data_2_775j _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H63 P Pb Si8' _chemical_formula_weight 790.60 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Pb' 'Pb' -3.3944 10.1111 '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 9.7005(19) _cell_length_b 21.430(4) _cell_length_c 19.585(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.19(3) _cell_angle_gamma 90.00 _cell_volume 3947.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16343 _cell_measurement_theta_min 4.669 _cell_measurement_theta_max 52.574 _exptl_crystal_description blocks _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 4.569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2901 _exptl_absorpt_correction_T_max 0.4618 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30193 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7996 _reflns_number_gt 7139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution '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^)+(0.0556P)^2^+84.5800P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7996 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1617 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Pb1 Pb 0.24382(4) 0.744260(14) 0.036112(17) 0.01919(12) Uani 1 1 d . . . Si4 Si 0.2791(3) 0.65132(11) 0.13368(13) 0.0205(5) Uani 1 1 d . . . Si1 Si 0.2630(3) 0.83971(11) 0.13011(13) 0.0208(5) Uani 1 1 d . . . P1 P -0.0406(2) 0.72737(11) -0.02231(12) 0.0223(5) Uani 1 1 d . . . Si7 Si 0.3735(3) 0.56602(11) 0.08583(14) 0.0232(5) Uani 1 1 d . . . Si5 Si 0.3852(3) 0.91107(12) 0.07509(15) 0.0265(5) Uani 1 1 d . . . Si2 Si 0.4121(3) 0.80152(11) 0.23645(13) 0.0222(5) Uani 1 1 d . . . Si3 Si 0.4698(3) 0.69760(11) 0.21638(13) 0.0219(5) Uani 1 1 d . . . Si8 Si 0.1189(3) 0.60911(12) 0.19365(14) 0.0264(5) Uani 1 1 d . . . Si6 Si 0.0789(3) 0.89596(12) 0.16001(14) 0.0265(5) Uani 1 1 d . . . C2 C 0.5832(10) 0.8475(5) 0.2679(6) 0.033(2) Uani 1 1 d . . . H2A H 0.5608 0.8920 0.2696 0.050 Uiso 1 1 calc R . . H2B H 0.6440 0.8411 0.2352 0.050 Uiso 1 1 calc R . . H2C H 0.6330 0.8333 0.3150 0.050 Uiso 1 1 calc R . . C3 C 0.5248(12) 0.6533(5) 0.3017(5) 0.036(2) Uani 1 1 d . . . H3A H 0.5454 0.6099 0.2920 0.055 Uiso 1 1 calc R . . H3B H 0.4475 0.6543 0.3259 0.055 Uiso 1 1 calc R . . H3C H 0.6100 0.6725 0.3317 0.055 Uiso 1 1 calc