Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Hitchcock, P. B.' 'Nixon, J.' 'Sakarya, Nurgun' _publ_contact_author_name 'Prof J Nixon' _publ_contact_author_address ; Prof J Nixon School of Chemistry, Physics and Environmental Sciences Sussex University Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email 'J.NIXON@SUSSEX.AC.UK' _publ_section_title ; Remarkable organophosphorus cage compounds from the reactin of cobaltocene and the triphosphole P3C2But2CH(SiMe3)2: Crystal and molecular structures of [Co(n5-C5H5)(n4-C4H4CHCHP6C4But4)] and P6C4But4CH(SiMe3) ; data_feb897 _database_code_CSD 172116 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Co(Cp)(CpP6cage)]' _chemical_formula_moiety 'C31 H47 Co P6' _chemical_formula_sum 'C31 H47 Co P6' _chemical_formula_weight 664.44 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 9.634(3) _cell_length_b 32.706(7) _cell_length_c 10.510(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.16(2) _cell_angle_gamma 90.00 _cell_volume 3278.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method ? _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_type 'psi-scan data' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 1.00 _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 'CAD4' _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6120 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0948 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 24.98 _reflns_number_total 5769 _reflns_number_observed 3897 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 23 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+6.1285P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding mode' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5746 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_obs 0.0563 _refine_ls_wR_factor_all 0.1553 _refine_ls_wR_factor_obs 0.1187 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_goodness_of_fit_obs 1.047 _refine_ls_restrained_S_all 1.114 _refine_ls_restrained_S_obs 1.047 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co Co 0.24015(8) 0.67737(2) 0.39420(7) 0.0259(2) Uani 1 d . . P1 P 0.59071(14) 0.61862(4) 0.87683(13) 0.0201(3) Uani 1 d . . P2 P 0.56471(14) 0.58041(4) 0.70417(13) 0.0185(3) Uani 1 d . . P3 P 0.84590(14) 0.55680(4) 0.87894(12) 0.0203(3) Uani 1 d . . P4 P 0.87014(14) 0.60151(4) 0.66637(13) 0.0213(3) Uani 1 d . . P5 P 0.73476(14) 0.65538(4) 0.65609(13) 0.0212(3) Uani 1 d . . P6 P 0.86601(14) 0.63741(4) 0.94360(13) 0.0235(3) Uani 1 d . . C1 C 0.1427(8) 0.7275(2) 0.3017(7) 0.057(2) Uani 1 d . . H1 H 0.1800(8) 0.7443(2) 0.2411(7) 0.068 Uiso 1 calc R . C2 C 0.1620(7) 0.7332(2) 0.4341(7) 0.049(2) Uani 1 d . . H2 H 0.2165(7) 0.7542(2) 0.4796(7) 0.059 Uiso 1 calc R . C3 C 0.0892(7) 0.7034(2) 0.4877(7) 0.048(2) Uani 1 d . . H3 H 0.0818(7) 0.7007(2) 0.5765(7) 0.058 Uiso 1 calc R . C4 C 0.0282(7) 0.6780(2) 0.3901(9) 0.056(2) Uani 1 d . . H4 H -0.0259(7) 0.6543(2) 0.4010(9) 0.067 Uiso 1 calc R . C5 C 0.0595(8) 0.6930(3) 0.2727(7) 0.067(3) Uani 1 d . . H5 H 0.0299(8) 0.6819(3) 0.1897(7) 0.081 Uiso 1 calc R . C6 C 0.3218(5) 0.62457(15) 0.4762(5) 