) . . ? C29 Si2 Co4 127.0(3) . . ? Co2 Si2 Co4 107.60(11) . . ? C29 Si2 Co1 124.6(3) . . ? Co2 Si2 Co1 68.73(8) . . ? Co4 Si2 Co1 67.27(8) . . ? C29 Si2 Co3 127.7(3) . . ? Co2 Si2 Co3 71.34(8) . . ? Co4 Si2 Co3 71.21(8) . . ? Co1 Si2 Co3 107.70(11) . . ? C29 Si2 Si1 178.3(3) . . ? Co2 Si2 Si1 54.12(8) . . ? Co4 Si2 Si1 53.61(8) . . ? Co1 Si2 Si1 53.81(8) . . ? Co3 Si2 Si1 53.89(8) . . ? C32 Si3 Co8 124.2(3) . . ? C32 Si3 Co6 127.9(3) . . ? Co8 Si3 Co6 107.61(11) . . ? C32 Si3 Co7 127.6(3) . . ? Co8 Si3 Co7 71.97(8) . . ? Co6 Si3 Co7 70.73(9) . . ? C32 Si3 Co5 124.7(3) . . ? Co8 Si3 Co5 68.76(8) . . ? Co6 Si3 Co5 67.16(8) . . ? Co7 Si3 Co5 107.75(10) . . ? C32 Si3 Si4 177.6(3) . . ? Co8 Si3 Si4 53.82(8) . . ? Co6 Si3 Si4 53.93(8) . . ? Co7 Si3 Si4 53.82(8) . . ? Co5 Si3 Si4 53.96(8) . . ? C35 Si4 Co8 125.7(3) . . ? C35 Si4 Co7 124.8(3) . . ? Co8 Si4 Co7 72.18(9) . . ? C35 Si4 Co6 126.4(3) . . ? Co8 Si4 Co6 107.75(11) . . ? Co7 Si4 Co6 70.89(9) . . ? C35 Si4 Co5 126.7(3) . . ? Co8 Si4 Co5 69.03(8) . . ? Co7 Si4 Co5 108.47(11) . . ? Co6 Si4 Co5 67.40(8) . . ? C35 Si4 Si3 178.8(3) . . ? Co8 Si4 Si3 53.92(8) . . ? Co7 Si4 Si3 54.10(8) . . ? Co6 Si4 Si3 53.98(8) . . ? Co5 Si4 Si3 54.40(8) . . ? O1 C1 Co1 174.1(10) . . ? O2 C2 Co1 173.5(9) . . ? O3 C3 Co2 174.8(9) . . ? O4 C4 Co2 156.9(9) . . ? O4 C4 Co1 124.1(8) . . ? Co2 C4 Co1 78.9(4) . . ? O5 C5 Co2 177.3(11) . . ? O6 C6 Co3 171.9(10) . . ? O7 C7 Co3 176.8(9) . . ? O8 C8 Co3 176.8(9) . . ? O9 C9 Co4 175.7(9) . . ? O10 C10 Co4 175.4(10) . . ? O11 C11 Co4 144.9(8) . . ? O11 C11 Co1 133.5(8) . . ? Co4 C11 Co1 81.6(4) . . ? O12 C12 Co5 175.3(9) . . ? O13 C13 Co5 174.7(9) . . ? O14 C14 Co6 143.4(9) . . ? O14 C14 Co5 133.3(8) . . ? Co6 C14 Co5 83.3(4) . . ? O15 C15 Co6 174.8(8) . . ? O16 C16 Co6 176.0(8) . . ? O17 C17 Co7 177.6(9) . . ? O18 C18 Co7 168.9(9) . . ? O19 C19 Co7 174.9(9) . . ? O20 C20 Co8 177.2(10) . . ? O21 C21 Co8 172.5(9) . . ? O22 C22 Co8 158.3(10) . . ? O22 C22 Co5 124.1(8) . . ? Co8 C22 Co5 77.6(4) . . ? C24 C23 C28 115.1(8) . . ? C24 C23 Si1 123.1(7) . . ? C28 C23 Si1 121.7(7) . . ? C23 C24 C25 123.0(10) . . ? C26 C25 C24 116.7(11) . . ? C27 C26 C25 121.9(11) . . ? C26 C27 C28 119.9(11) . . ? C27 C28 C23 123.3(9) . . ? C30 C29 C34 117.8(8) . . ? C30 C29 Si2 121.7(7) . . ? C34 C29 Si2 120.5(6) . . ? C29 C30 C31 122.2(9) . . ? C30 C31 C32 121.2(8) . . ? C31 C32 C33 116.9(8) . . ? C31 C32 Si3 121.6(7) . . ? C33 C32 Si3 121.4(6) . . ? C34 C33 C32 121.7(8) . . ? C33 C34 C29 120.2(8) . . ? C36 C35 C40 121.0(8) . . ? C36 C35 Si4 122.6(7) . . ? C40 C35 Si4 116.4(7) . . ? C35 C36 C37 119.0(9) . . ? C36 C37 C38 121.7(9) . . ? C39 C38 C37 119.7(9) . . ? C38 C39 C40 120.6(9) . . ? C39 C40 C35 117.9(9) . . ? Cl91 C91 Cl92 117.8(7) . . ? Cl94 C92 Cl93 126(2) 1_655 . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.199 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.114 data_fire _database_code_CSD 193183 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H10 Co4 O11 Si2, 0.5(C7 H8)' _chemical_formula_sum 'C26.50 H14 Co4 O11 Si2' _chemical_formula_weight 800.28 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.460(10) _cell_length_b 21.580(10) _cell_length_c 14.850(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.090(10) _cell_angle_gamma 90.00 _cell_volume 3032(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 2.287 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.2974 _exptl_absorpt_correction_T_max 0.5470 _exptl_absorpt_process_details 'phi scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nicolet P3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6401 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5960 _reflns_number_gt 4641 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL' _computing_cell_refinement 'SHELXTL' _computing_data_reduction 'SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III' _computing_publication_material 'WinGx' _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^)+(0.0496P)^2^+2.2501P] 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 5960 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.15078(4) 0.23603(2) 0.36433(3) 0.01536(11) Uani 1 1 d . . . Co2 Co -0.06116(5) 0.27525(2) 0.45561(3) 0.01640(11) Uani 1 1 d . . . Co3 Co -0.23247(4) 0.26480(2) 0.31536(3) 0.01586(11) Uani 1 1 d . . . Co4 Co -0.01013(5) 0.22217(2) 0.21668(3) 0.01526(11) Uani 1 1 d . . . Si1 Si -0.07104(9) 0.19065(4) 0.36034(6) 0.01502(19) Uani 1 1 d . . . Si2 Si -0.00922(9) 0.30809(4) 0.31017(6) 0.01420(19) Uani 1 1 d . . . C1 C 0.1372(4) 0.26129(16) 0.4866(2) 0.0211(7) Uani 1 1 d . . . O1 O 0.2056(3) 0.26605(14) 0.55112(17) 0.0360(7) Uani 1 1 d . . . C2 C 0.2357(4) 0.16328(16) 0.3928(2) 0.0210(7) Uani 1 1 d . . . O2 O 0.2952(3) 0.11972(12) 0.41351(17) 0.0317(6) Uani 1 1 d . . . C3 C 0.2968(3) 0.28624(16) 0.3347(2) 0.0197(7) Uani 1 1 d . . . O3 O 0.3915(3) 0.31657(12) 0.31736(18) 0.0323(6) Uani 1 1 d . . . C4 C -0.1202(4) 0.22862(16) 0.5490(2) 0.0212(7) Uani 1 1 d . . . O4 O -0.1530(3) 0.20044(13) 0.61047(17) 0.0355(7) Uani 1 1 d . . . C5 