R . . C1 C 0.3240(12) 0.8044(5) 0.3128(5) 0.035(2) Uani 1 1 d . . . H1A H 0.3861 0.7847 0.3543 0.053 Uiso 1 1 calc R . . H1B H 0.2331 0.7821 0.3001 0.053 Uiso 1 1 calc R . . H1C H 0.3072 0.8480 0.3237 0.053 Uiso 1 1 calc R . . C4 C 0.6300(10) 0.7018(5) 0.1773(6) 0.035(2) Uani 1 1 d . . . H4A H 0.7099 0.7208 0.2115 0.053 Uiso 1 1 calc R . . H4B H 0.6068 0.7272 0.1344 0.053 Uiso 1 1 calc R . . H4C H 0.6562 0.6596 0.1658 0.053 Uiso 1 1 calc R . . C5 C 0.5660(12) 0.8807(6) 0.0717(7) 0.046(3) Uani 1 1 d . . . H5A H 0.5584 0.8365 0.0584 0.069 Uiso 1 1 calc R . . H5B H 0.6319 0.8853 0.1181 0.069 Uiso 1 1 calc R . . H5C H 0.6014 0.9044 0.0368 0.069 Uiso 1 1 calc R . . C19 C -0.1842(11) 0.7418(5) 0.0213(5) 0.030(2) Uani 1 1 d . . . H19A H -0.1703 0.7138 0.0627 0.036 Uiso 1 1 calc R . . H19B H -0.1756 0.7852 0.0390 0.036 Uiso 1 1 calc R . . C17 C -0.0896(10) 0.7736(4) -0.1038(5) 0.0260(19) Uani 1 1 d . . . H17A H -0.0181 0.7668 -0.1315 0.031 Uiso 1 1 calc R . . H17B H -0.1828 0.7592 -0.1325 0.031 Uiso 1 1 calc R . . C13 C 0.2265(11) 0.5096(5) 0.0433(6) 0.034(2) Uani 1 1 d . . . H13A H 0.1487 0.5327 0.0122 0.051 Uiso 1 1 calc R . . H13B H 0.1909 0.4886 0.0800 0.051 Uiso 1 1 calc R . . H13C H 0.2639 0.4785 0.0159 0.051 Uiso 1 1 calc R . . C15 C -0.0503(10) 0.5802(5) 0.1339(5) 0.032(2) Uani 1 1 d . . . H15A H -0.1049 0.5569 0.1614 0.048 Uiso 1 1 calc R . . H15B H -0.0280 0.5528 0.0980 0.048 Uiso 1 1 calc R . . H15C H -0.1065 0.6158 0.1109 0.048 Uiso 1 1 calc R . . C20 C -0.3355(12) 0.7323(6) -0.0242(6) 0.038(2) Uani 1 1 d . . . H20A H -0.3514 0.7599 -0.0653 0.056 Uiso 1 1 calc R . . H20B H -0.4041 0.7422 0.0036 0.056 Uiso 1 1 calc R . . H20C H -0.3477 0.6888 -0.0399 0.056 Uiso 1 1 calc R . . C9 C -0.0301(11) 0.9411(5) 0.0830(6) 0.037(2) Uani 1 1 d . . . H9A H -0.0737 0.9121 0.0451 0.056 Uiso 1 1 calc R . . H9B H 0.0314 0.9704 0.0659 0.056 Uiso 1 1 calc R . . H9C H -0.1048 0.9643 0.0978 0.056 Uiso 1 1 calc R . . C10 C -0.0474(11) 0.8449(5) 0.1939(6) 0.036(2) Uani 1 1 d . . . H10A H -0.1281 0.8700 0.2000 0.054 Uiso 1 1 calc R . . H10B H 0.0020 0.8269 0.2393 0.054 Uiso 1 1 calc R . . H10C H -0.0819 0.8113 0.1601 0.054 Uiso 1 1 calc R . . C8 C 0.1572(12) 0.9543(5) 0.2315(6) 0.040(3) Uani 1 1 d . . . H8A H 0.2117 0.9857 0.2129 0.059 Uiso 1 1 calc R . . H8B H 0.2201 