0.0231(12) Uani 1 d . . H6 H 0.2501(5) 0.60981(15) 0.5096(5) 0.028 Uiso 1 calc R . C7 C 0.3355(6) 0.6282(2) 0.3436(5) 0.0300(14) Uani 1 d . . H7 H 0.2982(6) 0.6102(2) 0.2764(5) 0.036 Uiso 1 calc R . C8 C 0.4157(6) 0.6639(2) 0.3318(5) 0.0303(14) Uani 1 d . . H8 H 0.4427(6) 0.6745(2) 0.2549(5) 0.036 Uiso 1 calc R . C9 C 0.4478(6) 0.6806(2) 0.4557(5) 0.0255(12) Uani 1 d . . H9 H 0.4716(6) 0.7083(2) 0.4739(5) 0.031 Uiso 1 calc R . C10 C 0.4389(5) 0.64780(15) 0.5558(5) 0.0213(11) Uani 1 d . . H10 H 0.4064(5) 0.65962(15) 0.6342(5) 0.026 Uiso 1 calc R . C11 C 0.5773(5) 0.6236(2) 0.5918(5) 0.0196(11) Uani 1 d . . H11 H 0.5991(5) 0.6112(2) 0.5101(5) 0.024 Uiso 1 calc R . C12 C 0.7148(5) 0.6591(2) 0.8292(5) 0.0230(12) Uani 1 d . . C13 C 0.6801(6) 0.7045(2) 0.8688(5) 0.0300(14) Uani 1 d . . C14 C 0.5440(6) 0.7195(2) 0.7893(6) 0.0344(15) Uani 1 d . . H14C H 0.5530(6) 0.7182(2) 0.6977(6) 0.052 Uiso 1 calc R . H14B H 0.5258(6) 0.7478(2) 0.8128(6) 0.052 Uiso 1 calc R . H14A H 0.4659(6) 0.7021(2) 0.8066(6) 0.052 Uiso 1 calc R . C15 C 0.8003(7) 0.7325(2) 0.8457(7) 0.050(2) Uani 1 d . . H15C H 0.8134(7) 0.7311(2) 0.7551(7) 0.075 Uiso 1 calc R . H15B H 0.8865(7) 0.7237(2) 0.8997(7) 0.075 Uiso 1 calc R . H15A H 0.7783(7) 0.7607(2) 0.8675(7) 0.075 Uiso 1 calc R . C16 C 0.6614(7) 0.7071(2) 1.0094(6) 0.047(2) Uani 1 d . . H16C H 0.5842(7) 0.6892(2) 1.0255(6) 0.071 Uiso 1 calc R . H16B H 0.6398(7) 0.7353(2) 1.0307(6) 0.071 Uiso 1 calc R . H16A H 0.7481(7) 0.6984(2) 1.0629(6) 0.071 Uiso 1 calc R . C17 C 0.7462(5) 0.5605(2) 0.7107(5) 0.0180(11) Uani 1 d . . C18 C 0.7467(6) 0.5189(2) 0.6357(5) 0.0272(13) Uani 1 d . . C19 C 0.6795(7) 0.5256(2) 0.4966(5) 0.0342(14) Uani 1 d . . H19C H 0.7327(7) 0.5463(2) 0.4565(5) 0.051 Uiso 1 calc R . H19B H 0.5826(7) 0.5349(2) 0.4950(5) 0.051 Uiso 1 calc R . H19A H 0.6801(7) 0.4998(2) 0.4489(5) 0.051 Uiso 1 calc R . C20 C 0.8951(7) 0.5033(2) 0.6342(6) 0.042(2) Uani 1 d . . H20C H 0.9486(7) 0.5236(2) 0.5926(6) 0.064 Uiso 1 calc R . H20B H 0.8920(7) 0.4775(2) 0.5863(6) 0.064 Uiso 1 calc R . H20A H 0.9403(7) 0.4988(2) 0.7226(6) 0.064 Uiso 1 calc R . C21 C 0.6665(7) 0.4869(2) 0.7005(6) 0.037(2) Uani 1 d . . H21C H 0.5703(7) 0.4963(2) 0.7024(6) 0.056 Uiso 1 calc R . H21B H 0.7129(7) 0.4824(2) 0.7886(6) 0.056 Uiso 1 calc R . H21A H 0.6645(7) 0.4612(2) 0.6523(6) 0.056 Uiso 1 calc R . C22 C 0.7464(5) 0.5931(2) 0.9705(5) 0.0208(12) Uani 1 d . . C23 C 0.7274(6) 0.5776(2) 1.1049(5) 0.0313(14) Uani 1 d . . C24 C 0.6307(7) 0.5403(2) 1.0886(6) 0.047(2) Uani 1 d . . H24C H 0.5402(7) 0.5480(2) 1.0399(6) 0.071 Uiso 1 calc R . H24B H 0.6164(7) 0.5300(2) 1.1734(6) 0.071 Uiso 1 calc R . H24A H 0.6737(7) 0.5188(2) 1.0421(6) 0.071 Uiso 1 calc R . C25 C 0.6645(7) 0.6106(2) 1.1833(6) 0.048(2) Uani 1 d . . H25C H 0.7270(7) 0.6344(2) 1.1935(6) 0.072 Uiso 1 calc R . H25B H 0.6538(7) 0.5996(2) 1.2682(6) 0.072 Uiso 1 calc R . H25A H 0.5726(7) 0.6188(2) 1.1385(6) 0.072 Uiso 1 calc R . C26 C 0.8691(6) 0.5656(2) 1.1809(5) 0.042(2) Uani 1 d . . H26C H 0.9307(6) 0.5896(2) 1.1911(5) 0.064 Uiso 1 calc R . H26B H 0.9123(6) 0.5442(2) 1.1344(5) 0.064 Uiso 1 calc R . H26A H 0.8550(6) 