C -0.0531(4) 0.35423(17) 0.5009(2) 0.0250(8) Uani 1 1 d . . . O5 O -0.0413(3) 0.40128(13) 0.53249(18) 0.0406(7) Uani 1 1 d . . . C6 C -0.3605(4) 0.20387(17) 0.2940(3) 0.0267(8) Uani 1 1 d . . . O6 O -0.4447(3) 0.16848(13) 0.2772(2) 0.0475(8) Uani 1 1 d . . . C7 C -0.2926(4) 0.32203(16) 0.2347(2) 0.0226(7) Uani 1 1 d . . . O7 O -0.3341(3) 0.35515(13) 0.18118(19) 0.0381(7) Uani 1 1 d . . . C8 C -0.3028(4) 0.29567(18) 0.4184(2) 0.0277(8) Uani 1 1 d . . . O8 O -0.3802(3) 0.31550(14) 0.47034(18) 0.0369(7) Uani 1 1 d . . . C9 C -0.1158(4) 0.15859(17) 0.1731(2) 0.0247(8) Uani 1 1 d . . . O9 O -0.1838(3) 0.11958(13) 0.1462(2) 0.0438(8) Uani 1 1 d . . . C10 C 0.1604(4) 0.18752(17) 0.2023(2) 0.0243(8) Uani 1 1 d . . . O10 O 0.2599(3) 0.16212(14) 0.18091(17) 0.0372(7) Uani 1 1 d . . . C11 C -0.0108(4) 0.27691(16) 0.1235(2) 0.0215(7) Uani 1 1 d . . . O11 O -0.0120(3) 0.30983(12) 0.06432(17) 0.0334(6) Uani 1 1 d . . . C12 C -0.1188(4) 0.10909(15) 0.3897(2) 0.0214(7) Uani 1 1 d . . . C13 C -0.0402(4) 0.05946(16) 0.3569(3) 0.0294(8) Uani 1 1 d . . . H13 H 0.0419 0.0671 0.3219 0.035 Uiso 1 1 calc R . . C14 C -0.0810(5) -0.00153(18) 0.3750(3) 0.0391(10) Uani 1 1 d . . . H14 H -0.0259 -0.0351 0.3530 0.047 Uiso 1 1 calc R . . C15 C -0.2005(5) -0.01298(19) 0.4245(3) 0.0419(11) Uani 1 1 d . . . H15 H -0.2282 -0.0545 0.4366 0.050 Uiso 1 1 calc R . . C16 C -0.2808(5) 0.0357(2) 0.4571(3) 0.0418(11) Uani 1 1 d . . . H16 H -0.3637 0.0276 0.4911 0.050 Uiso 1 1 calc R . . C17 C -0.2403(4) 0.09645(17) 0.4399(2) 0.0291(8) Uani 1 1 d . . . H17 H -0.2957 0.1297 0.4625 0.035 Uiso 1 1 calc R . . C18 C 0.0206(3) 0.39058(15) 0.2767(2) 0.0175(7) Uani 1 1 d . . . C19 C 0.1323(4) 0.40935(15) 0.2210(2) 0.0218(7) Uani 1 1 d . . . H19 H 0.1967 0.3794 0.1985 0.026 Uiso 1 1 calc R . . C20 C 0.1494(4) 0.47144(16) 0.1982(2) 0.0277(8) Uani 1 1 d . . . H20 H 0.2250 0.4837 0.1601 0.033 Uiso 1 1 calc R . . C21 C 0.0565(4) 0.51532(17) 0.2312(3) 0.0334(9) Uani 1 1 d . . . H21 H 0.0694 0.5578 0.2164 0.040 Uiso 1 1 calc R . . C22 C -0.0554(4) 0.49776(17) 0.2854(3) 0.0325(9) Uani 1 1 d . . . H22 H -0.1200 0.5280 0.3070 0.039 Uiso 1 1 calc R . . C23 C -0.0731(4) 0.43580(16) 0.3082(2) 0.0253(8) Uani 1 1 d . . . H23 H -0.1498 0.4240 0.3456 0.030 Uiso 1 1 calc R . . C24 C 1.0727(11) 0.0155(5) 0.9324(12) 0.184(9) Uani 1 1 d . . . C25 C 0.8197(10) 0.0258(5) 0.9239(7) 0.129(3) Uani 1 1 d . . . C26 C 0.9354(13) 0.0267(5) 0.8727(7) 0.061(3) Uani 0.50 1 d P . . C27 C 1.175(2) 0.0011(8) 0.9839(13) 0.113(8) Uani 0.50 1 d P . . C28 C 0.963(3) 0.0097(5) 0.9771(12) 0.137(10) Uani 0.50 1 d P . . 