0.9327 0.2712 0.059 Uiso 1 1 calc R . . H8C H 0.0804 0.9748 0.2475 0.059 Uiso 1 1 calc R . . C14 C 0.2035(11) 0.5412(5) 0.2490(6) 0.038(2) Uani 1 1 d . . . H14A H 0.2982 0.5532 0.2767 0.057 Uiso 1 1 calc R . . H14B H 0.2120 0.5060 0.2183 0.057 Uiso 1 1 calc R . . H14C H 0.1444 0.5289 0.2808 0.057 Uiso 1 1 calc R . . C12 C 0.5077(11) 0.5206(5) 0.1531(5) 0.033(2) Uani 1 1 d . . . H12A H 0.5361 0.4833 0.1309 0.050 Uiso 1 1 calc R . . H12B H 0.4656 0.5081 0.1916 0.050 Uiso 1 1 calc R . . H12C H 0.5914 0.5467 0.1717 0.050 Uiso 1 1 calc R . . C11 C 0.4645(12) 0.5926(5) 0.0164(6) 0.037(2) Uani 1 1 d . . . H11A H 0.4903 0.5561 -0.0080 0.056 Uiso 1 1 calc R . . H11B H 0.5506 0.6160 0.0387 0.056 Uiso 1 1 calc R . . H11C H 0.4001 0.6194 -0.0175 0.056 Uiso 1 1 calc R . . C22 C 0.0286(13) 0.6272(5) -0.1012(6) 0.040(3) Uani 1 1 d . . . H22A H 0.0062 0.6526 -0.1441 0.061 Uiso 1 1 calc R . . H22B H 0.0125 0.5831 -0.1138 0.061 Uiso 1 1 calc R . . H22C H 0.1284 0.6334 -0.0764 0.061 Uiso 1 1 calc R . . C18 C -0.0983(12) 0.8436(5) -0.0883(6) 0.035(2) Uani 1 1 d . . . H18A H -0.1766 0.8510 -0.0658 0.053 Uiso 1 1 calc R . . H18B H -0.1151 0.8672 -0.1324 0.053 Uiso 1 1 calc R . . H18C H -0.0087 0.8573 -0.0567 0.053 Uiso 1 1 calc R . . C21 C -0.0671(11) 0.6466(4) -0.0532(5) 0.029(2) Uani 1 1 d . . . H21A H -0.0489 0.6185 -0.0119 0.035 Uiso 1 1 calc R . . H21B H -0.1677 0.6412 -0.0792 0.035 Uiso 1 1 calc R . . C6 C 0.2840(11) 0.9219(5) -0.0180(6) 0.038(2) Uani 1 1 d . . . H6A H 0.1897 0.9389 -0.0192 0.057 Uiso 1 1 calc R . . H6B H 0.2736 0.8815 -0.0424 0.057 Uiso 1 1 calc R . . H6C H 0.3355 0.9508 -0.0416 0.057 Uiso 1 1 calc R . . C16 C 0.0669(14) 0.6665(6) 0.2542(7) 0.048(3) Uani 1 1 d . . . H16A H 0.0301 0.7044 0.2279 0.072 Uiso 1 1 calc R . . H16B H 0.1501 0.6771 0.2921 0.072 Uiso 1 1 calc R . . H16C H -0.0070 0.6483 0.2744 0.072 Uiso 1 1 calc R . . C7 C 0.4094(15) 0.9901(5) 0.1176(8) 0.054(3) Uani 1 1 d . . . H7A H 0.4528 1.0184 0.0895 0.080 Uiso 1 1 calc R . . H7B H 0.4714 0.9866 0.1652 0.080 Uiso 1 1 calc R . . H7C H 0.3167 1.0066 0.1204 0.080 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 Pb1 0.02067(18) 0.01709(17) 0.01880(17) -0.00045(11) 0.00291(12) 0.00033(11) Si4 0.0226(12) 0.0167(11) 0.0226(12) -0.0009(9) 0.0066(10) -0.0008(9) Si1 0.0213(12) 0.0174(11) 