0.5554(2) 1.2658(5) 0.064 Uiso 1 calc R . C27 C 0.9521(5) 0.6025(2) 0.8381(5) 0.0224(12) Uani 1 d . . C28 C 1.1146(5) 0.6026(2) 0.8639(5) 0.0279(13) Uani 1 d . . C29 C 1.1651(6) 0.6437(2) 0.8172(7) 0.046(2) Uani 1 d . . H29C H 1.1307(6) 0.6470(2) 0.7255(7) 0.069 Uiso 1 calc R . H29B H 1.2678(6) 0.6444(2) 0.8307(7) 0.069 Uiso 1 calc R . H29A H 1.1290(6) 0.6660(2) 0.8657(7) 0.069 Uiso 1 calc R . C30 C 1.1756(6) 0.5682(2) 0.7921(6) 0.041(2) Uani 1 d . . H30C H 1.1433(6) 0.5709(2) 0.6998(6) 0.062 Uiso 1 calc R . H30B H 1.1447(6) 0.5418(2) 0.8224(6) 0.062 Uiso 1 calc R . H30A H 1.2783(6) 0.5696(2) 0.8078(6) 0.062 Uiso 1 calc R . C31 C 1.1674(6) 0.5972(2) 1.0059(6) 0.045(2) Uani 1 d . . H31C H 1.1296(6) 0.6190(2) 1.0549(6) 0.068 Uiso 1 calc R . H31B H 1.2700(6) 0.5984(2) 1.0200(6) 0.068 Uiso 1 calc R . H31A H 1.1365(6) 0.5706(2) 1.0347(6) 0.068 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 Co 0.0282(4) 0.0218(4) 0.0255(4) 0.0014(3) -0.0041(3) 0.0080(3) P1 0.0154(7) 0.0234(7) 0.0218(7) 0.0010(6) 0.0035(5) 0.0041(6) P2 0.0159(7) 0.0172(7) 0.0222(7) 0.0024(5) 0.0024(5) 0.0004(6) P3 0.0185(7) 0.0234(7) 0.0195(7) 0.0050(6) 0.0048(6) 0.0062(6) P4 0.0165(7) 0.0259(8) 0.0224(7) 0.0060(6) 0.0055(6) 0.0037(6) P5 0.0181(7) 0.0190(7) 0.0263(7) 0.0060(6) 0.0021(6) -0.0018(6) P6 0.0185(7) 0.0253(8) 0.0249(7) -0.0019(6) -0.0037(6) 0.0022(6) C1 0.061(5) 0.058(5) 0.054(5) 0.034(4) 0.017(4) 0.040(4) C2 0.048(4) 0.030(4) 0.066(5) -0.006(3) -0.002(4) 0.020(3) C3 0.046(4) 0.060(5) 0.038(4) 0.008(4) 0.004(3) 0.032(4) C4 0.026(4) 0.041(4) 0.098(7) 0.002(4) 0.003(4) 0.010(3) C5 0.049(5) 0.095(7) 0.047(5) -0.026(5) -0.031(4) 0.044(5) C6 0.020(3) 0.015(3) 0.032(3) 0.003(2) -0.003(2) 0.001(2) C7 0.039(3) 0.022(3) 0.026(3) -0.001(2) -0.006(3) 0.013(3) C8 0.037(4) 0.025(3) 0.030(3) 0.008(2) 0.006(3) 0.016(3) C9 0.030(3) 0.013(3) 0.033(3) 0.003(2) 0.003(2) 0.007(2) C10 0.022(3) 0.018(3) 0.024(3) 0.001(2) 0.002(2) 0.002(2) C11 0.017(3) 0.021(3) 0.021(3) 0.000(2) 0.004(2) 0.001(2) C12 0.020(3) 0.022(3) 0.026(3) -0.001(2) 0.001(2) 0.004(2) C13 0.032(3) 0.018(3) 0.036(3) -0.007(2) -0.010(3) 0.001(2) C14 0.044(4) 0.021(3) 0.035(3) -0.007(2) -0.007(3) 0.014(3) C15 0.049(4) 0.020(3) 0.073(5) 0.000(3) -0.014(4) -0.005(3) C16 0.057(5) 0.038(4) 0.041(4) -0.015(3) -0.012(3) 0.023(3) C17 0.013(2) 0.024(3) 0.016(2) 0.006(2) 0.000(2) 0.003(2) C18 0.034(3) 0.019(3) 0.029(3) -0.002(2) 0.005(3) 0.012(3) C19 0.046(4) 0.029(3) 0.027(3) -0.009(3) 0.005(3) 0.004(3) C20 0.044(4) 0.038(4) 0.046(4) -0.012(3) 0.007(3) 0.022(3) C21 0.057(4) 0.021(3) 0.033(3) 0.001(3) 0.001(3) 0.004(3) C22 0.016(3) 0.028(3) 0.019(3) 0.001(2) 0.001(2) 0.003(2) C23 0.032(3) 0.042(4) 0.022(3) 0.011(3) 0.009(3) 0.015(3) C24 0.039(4) 0.062(5) 0.044(4) 0.023(4) 0.018(3) 0.004(4) C25 0.054(4) 0.071(5) 0.023(3) 0.004(3) 0.019(3) 0.029(4) C26 0.043(4) 0.061(4) 0.025(3) 0.010(3) 0.008(3) 0.026(3) C27 0.016(3) 0.031(3) 0.020(3) 0.007(2) 0.001(2) 0.003(2) C28 0.011(3) 0.035(3) 0.038(3) 0.010(3) 0.003(2) -0.002(2) C29 0.020(3) 0.054(4) 0.062(5) 0.018(4) 0.000(3) -0.005(3) C30 0.017(3) 0.058(4) 0.051(4) 0.011(3) 0.011(3) 0.008(3) C31 