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 0.0125(2) 0.0151(2) 0.0185(2) 0.00129(17) -0.00092(17) 0.00043(17) Co2 0.0180(2) 0.0160(2) 0.0153(2) 0.00023(17) 0.00205(17) 0.00011(17) Co3 0.0121(2) 0.0162(2) 0.0193(2) 0.00253(17) -0.00038(16) -0.00102(17) Co4 0.0161(2) 0.0147(2) 0.0150(2) 0.00080(16) -0.00060(16) -0.00197(17) Si1 0.0151(4) 0.0131(4) 0.0169(4) 0.0022(3) 0.0007(3) -0.0008(3) Si2 0.0127(4) 0.0121(4) 0.0178(4) 0.0013(3) 0.0004(3) -0.0007(3) C1 0.0209(18) 0.0226(18) 0.0197(16) 0.0004(14) -0.0008(14) -0.0022(14) O1 0.0307(15) 0.0527(19) 0.0244(13) -0.0063(13) -0.0110(11) 0.0054(13) C2 0.0195(17) 0.0231(18) 0.0203(17) 0.0001(14) -0.0011(13) -0.0003(15) O2 0.0351(15) 0.0224(14) 0.0376(15) 0.0055(11) -0.0011(12) 0.0099(12) C3 0.0143(16) 0.0249(18) 0.0201(16) -0.0027(14) -0.0031(13) 0.0065(14) O3 0.0193(13) 0.0360(16) 0.0415(16) 0.0052(12) -0.0026(11) -0.0105(12) C4 0.0191(17) 0.0266(19) 0.0180(16) 0.0021(14) 0.0026(13) -0.0011(14) O4 0.0429(17) 0.0393(16) 0.0242(14) 0.0088(12) 0.0057(12) -0.0077(13) C5 0.028(2) 0.023(2) 0.0238(18) 0.0008(15) -0.0005(15) -0.0002(15) O5 0.061(2) 0.0227(15) 0.0379(16) -0.0114(12) -0.0004(14) -0.0033(13) C6 0.0174(18) 0.0233(19) 0.040(2) 0.0044(16) -0.0029(15) -0.0012(15) O6 0.0278(16) 0.0290(16) 0.086(2) 0.0009(15) -0.0159(15) -0.0101(13) C7 0.0173(17) 0.0228(18) 0.0278(18) 0.0019(15) -0.0019(14) -0.0034(14) O7 0.0362(16) 0.0336(16) 0.0445(17) 0.0160(13) -0.0108(13) 0.0029(13) C8 0.026(2) 0.031(2) 0.0266(19) 0.0058(16) 0.0000(16) -0.0013(16) O8 0.0261(15) 0.0553(19) 0.0293(14) -0.0013(13) 0.0045(12) 0.0090(13) C9 0.029(2) 0.0231(19) 0.0220(17) 0.0030(15) -0.0046(15) 0.0006(16) O9 0.055(2) 0.0289(16) 0.0472(18) -0.0044(13) -0.0180(15) -0.0158(14) C10 0.0226(19) 0.030(2) 0.0199(17) 0.0050(15) 0.0016(14) 0.0002(16) O10 0.0274(15) 0.0564(19) 0.0279(14) -0.0010(13) 0.0034(12) 0.0147(14) C11 0.0200(18) 0.0253(19) 0.0193(17) 0.0003(15) -0.0014(13) -0.0029(14) O11 0.0411(17) 0.0339(15) 0.0251(13) 0.0108(12) -0.0058(11) -0.0050(13) C12 0.0271(19) 0.0175(17) 0.0196(16) 0.0043(13) -0.0012(14) -0.0050(14) C13 0.036(2) 0.0178(18) 0.034(2) 0.0008(15) -0.0013(17) -0.0013(16) C14 0.057(3) 0.0173(19) 0.043(2) -0.0004(17) -0.003(2) 0.0002(19) C15 0.071(3) 0.021(2) 0.034(2) 0.0000(17) 0.000(2) -0.019(2) C16 0.054(3) 0.040(3) 0.031(2) -0.0003(18) 0.0107(19) -0.026(2) C17 0.038(2) 0.025(2) 0.0237(18) 0.0010(15) 0.0035(16) -0.0084(16) C18 0.0193(17) 0.0130(16) 0.0200(16) 