0.0230(12) -0.0020(9) 0.0041(10) 0.0006(9) P1 0.0229(11) 0.0224(11) 0.0197(11) 0.0009(9) 0.0016(9) -0.0008(9) Si7 0.0253(12) 0.0166(11) 0.0274(13) -0.0011(9) 0.0060(10) 0.0008(9) Si5 0.0228(12) 0.0216(12) 0.0350(14) 0.0028(10) 0.0068(11) -0.0009(10) Si2 0.0226(12) 0.0205(12) 0.0224(12) -0.0026(9) 0.0031(10) 0.0009(9) Si3 0.0206(11) 0.0180(11) 0.0254(12) 0.0007(9) 0.0024(10) 0.0006(9) Si8 0.0267(13) 0.0262(13) 0.0277(13) 0.0016(10) 0.0095(11) -0.0028(10) Si6 0.0218(12) 0.0264(13) 0.0299(13) -0.0051(10) 0.0040(10) 0.0040(10) C2 0.028(5) 0.024(5) 0.042(6) -0.007(4) -0.002(4) -0.010(4) C3 0.042(6) 0.026(5) 0.029(5) 0.006(4) -0.014(4) -0.004(4) C1 0.048(6) 0.031(5) 0.031(5) 0.001(4) 0.017(5) 0.010(5) C4 0.027(5) 0.021(5) 0.061(7) -0.008(5) 0.017(5) 0.002(4) C5 0.031(6) 0.050(7) 0.061(8) 0.014(6) 0.019(5) 0.003(5) C19 0.036(5) 0.034(5) 0.022(5) 0.004(4) 0.008(4) 0.006(4) C17 0.028(5) 0.023(5) 0.025(4) 0.009(4) 0.003(4) 0.003(4) C13 0.036(5) 0.023(5) 0.042(6) -0.009(4) 0.007(5) -0.002(4) C15 0.027(5) 0.033(5) 0.034(5) 0.004(4) 0.006(4) -0.008(4) C20 0.034(6) 0.046(6) 0.036(6) 0.001(5) 0.015(5) -0.005(5) C9 0.035(6) 0.033(5) 0.043(6) 0.006(5) 0.009(5) 0.016(4) C10 0.030(5) 0.045(6) 0.037(6) -0.005(5) 0.016(5) 0.000(4) C8 0.042(6) 0.035(6) 0.042(6) -0.020(5) 0.010(5) 0.005(5) C14 0.032(5) 0.043(6) 0.035(6) 0.014(5) 0.004(4) -0.011(5) C12 0.034(5) 0.029(5) 0.035(5) 0.003(4) 0.006(4) 0.007(4) C11 0.048(6) 0.028(5) 0.044(6) -0.002(4) 0.028(5) 0.003(5) C22 0.055(7) 0.034(6) 0.036(6) -0.005(5) 0.020(5) -0.002(5) C18 0.044(6) 0.028(5) 0.035(5) 0.005(4) 0.013(5) 0.001(4) C21 0.034(5) 0.019(4) 0.033(5) -0.001(4) 0.006(4) -0.002(4) C6 0.034(6) 0.034(6) 0.048(6) 0.011(5) 0.011(5) -0.001(4) C16 0.051(7) 0.054(7) 0.049(7) -0.011(6) 0.032(6) -0.012(6) C7 0.069(9) 0.026(6) 0.077(9) -0.011(6) 0.037(7) -0.021(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 Pb1 Si4 2.723(2) . ? Pb1 Si1 2.728(2) . ? Pb1 P1 2.740(2) . ? Si4 Si7 2.341(3) . ? Si4 Si8 2.347(3) . ? Si4 Si3 2.358(3) . ? Si1 Si6 2.345(3) . ? Si1 Si5 2.352(4) . ? Si1 Si2 2.371(3) . ? P1 C19 1.829(10) . ? P1 C21 1.830(9) . ? P1 C17 1.840(9) . ? Si7 C12 1.880(10) . ? Si7 C11 1.881(10) . ? Si7 C13 1.899(10) . ? Si5 C6 1.862(11) . ? Si5 C7 1.877(12) . ? Si5 C5 1.887(11) . ? Si2 C2 1.898(9) . ? Si2 C1 1.898(10) . ? Si2 Si3 2.353(3) . ? Si3 C3 1.882(10) . ? Si3 C4 1.896(10) . ? Si8 C16 1.862(12) . ? Si8 C15 1.872(10) . ? Si8 C14 1.879(11) . ? Si6 C10 1.880(11) . ? Si6 C9 1.883(10) . ? Si6 C8 1.893(10) . ? C19 C20 1.532(15) . ? C17 C18 1.538(13) . ? C22 C21 1.531(14) . ? 