0.018(3) 0.070(5) 0.045(4) 0.012(4) -0.004(3) 0.009(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 Co C8 1.949(6) . ? Co C7 1.963(5) . ? Co C9 2.016(5) . ? Co C4 2.036(7) . ? Co C6 2.038(5) . ? Co C2 2.041(6) . ? Co C3 2.052(7) . ? Co C1 2.063(6) . ? Co C5 2.072(6) . ? P1 C22 1.870(5) . ? P1 C12 1.897(6) . ? P1 P2 2.188(2) . ? P2 C11 1.857(5) . ? P2 C17 1.858(5) . ? P3 C22 1.876(5) . ? P3 C17 1.893(5) . ? P3 C27 1.893(5) . ? P4 C27 1.865(5) . ? P4 C17 1.897(5) . ? P4 P5 2.185(2) . ? P5 C12 1.861(5) . ? P5 C11 1.882(5) . ? P6 C27 1.867(6) . ? P6 C12 1.890(5) . ? P6 C22 1.897(5) . ? C1 C5 1.392(11) . ? C1 C2 1.391(10) . ? C2 C3 1.367(10) . ? C3 C4 1.385(10) . ? C4 C5 1.401(11) . ? C6 C7 1.423(8) . ? C6 C10 1.510(7) . ? C7 C8 1.414(8) . ? C8 C9 1.405(8) . ? C9 C10 1.513(7) . ? C10 C11 1.550(7) . ? C12 C13 1.591(7) . ? C13 C16 1.516(8) . ? C13 C15 1.522(8) . ? C13 C14 1.532(7) . ? C17 C18 1.573(7) . ? C18 C21 1.519(8) . ? C18 C20 1.520(8) . ? C18 C19 1.528(7) . ? C22 C23 1.536(7) . ? C23 C24 1.530(9) . ? C23 C26 1.531(8) . ? C23 C25 1.534(8) . ? C27 C28 1.551(7) . ? C28 C31 1.518(8) . ? C28 C30 1.519(8) . ? C28 C29 1.533(8) . ? 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 C8 Co C7 42.4(2) . . ? C8 Co C9 41.5(2) . . ? C7 Co C9 69.4(2) . . ? C8 Co C4 155.6(3) . . ? C7 Co C4 120.6(3) . . ? C9 Co C4 162.3(3) . . ? C8 Co C6 69.4(2) . . ? C7 Co C6 41.6(2) . . ? C9 Co C6 66.6(2) . . ? C4 Co C6 110.1(3) . . ? C8 Co C2 129.4(3) . . ? C7 Co C2 171.6(3) . . ? C9 Co C2 105.4(3) . . ? C4 Co C2 66.3(3) . . ? C6 Co C2 143.4(3) . . ? C8 Co C3 164.3(3) . . ? C7 Co C3 149.4(3) . . ? C9 Co C3 124.3(3) . . ? C4 Co C3 39.6(3) . . ? C6 Co C3 114.0(3) . . ? C2 Co C3 39.0(3) . . ? C8 Co C1 112.3(3) . . ? C7 Co C1 136.3(3) . . ? C9 Co C1 118.3(3) . . ? C4 Co C1 66.1(3) . . ? C6 Co C1 174.6(3) . . ? C2 Co C1 39.6(3) . . ? C3 Co C1 65.8(3) . . ? C8 Co C5 122.8(3) . . ? C7 Co C5 114.8(3) . . ? C9 Co C5 153.3(3) . . ? C4 Co C5 39.9(3) . . ? C6 Co C5 135.3(3) . . ? C2 Co C5 66.6(3) . . ? C3 Co C5 66.6(3) . . ? C1 Co C5 39.3(3) . . ? C22 P1 C12 87.8(2) . . ? C22 P1 P2 99.8(2) . . ? C12 P1 P2 100.5(2) . . ? C11 P2 C17 98.3(2) . . ? C11 P2 P1 94.7(2) . . ? C17 P2 P1 100.0(2) . . ? C22 P3 C17 102.1(2) . . ? C22 P3 C27 87.1(2) . . ? C17 P3 C27 87.5(2) . . ? C27 P4 C17 88.2(2) . . ? C27 P4 P5 101.7(2) . . ? C17 P4 P5 100.9(2) . . ? C12 P5 C11 101.3(2) . . ? C12 P5 P4 98.5(2) . . ? C11 P5 P4 91.0(2) . . ? C27 P6 C12 102.7(2) . . ? C27 P6 C22 87.2(2) . . ? C12 P6 C22 87.2(2) . . ? C5 C1 C2 108.6(7) . . ? C5 C1 Co 70.7(4) . . ? C2 C1 Co 69.3(4) . . ? C3 C2 C1 108.3(7) . . ? C3 C2 Co 70.9(4) . . ? C1 C2 Co 71.0(4) . . ? C2 C3 C4 108.1(7) . . ? C2 C3 Co 70.1(4) . . ? C4 C3 Co 69.6(4) . . ? C3 C4 C5 108.7(7) . . ? C3 C4 Co 70.8(4) . . ? C5 C4 Co 71.4(4) . . ? C1 C5 C4 106.3(6) . . ? C1 C5 Co 70.0(4) . . ? C4 C5 Co 68.7(4) . . ? C7 C6 C10 109.6(5) . . ? C7 C6 Co 66.4(3) . . ? C10 C6 Co 91.2(3) . . ? C8 C7 C6 106.4(5) . . ? C8 C7 Co 68.3(3) . . ? C6 C7 Co 72.0(3) . . ? C9 C8 C7 106.9(5) . . ? C9 C8 Co 71.8(3) . . ? C7 C8 Co 69.3(3) . . ? C8 C9 C10 110.0(5) . . ? C8 C9 Co 66.7(3) . . ? C10 