0.0004(12) -0.0019(13) -0.0001(13) C19 0.0223(18) 0.0171(17) 0.0260(17) 0.0006(14) 0.0024(14) -0.0001(14) C20 0.033(2) 0.0209(19) 0.0295(19) 0.0034(15) 0.0083(16) -0.0073(16) C21 0.042(2) 0.0173(19) 0.041(2) 0.0070(16) 0.0030(18) -0.0038(17) C22 0.038(2) 0.0159(18) 0.044(2) 0.0003(16) 0.0082(19) 0.0071(16) C23 0.0229(19) 0.0241(19) 0.0290(19) 0.0041(15) 0.0054(15) 0.0019(15) C24 0.063(6) 0.077(7) 0.41(3) -0.055(10) 0.068(10) -0.021(5) C25 0.102(7) 0.137(9) 0.149(9) 0.024(7) -0.038(7) -0.004(6) C26 0.065(7) 0.056(7) 0.063(7) 0.017(5) 0.024(6) 0.007(6) C27 0.157(18) 0.073(11) 0.110(13) -0.048(9) 0.085(13) -0.070(12) C28 0.29(3) 0.019(6) 0.102(13) 0.025(7) -0.116(16) -0.039(11) _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 C3 1.810(4) . ? Co1 C2 1.813(4) . ? Co1 C1 1.900(4) . ? Co1 Si2 2.3134(15) . ? Co1 Si1 2.316(2) . ? Co1 Co2 2.5655(18) . ? Co1 Co4 2.6840(16) . ? Co2 C4 1.803(3) . ? Co2 C5 1.834(4) . ? Co2 C1 1.955(4) . ? Co2 Si1 2.3115(13) . ? Co2 Si2 2.3262(16) . ? Co2 C8 2.392(4) . ? Co2 Co3 2.6466(16) . ? Co3 C8 1.797(4) . ? Co3 C7 1.812(4) . ? Co3 C6 1.815(4) . ? Co3 Si1 2.3099(15) . ? Co3 Si2 2.311(2) . ? Co3 Co4 2.7253(19) . ? Co4 C10 1.791(4) . ? Co4 C9 1.816(4) . ? Co4 C11 1.819(4) . ? Co4 Si1 2.3128(16) . ? Co4 Si2 2.3163(13) . ? Si1 C12 1.869(3) . ? Si1 Si2 2.7056(16) . ? Si2 C18 1.870(3) . ? C1 O1 1.160(4) . ? C2 O2 1.137(4) . ? C3 O3 1.139(4) . ? C4 O4 1.140(4) . ? C5 O5 1.124(4) . ? C6 O6 1.131(4) . ? C7 O7 1.138(4) . ? C8 O8 1.147(4) . ? C9 O9 1.132(4) . ? C10 O10 1.135(4) . ? C11 O11 1.131(4) . ? C12 C13 1.392(5) . ? C12 C17 1.397(5) . ? C13 C14 1.398(5) . ? C14 C15 1.372(6) . ? C15 C16 1.384(6) . ? C16 C17 1.390(5) . ? C18 C23 1.399(5) . ? C18 C19 1.403(5) . ? C19 C20 1.391(5) . ? C20 C21 1.382(5) . ? C21 C22 1.384(5) . ? C22 C23 1.389(5) . ? C24 C28 1.24(3) . ? C24 C27 1.27(3) . ? C24 C28 1.49(3) 3_757 ? C24 C26 1.590(19) . ? C25 C26 1.334(13) . ? C25 C27 1.49(2) 3_757 ? C25 C28 1.61(2) . ? C26 C28 1.614(18) . ? C27 C28 1.45(4) 3_757 ? C27 C25 1.49(2) 3_757 ? C27 C28 2.02(4) . ? C28 C28 1.06(3) 3_757 ? C28 C27 1.45(4) 3_757 ? C28 C24 1.49(3) 3_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 C3 Co1 C2 103.70(16) . . ? C3 Co1 C1 96.49(14) . . ? C2 Co1 C1 93.20(15) . . ? C3 Co1 Si2 90.71(12) . . ? C2 Co1 Si2 162.26(11) . . ? C1 Co1 Si2 95.41(11) . . ? C3 Co1 Si1 159.78(11) . . ? C2 Co1 Si1 92.35(12) . . ? C1 Co1 Si1 94.78(11) . . ? Si2 Co1 Si1 71.52(6) . . ? C3 Co1 Co2 121.88(11) . . ? C2 Co1 Co2 120.57(11) . . ? C1 Co1 Co2 49.20(11) . . ? Si2 Co1 Co2 