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 Si4 Pb1 Si1 95.67(8) . . ? Si4 Pb1 P1 97.86(7) . . ? Si1 Pb1 P1 106.01(7) . . ? Si7 Si4 Si8 105.75(13) . . ? Si7 Si4 Si3 106.58(13) . . ? Si8 Si4 Si3 108.82(13) . . ? Si7 Si4 Pb1 106.53(11) . . ? Si8 Si4 Pb1 130.42(12) . . ? Si3 Si4 Pb1 96.71(10) . . ? Si6 Si1 Si5 106.29(13) . . ? Si6 Si1 Si2 107.24(13) . . ? Si5 Si1 Si2 111.04(13) . . ? Si6 Si1 Pb1 128.62(12) . . ? Si5 Si1 Pb1 97.87(11) . . ? Si2 Si1 Pb1 105.06(10) . . ? C19 P1 C21 104.7(5) . . ? C19 P1 C17 104.5(4) . . ? C21 P1 C17 103.7(5) . . ? C19 P1 Pb1 125.9(3) . . ? C21 P1 Pb1 108.0(3) . . ? C17 P1 Pb1 108.1(3) . . ? C12 Si7 C11 107.2(5) . . ? C12 Si7 C13 107.1(5) . . ? C11 Si7 C13 108.1(5) . . ? C12 Si7 Si4 113.3(3) . . ? C11 Si7 Si4 110.6(3) . . ? C13 Si7 Si4 110.3(3) . . ? C6 Si5 C7 107.5(6) . . ? C6 Si5 C5 106.2(6) . . ? C7 Si5 C5 108.1(6) . . ? C6 Si5 Si1 109.0(4) . . ? C7 Si5 Si1 113.9(4) . . ? C5 Si5 Si1 111.7(4) . . ? C2 Si2 C1 104.7(5) . . ? C2 Si2 Si3 108.7(3) . . ? C1 Si2 Si3 109.5(3) . . ? C2 Si2 Si1 113.7(4) . . ? C1 Si2 Si1 112.6(4) . . ? Si3 Si2 Si1 107.38(12) . . ? C3 Si3 C4 107.5(5) . . ? C3 Si3 Si2 110.9(4) . . ? C4 Si3 Si2 105.9(3) . . ? C3 Si3 Si4 113.7(3) . . ? C4 Si3 Si4 109.0(4) . . ? Si2 Si3 Si4 109.54(13) . . ? C16 Si8 C15 106.5(5) . . ? C16 Si8 C14 107.0(6) . . ? C15 Si8 C14 107.2(5) . . ? C16 Si8 Si4 112.3(4) . . ? C15 Si8 Si4 113.6(3) . . ? C14 Si8 Si4 109.8(4) . . ? C10 Si6 C9 107.2(5) . . ? C10 Si6 C8 107.6(5) . . ? C9 Si6 C8 107.3(5) . . ? C10 Si6 Si1 113.0(4) . . ? C9 Si6 Si1 112.1(4) . . ? C8 Si6 Si1 109.4(4) . . ? C20 C19 P1 115.9(7) . . ? C18 C17 P1 111.6(7) . . ? C22 C21 P1 113.8(7) . . ? 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 Si1 Pb1 Si4 Si7 -154.23(11) . . . . ? P1 Pb1 Si4 Si7 98.70(11) . . . . ? Si1 Pb1 Si4 Si8 77.11(16) . . . . ? P1 Pb1 Si4 Si8 -29.96(16) . . . . ? Si1 Pb1 Si4 Si3 -44.68(11) . . . . ? P1 Pb1 Si4 Si3 -151.75(10) . . . . ? Si4 Pb1 Si1 Si6 -98.25(16) . . . . ? P1 Pb1 Si1 Si6 1.63(17) . . . . ? Si4 Pb1 Si1 Si5 