C9 Co 92.0(3) . . ? C6 C10 C9 94.7(4) . . ? C6 C10 C11 115.3(4) . . ? C9 C10 C11 113.5(4) . . ? C10 C11 P2 114.3(3) . . ? C10 C11 P5 115.4(3) . . ? P2 C11 P5 108.3(2) . . ? C13 C12 P5 111.8(4) . . ? C13 C12 P6 110.8(3) . . ? P5 C12 P6 114.8(3) . . ? C13 C12 P1 114.8(4) . . ? P5 C12 P1 111.6(3) . . ? P6 C12 P1 91.6(2) . . ? C16 C13 C15 108.7(5) . . ? C16 C13 C14 107.6(5) . . ? C15 C13 C14 109.4(5) . . ? C16 C13 C12 111.4(5) . . ? C15 C13 C12 109.1(5) . . ? C14 C13 C12 110.5(4) . . ? C18 C17 P2 110.8(3) . . ? C18 C17 P3 112.1(3) . . ? P2 C17 P3 114.0(3) . . ? C18 C17 P4 116.2(4) . . ? P2 C17 P4 111.4(3) . . ? P3 C17 P4 91.2(2) . . ? C21 C18 C20 108.2(5) . . ? C21 C18 C19 110.8(5) . . ? C20 C18 C19 108.0(5) . . ? C21 C18 C17 109.5(4) . . ? C20 C18 C17 111.4(5) . . ? C19 C18 C17 109.0(4) . . ? C23 C22 P1 116.1(4) . . ? C23 C22 P3 113.5(4) . . ? P1 C22 P3 116.3(3) . . ? C23 C22 P6 123.0(4) . . ? P1 C22 P6 92.3(2) . . ? P3 C22 P6 92.4(2) . . ? C24 C23 C26 109.7(5) . . ? C24 C23 C25 109.9(5) . . ? C26 C23 C25 106.9(5) . . ? C24 C23 C22 108.1(5) . . ? C26 C23 C22 110.5(5) . . ? C25 C23 C22 111.7(5) . . ? C28 C27 P4 116.6(4) . . ? C28 C27 P6 114.6(4) . . ? P4 C27 P6 115.0(3) . . ? C28 C27 P3 121.8(4) . . ? P4 C27 P3 92.2(2) . . ? P6 C27 P3 92.8(2) . . ? C31 C28 C30 107.6(5) . . ? C31 C28 C29 109.9(5) . . ? C30 C28 C29 109.2(5) . . ? C31 C28 C27 111.1(5) . . ? C30 C28 C27 111.3(5) . . ? C29 C28 C27 107.8(4) . . ? _refine_diff_density_max 1.567 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.100 #===END data_sep499 _database_code_CSD 172117 _audit_creation_date 1999-09-03T11:46:36-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FO #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[(CtBu)4P6CHSiMe3]' _chemical_formula_moiety 'C24 H46 P6 Si' _chemical_formula_structural 'C24 H46 P6 Si' _chemical_formula_sum 'C24 H46 P6 Si' _chemical_formula_weight 548.52 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2274(2) _cell_length_b 12.3429(4) _cell_length_c 12.7112(4) _cell_angle_alpha 100.210(2) _cell_angle_beta 97.134(2) _cell_angle_gamma 102.000(2) _cell_volume 1522.92(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11528 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.88 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 18033 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.96 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 7193 _reflns_number_gt 5978 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXLS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The hydrogen atom on C5 was located on a difference map and freely refined; all other H atoms were in riding mode. 