56.67(5) . . ? Si1 Co1 Co2 56.24(5) . . ? C3 Co1 Co4 107.48(11) . . ? C2 Co1 Co4 110.16(11) . . ? C1 Co1 Co4 140.67(11) . . ? Si2 Co1 Co4 54.62(4) . . ? Si1 Co1 Co4 54.50(4) . . ? Co2 Co1 Co4 91.47(7) . . ? C4 Co2 C5 104.43(16) . . ? C4 Co2 C1 91.79(15) . . ? C5 Co2 C1 91.00(15) . . ? C4 Co2 Si1 91.02(12) . . ? C5 Co2 Si1 163.78(11) . . ? C1 Co2 Si1 93.46(10) . . ? C4 Co2 Si2 161.88(11) . . ? C5 Co2 Si2 92.79(12) . . ? C1 Co2 Si2 93.52(11) . . ? Si1 Co2 Si2 71.38(5) . . ? C4 Co2 C8 89.06(14) . . ? C5 Co2 C8 87.30(15) . . ? C1 Co2 C8 178.24(14) . . ? Si1 Co2 C8 88.07(10) . . ? Si2 Co2 C8 86.13(9) . . ? C4 Co2 Co1 117.75(11) . . ? C5 Co2 Co1 117.92(12) . . ? C1 Co2 Co1 47.38(11) . . ? Si1 Co2 Co1 56.42(4) . . ? Si2 Co2 Co1 56.19(3) . . ? C8 Co2 Co1 133.31(10) . . ? C4 Co2 Co3 111.58(12) . . ? C5 Co2 Co3 113.14(11) . . ? C1 Co2 Co3 139.34(10) . . ? Si1 Co2 Co3 55.03(3) . . ? Si2 Co2 Co3 54.92(5) . . ? C8 Co2 Co3 41.41(9) . . ? Co1 Co2 Co3 91.96(7) . . ? C8 Co3 C7 101.19(17) . . ? C8 Co3 C6 99.74(18) . . ? C7 Co3 C6 99.77(16) . . ? C8 Co3 Si1 104.83(13) . . ? C7 Co3 Si1 150.48(12) . . ? C6 Co3 Si1 89.40(13) . . ? C8 Co3 Si2 102.60(13) . . ? C7 Co3 Si2 89.33(12) . . ? C6 Co3 Si2 153.73(12) . . ? Si1 Co3 Si2 71.69(6) . . ? C8 Co3 Co2 61.68(13) . . ? C7 Co3 Co2 130.81(11) . . ? C6 Co3 Co2 127.35(12) . . ? Si1 Co3 Co2 55.09(4) . . ? Si2 Co3 Co2 55.47(4) . . ? C8 Co3 Co4 150.44(12) . . ? C7 Co3 Co4 96.67(12) . . ? C6 Co3 Co4 100.20(13) . . ? Si1 Co3 Co4 53.93(5) . . ? Si2 Co3 Co4 54.01(5) . . ? Co2 Co3 Co4 88.84(7) . . ? C10 Co4 C9 97.92(18) . . ? C10 Co4 C11 100.53(15) . . ? C9 Co4 C11 102.61(15) . . ? C10 Co4 Si1 102.28(11) . . ? C9 Co4 Si1 88.20(12) . . ? C11 Co4 Si1 153.09(11) . . ? C10 Co4 Si2 113.76(12) . . ? C9 Co4 Si2 145.06(12) . . ? C11 Co4 Si2 86.33(12) . . ? Si1 Co4 Si2 71.53(5) . . ? C10 Co4 Co1 68.53(12) . . ? C9 Co4 Co1 133.35(11) . . ? C11 Co4 Co1 123.38(11) . . ? Si1 Co4 Co1 54.62(5) . . ? Si2 Co4 Co1 54.52(3) . . ? C10 Co4 Co3 154.28(11) . . ? C9 Co4 Co3 91.24(13) . . ? C11 Co4 Co3 100.82(11) . . ? Si1 Co4 Co3 53.82(3) . . ? Si2 Co4 Co3 53.82(4) . . ? Co1 Co4 Co3 87.73(7) . . ? C12 Si1 Co3 124.05(13) . . ? C12 Si1 Co2 127.62(11) . . ? Co3 Si1 Co2 69.88(4) . . ? C12 Si1 Co4 123.57(11) . . ? Co3 Si1 Co4 72.25(4) . . ? Co2 Si1 Co4 108.81(5) . . ? C12 Si1 Co1 127.70(12) . . ? Co3 Si1 Co1 108.24(7) . . ? Co2 Si1 Co1 67.34(3) . . ? Co4 Si1 Co1 70.87(3) . . ? C12 Si1 Si2 177.18(11) . . ? Co3 Si1 Si2 54.17(5) . . ? Co2 Si1 Si2 54.56(4) . . ? Co4 Si1 Si2 54.29(3) . . ? Co1 Si1 