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^)+(0.0444P)^2^+0.3963P] 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_number_reflns 7193 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.252 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.045 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P1 P 0.30240(4) 0.35283(4) 0.31703(3) 0.03574(11) Uani 1 1 d . . . P2 P 0.32474(4) 0.18889(4) 0.23155(4) 0.03605(11) Uani 1 1 d . . . P3 P 0.11751(4) 0.14739(4) 0.39212(4) 0.03784(11) Uani 1 1 d . . . P4 P 0.01066(4) 0.10553(4) 0.17771(4) 0.03846(11) Uani 1 1 d . . . P5 P 0.09067(4) 0.25099(4) 0.10659(4) 0.03835(11) Uani 1 1 d . . . P6 P 0.04127(4) 0.33548(4) 0.34610(4) 0.03766(11) Uani 1 1 d . . . Si Si 0.38705(5) 0.26375(4) 0.01646(4) 0.04376(12) Uani 1 1 d . . . C1 C 0.19848(16) 0.30319(14) 0.41828(13) 0.0366(3) Uani 1 1 d . . . C2 C 0.17339(16) 0.09250(14) 0.26100(14) 0.0369(3) Uani 1 1 d . . . C3 C -0.03108(15) 0.17885(14) 0.30683(14) 0.0372(3) Uani 1 1 d . . . C4 C 0.13959(16) 0.36458(14) 0.23337(13) 0.0362(3) Uani 1 1 d . . . C5 C 0.25252(17) 0.20524(15) 0.09516(14) 0.0380(3) Uani 1 1 d . . . H5 H 0.223(2) 0.1312(18) 0.0561(17) 0.046(5) Uiso 1 1 d . . . C6 C 0.25795(18) 0.35734(17) 0.53944(15) 0.0457(4) Uani 1 1 d . . . C7 C 0.3832(2) 0.3132(2) 0.57013(18) 0.0648(6) Uani 1 1 d . . . H7A H 0.4489 0.3342 0.5251 0.097 Uiso 1 1 calc R . . H7B H 0.3579 0.2322 0.5597 0.097 Uiso 1 1 calc R . . H7C H 0.4216 0.3454 0.6448 0.097 Uiso 1 1 calc R . . C8 C 0.1536(2) 0.3239(2) 0.61214(17) 0.0633(6) Uani 1 1 d . . . H8A H 0.0745 0.3513 0.593 0.095 Uiso 1 1 calc R . . H8B H 0.1924 0.3565 0.6866 0.095 Uiso 1 1 calc R . . H8C H 0.1287 0.2429 0.6022 0.095 Uiso 1 1 calc R . . C9 C 0.2961(3) 0.4863(2) 0.55820(18) 0.0668(6) Uani 1 1 d . . . H9A H 0.2168 0.5133 0.5388 0.1 Uiso 1 1 calc R . . H9B H 0.3624 0.5093 0.5143 0.1 Uiso 1 1 calc R . . H9C H 0.3332 0.5174 0.6333 0.1 Uiso 1 1 calc R . . C10 C 0.19448(19) -0.03170(16) 0.25013(18) 0.0488(4) Uani 1 1 d . . . C11 C 0.2229(3) -0.07443(19) 0.1365(2) 0.0658(6) Uani 1 1 d . . . H11A H 0.3029 -0.0253 0.1241 0.099 Uiso 1 1 calc R . . H11B H 0.1472 -0.0749 0.0833 0.099 Uiso 1 1 calc R . . H11C H 0.2362 -0.1498 0.1306 0.099 Uiso 1 1 calc R . . C12 C 0.3139(2) -0.0319(2) 0.3360(2) 0.0667(6) Uani 1 1 d . . . H12A H 0.3943 0.0182 0.3255 0.1 Uiso 1 1 calc R . . H12B H 0.3277 -0.1073 0.3292 0.1 Uiso 1 1 calc R . . H12C H 0.2943 -0.0068 0.4069 0.1 Uiso 1 1 calc R . . C13 C 0.0673(2) -0.11181(18) 0.2682(2) 0.0661(6) Uani 1 1 d . . . H13A H -0.0082 -0.1125 0.2149 0.099 Uiso 1 1 calc R . . H13B H 0.0485 -0.0863 0.3393 0.099 Uiso 1 1 calc R . . H13C H 0.0819 -0.1869 0.2618 0.099 Uiso 1 1 calc R . . C14 C -0.18110(17) 0.14060(17) 0.32391(16) 0.0463(4) Uani 1 1 d . . . C15 C -0.2221(2) 0.0124(2) 0.3144(2) 0.0671(6) Uani 1 1 d . . . H15A H -0.1651 -0.0088 0.3693 0.101 Uiso 1 1 calc R . . H15B H -0.2119 -0.0253 0.2441 0.101 Uiso 1 1 calc R . . H15C H -0.3149 -0.0092 0.3238 0.101 Uiso 1 1 calc R . . C16 C -0.1996(2) 0.1976(2) 0.4369(2) 0.0635(6) Uani 1 1 d . . . H16A H -0.1744 0.2784 0.445 0.095 Uiso 1 1 calc R . . H16B H -0.1431 0.1753 0.4913 0.095 Uiso 1 1 calc R . . H16C H -0.2927 0.1748 0.4452 0.095 Uiso 1 1 calc R . . C17 C -0.2701(2) 0.1769(2) 0.2375(2) 0.0688(6) Uani 1 1 d . . . H17A H -0.2429 0.2575 0.2446 0.103 Uiso 1 1 calc R . . H17B H -0.3632 0.1561 0.2466 0.103 Uiso 1 1 calc R . . H17C H -0.2602 0.1399 0.1668 0.103 Uiso 1 1 calc R . . C18 C 0.1374(2) 0.48498(16) 0.20824(16) 0.0469(4) Uani 1 1 d . . . C19 C -0.0083(3) 0.4857(2) 0.1626(2) 0.0651(6) Uani 1 1 d . . . H19A H -0.0405 0.4276 0.0981 0.098 Uiso 1 1 calc R . . H19B H -0.0102 0.5581 0.1456 0.098 Uiso 1 1 calc R . . H19C H -0.0654 0.4718 0.2156 0.098 Uiso 1 1 calc R . . C20 C 0.1867(3) 0.57776(17) 0.31093(19) 0.0617(6) Uani 1 1 d . . . H20A H 0.1304 0.5623 0.3641 0.093 Uiso 1 1 calc R . . H20B H 0.1818 0.6497 0.294 0.093 Uiso 1 1 calc R . . H20C H 0.2788 0.5795 0.3392 0.093 Uiso 1 1 calc R . . C21 C 0.2293(3) 0.5116(2) 0.1254(2) 0.0705(7) Uani 1 1 d . . . H21A H 0.1998 0.4542 0.0602 0.106 Uiso 1 1 calc R . . H21B H 0.321 0.5132 0.1547 0.106 Uiso 1 1 calc R . . H21C H 0.2249 0.584 0.1094 0.106 Uiso 1 1 calc R . . C22 C 0.4661(3) 0.1444(2) -0.0282(2) 0.0676(6) Uani 1 1 d . . . H22A H 0.5075 0.1225 0.0343 0.101 Uiso 1 1 calc R . . H22B H 0.5339 0.1678 -0.0707 0.101 Uiso 1 1 calc R . . H22C H 0.3978 0.0812 -0.0711 0.101 Uiso 1 1 calc R . . C23 C 0.3075(2) 0.3038(2) -0.10598(18) 0.0630(6) Uani 1 1 d . . . H23A H 0.266 0.3653 -0.0843 0.094 Uiso 1 1 calc R . . H23B H 0.2398 0.2399 -0.1485 0.094 Uiso 1 1 calc R . . H23C H 0.3756 0.3268 -0.1484 0.094 Uiso 1 1 calc R . . C24 C 0.5247(2) 0.3821(2) 0.1012(2) 0.0619(5) Uani 1 1 d . . . H24A H 0.4876 0.4456 0.1256 0.093 Uiso 1 1 calc R . . H24B H 0.5932 0.404 0.0588 0.093 Uiso 1 1 calc R . . H24C H 0.564 0.3575 0.1627 0.093 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 P1 0.0333(2) 0.0361(2) 0.0362(2) 0.01012(17) 0.00276(16) 0.00419(16) P2 0.0309(2) 0.0388(2) 0.0417(2) 0.01457(18) 0.00739(16) 0.00947(16) P3 0.0323(2) 0.0424(2) 0.0413(2) 0.01660(19) 0.00646(17) 0.00746(17) P4 0.0318(2) 0.0380(2) 0.0421(2) 0.00538(18) 0.00178(17) 0.00552(16) P5 0.0390(2) 0.0420(2) 0.0339(2) 0.00885(18) 0.00063(16) 0.01154(18) P6 0.0353(2) 0.0408(2) 0.0374(2) 0.00764(18) 0.00452(16) 0.01156(17) Si 0.0468(3) 0.0477(3) 0.0381(3) 0.0122(2) 0.0112(2) 0.0090(2) C1 0.0329(7) 0.0421(9) 0.0334(8) 0.0097(7) 0.0022(6) 0.0060(6) C2 0.0323(7) 0.0348(8) 0.0455(9) 0.0130(7) 0.0066(6) 0.0081(6) C3 0.0290(7) 0.0410(9) 0.0407(9) 0.0095(7) 0.0030(6) 0.0073(6) C4 0.0380(8) 0.0348(8) 0.0365(8) 0.0089(6) 0.0027(6) 0.0106(6) C5 0.0407(8) 0.0378(9) 0.0355(9) 0.0074(7) 0.0066(7) 0.0092(7) C6 0.0419(9) 0.0558(11) 0.0344(9) 0.0084(8) -0.0011(7) 0.0057(8) C7 0.0477(11) 0.0960(18) 0.0475(12) 0.0182(11) -0.0064(9) 0.0155(11) C8 0.0598(12) 0.0888(17) 0.0381(11) 0.0093(10) 0.0112(9) 0.0119(11) C9 0.0796(15) 0.0622(14) 0.0429(11) -0.0036(10) -0.0039(10) 0.0028(11) C10 0.0456(10) 0.0372(9) 0.0702(13) 0.0204(9) 0.0151(9) 0.0132(8) C11 0.0755(15) 0.0433(11) 0.0835(17) 0.0085(11) 0.0250(12) 0.0221(10) C12 0.0571(12) 0.0581(13) 0.0987(19) 0.0398(13) 0.0123(12) 0.0244(10) C13 0.0609(13) 0.0383(11) 0.105(2) 0.0274(11) 0.0227(12) 0.0094(9) C14 0.0298(8) 0.0556(11) 0.0535(11) 0.0128(9) 0.0088(7) 0.0077(7) C15 0.0428(11) 0.0606(14) 0.0936(18) 0.0164(12) 0.0185(11) -0.0016(9) C16 0.0487(11) 0.0771(15) 0.0680(14) 0.0170(12) 0.0258(10) 0.0110(10) C17 0.0335(9) 0.0983(19) 0.0774(16) 0.0272(14) 0.0034(9) 0.0174(11) C18 0.0593(11) 0.0397(9) 0.0482(11) 0.0164(8) 0.0086(8) 0.0204(8) C19 0.0769(15) 0.0628(13) 0.0647(14) 0.0197(11) -0.0004(11) 0.0379(12) C20 0.0789(15) 0.0385(10) 0.0681(14) 