Si2 54.19(3) . . ? C18 Si2 Co3 122.14(11) . . ? C18 Si2 Co1 129.30(12) . . ? Co3 Si2 Co1 108.31(7) . . ? C18 Si2 Co4 127.12(11) . . ? Co3 Si2 Co4 72.17(4) . . ? Co1 Si2 Co4 70.86(4) . . ? C18 Si2 Co2 124.66(11) . . ? Co3 Si2 Co2 69.61(3) . . ? Co1 Si2 Co2 67.14(4) . . ? Co4 Si2 Co2 108.18(5) . . ? C18 Si2 Si1 176.11(11) . . ? Co3 Si2 Si1 54.14(3) . . ? Co1 Si2 Si1 54.29(5) . . ? Co4 Si2 Si1 54.17(4) . . ? Co2 Si2 Si1 54.06(3) . . ? O1 C1 Co1 140.9(3) . . ? O1 C1 Co2 135.7(3) . . ? Co1 C1 Co2 83.42(13) . . ? O2 C2 Co1 175.8(3) . . ? O3 C3 Co1 177.9(3) . . ? O4 C4 Co2 176.9(3) . . ? O5 C5 Co2 175.4(3) . . ? O6 C6 Co3 175.6(3) . . ? O7 C7 Co3 175.9(3) . . ? O8 C8 Co3 161.5(3) . . ? O8 C8 Co2 121.6(3) . . ? Co3 C8 Co2 76.92(14) . . ? O9 C9 Co4 178.8(4) . . ? O10 C10 Co4 169.2(3) . . ? O11 C11 Co4 178.4(3) . . ? C13 C12 C17 118.5(3) . . ? C13 C12 Si1 120.9(3) . . ? C17 C12 Si1 120.5(3) . . ? C12 C13 C14 120.6(4) . . ? C15 C14 C13 120.0(4) . . ? C14 C15 C16 120.2(4) . . ? C15 C16 C17 120.0(4) . . ? C16 C17 C12 120.6(4) . . ? C23 C18 C19 118.3(3) . . ? C23 C18 Si2 118.7(2) . . ? C19 C18 Si2 123.1(2) . . ? C20 C19 C18 120.6(3) . . ? C21 C20 C19 120.0(3) . . ? C20 C21 C22 120.4(3) . . ? C21 C22 C23 119.9(3) . . ? C22 C23 C18 120.9(3) . . ? C28 C24 C27 107.0(17) . . ? C28 C24 C28 44.7(18) . 3_757 ? C27 C24 C28 62.7(16) . 3_757 ? C28 C24 C26 68.3(8) . . ? C27 C24 C26 173.4(13) . . ? C28 C24 C26 111.9(15) 3_757 . ? C26 C25 C27 120.3(12) . 3_757 ? C26 C25 C28 65.9(13) . . ? C27 C25 C28 55.7(14) 3_757 . ? C25 C26 C24 110.5(10) . . ? C25 C26 C28 65.2(14) . . ? C24 C26 C28 45.5(13) . . ? C24 C27 C28 66.0(14) . 3_757 ? C24 C27 C25 132.2(15) . 3_757 ? C28 C27 C25 66.3(8) 3_757 3_757 ? C24 C27 C28 36.0(11) . . ? C28 C27 C28 30.3(10) 3_757 . ? C25 C27 C28 96.4(10) 3_757 . ? C28 C28 C24 80(4) 3_757 . ? C28 C28 C27 106(3) 3_757 3_757 ? C24 C28 C27 170.7(15) . 3_757 ? C28 C28 C24 55(2) 3_757 3_757 ? C24 C28 C24 135.3(18) . 3_757 ? C27 C28 C24 51.3(14) 3_757 3_757 ? C28 C28 C25 163(4) 3_757 . ? C24 C28 C25 114.9(15) . . ? C27 C28 C25 58.1(17) 3_757 . ? C24 C28 C25 109(2) 3_757 . ? C28 C28 C26 144(5) 3_757 . ? C24 C28 C26 66.2(15) . . ? C27 C28 C26 106.1(19) 3_757 . ? C24 C28 C26 156(2) 3_757 . ? C25 C28 C26 49.0(7) . . ? C28 C28 C27 44(3) 3_757 . ? C24 C28 C27 37.0(12) . . ? C27 C28 C27 149.7(10) 3_757 . ? C24 C28 C27 98.5(11) 3_757 . ? C25 C28 C27 152.0(17) . . ? C26 C28 C27 103.1(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.941 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.096