0.0102(10) 0.0059(11) 0.0188(10) C21 0.0951(18) 0.0573(14) 0.0771(16) 0.0374(12) 0.0322(14) 0.0278(13) C22 0.0695(14) 0.0753(16) 0.0644(15) 0.0109(12) 0.0239(11) 0.0272(12) C23 0.0778(15) 0.0666(14) 0.0446(12) 0.0196(10) 0.0095(10) 0.0106(11) C24 0.0537(12) 0.0628(13) 0.0639(14) 0.0156(11) 0.0105(10) -0.0004(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 P1 C1 1.8735(17) . ? P1 C4 1.9078(16) . ? P1 P2 2.1913(6) . ? P2 C5 1.8600(17) . ? P2 C2 1.8675(17) . ? P3 C1 1.8807(17) . ? P3 C2 1.8871(18) . ? P3 C3 1.9029(16) . ? P4 C3 1.8716(18) . ? P4 C2 1.9107(16) . ? P4 P5 2.2042(6) . ? P5 C5 1.8707(17) . ? P5 C4 1.8761(17) . ? P6 C3 1.8724(18) . ? P6 C4 1.8930(18) . ? P6 C1 1.9014(16) . ? Si C23 1.858(2) . ? Si C22 1.860(2) . ? Si C24 1.867(2) . ? Si C5 1.8974(18) . ? C1 C6 1.556(2) . ? C2 C10 1.577(2) . ? C3 C14 1.563(2) . ? C4 C18 1.578(2) . ? C6 C9 1.525(3) . ? C6 C7 1.527(3) . ? C6 C8 1.536(3) . ? C10 C13 1.530(3) . ? C10 C11 1.532(3) . ? C10 C12 1.534(3) . ? C14 C17 1.527(3) . ? C14 C15 1.529(3) . ? C14 C16 1.536(3) . ? C18 C20 1.528(3) . ? C18 C21 1.529(3) . ? C18 C19 1.533(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C4 88.25(7) . . ? C1 P1 P2 99.19(6) . . ? C4 P1 P2 100.67(5) . . ? C5 P2 C2 98.97(8) . . ? C5 P2 P1 94.97(6) . . ? C2 P2 P1 100.39(6) . . ? C1 P3 C2 102.03(7) . . ? C1 P3 C3 86.97(7) . . ? C2 P3 C3 87.41(7) . . ? C3 P4 C2 87.63(7) . . ? C3 P4 P5 101.11(6) . . ? C2 P4 P5 100.41(5) . . ? C5 P5 C4 102.28(7) . . ? C5 P5 P4 91.48(6) . . ? C4 P5 P4 99.03(6) . . ? C3 P6 C4 102.91(8) . . ? C3 P6 C1 87.25(7) . . ? C4 P6 C1 87.87(7) . . ? C23 Si C22 108.44(12) . . ? C23 Si C24 112.15(11) . . ? C22 Si C24 107.07(11) . . ? C23 Si C5 110.37(9) . . ? C22 Si C5 105.19(10) . . ? C24 Si C5 113.22(9) . . ? C6 C1 P1 115.87(12) . . ? C6 C1 P3 114.10(12) . . ? P1 C1 P3 116.85(9) . . ? C6 C1 P6 122.15(12) . . ? P1 C1 P6 91.81(7) . . ? P3 C1 P6 92.47(7) . . ? C10 C2 P2 110.57(11) . . ? C10 C2 P3 113.57(12) . . ? P2 C2 P3 113.99(9) . . ? C10 C2 P4 115.16(12) . . ? P2 C2 P4 110.83(8) . . ? P3 C2 P4 91.62(7) . . ? C14 C3 P4 115.47(12) . . ? C14 C3 P6 114.38(12) . . ? P4 C3 P6 115.68(9) . . ? C14 C3 P3 122.92(12) . . ? P4 C3 P3 92.35(7) . . ? P6 C3 P3 92.69(7) . . ? C18 C4 P5 111.57(12) . . ? C18 C4 P6 111.48(12) . . ? P5 C4 P6 114.84(9) . . ? C18 C4 P1 116.13(12) . . ? P5 C4 P1 110.46(8) . . ? P6 C4 P1 91.01(7) . . ? P2 C5 P5 107.84(9) . . ? P2 C5 Si 113.01(9) . . ? P5 C5 Si 125.81(9) . . ? C9 C6 C7 110.03(18) . . ? C9 C6 C8 107.99(19) . . ? C7 C6 C8 109.15(17) . . ? C9 C6 C1 111.18(15) . . ? C7 C6 C1 108.01(16) . . ? C8 C6 C1 110.47(15) . . ? C13 C10 C11 108.50(19) . . ? C13 C10 C12 108.67(18) . . ? C11 C10 C12 110.05(18) . . ? C13 C10 C2 110.46(15) . . ? C11 C10 C2 109.97(16) . . ? C12 C10 C2 109.17(16) . . ? C17 C14 C15 110.67(18) . . ? C17 C14 C16 109.45(18) . . ? C15 C14 C16 107.81(18) . . ? C17 C14 C3 107.22(16) . . ? C15 C14 C3 111.02(15) . . ? C16 C14 C3 110.68(16) . . ? C20 C18 C21 108.23(19) . . ? C20 C18 C19 108.68(17) . . ? C21 C18 C19 109.42(18) . . ? C20 C18 C4 111.09(15) . . ? C21 C18 C4 110.49(15) . . ? C19 C18 C4 108.91(16) . . ? #===END