143.54(10) . . . . ? P1 Pb1 Si1 Si5 -116.59(10) . . . . ? Si4 Pb1 Si1 Si2 29.18(12) . . . . ? P1 Pb1 Si1 Si2 129.06(11) . . . . ? Si4 Pb1 P1 C19 67.6(4) . . . . ? Si1 Pb1 P1 C19 -30.6(4) . . . . ? Si4 Pb1 P1 C21 -56.7(3) . . . . ? Si1 Pb1 P1 C21 -154.9(3) . . . . ? Si4 Pb1 P1 C17 -168.2(3) . . . . ? Si1 Pb1 P1 C17 93.6(3) . . . . ? Si8 Si4 Si7 C12 -75.1(4) . . . . ? Si3 Si4 Si7 C12 40.6(4) . . . . ? Pb1 Si4 Si7 C12 143.1(4) . . . . ? Si8 Si4 Si7 C11 164.5(4) . . . . ? Si3 Si4 Si7 C11 -79.8(4) . . . . ? Pb1 Si4 Si7 C11 22.7(4) . . . . ? Si8 Si4 Si7 C13 45.0(4) . . . . ? Si3 Si4 Si7 C13 160.7(4) . . . . ? Pb1 Si4 Si7 C13 -96.9(4) . . . . ? Si6 Si1 Si5 C6 -79.7(4) . . . . ? Si2 Si1 Si5 C6 163.9(4) . . . . ? Pb1 Si1 Si5 C6 54.4(4) . . . . ? Si6 Si1 Si5 C7 40.4(6) . . . . ? Si2 Si1 Si5 C7 -76.0(5) . . . . ? Pb1 Si1 Si5 C7 174.5(5) . . . . ? Si6 Si1 Si5 C5 163.2(5) . . . . ? Si2 Si1 Si5 C5 46.9(5) . . . . ? Pb1 Si1 Si5 C5 -62.6(5) . . . . ? Si6 Si1 Si2 C2 -102.6(4) . . . . ? Si5 Si1 Si2 C2 13.1(4) . . . . ? Pb1 Si1 Si2 C2 117.9(4) . . . . ? Si6 Si1 Si2 C1 16.3(4) . . . . ? Si5 Si1 Si2 C1 132.0(4) . . . . ? Pb1 Si1 Si2 C1 -123.2(4) . . . . ? Si6 Si1 Si2 Si3 137.00(14) . . . . ? Si5 Si1 Si2 Si3 -107.28(15) . . . . ? Pb1 Si1 Si2 Si3 -2.48(15) . . . . ? C2 Si2 Si3 C3 78.6(6) . . . . ? C1 Si2 Si3 C3 -35.3(6) . . . . ? Si1 Si2 Si3 C3 -158.0(4) . . . . ? C2 Si2 Si3 C4 -37.7(5) . . . . ? C1 Si2 Si3 C4 -151.7(5) . . . . ? Si1 Si2 Si3 C4 85.7(4) . . . . ? C2 Si2 Si3 Si4 -155.1(4) . . . . ? C1 Si2 Si3 Si4 90.9(4) . . . . ? Si1 Si2 Si3 Si4 -31.70(17) . . . . ? Si7 Si4 Si3 C3 -76.4(4) . . . . ? Si8 Si4 Si3 C3 37.2(4) . . . . ? Pb1 Si4 Si3 C3 174.1(4) . . . . ? Si7 Si4 Si3 C4 43.5(4) . . . . ? Si8 Si4 Si3 C4 157.1(4) . . . . ? Pb1 Si4 Si3 C4 -66.0(4) . . . . ? Si7 Si4 Si3 Si2 158.96(13) . . . . ? Si8 Si4 Si3 Si2 -87.42(16) . . . . ? Pb1 Si4 Si3 Si2 49.46(14) . . . . ? Si7 Si4 Si8 C16 165.4(5) . . . . ? Si3 Si4 Si8 C16 51.2(5) . . . . ? Pb1 Si4 Si8 C16 -65.7(5) . . . . ? Si7 Si4 Si8 C15 -73.6(4) . . . . ? Si3 Si4 Si8 C15 172.2(4) . . . . ? Pb1 Si4 Si8 C15 55.3(4) . . . . ? Si7 Si4 Si8 C14 46.4(4) . . . . ? Si3 Si4 Si8 C14 -67.7(4) . . . . ? Pb1 Si4 Si8 C14 175.4(4) . . . . ? Si5 Si1 Si6 C10 172.3(4) . . . . ? Si2 Si1 Si6 C10 -68.9(4) . . . . ? Pb1 Si1 Si6 C10 57.7(4) . . . . ? Si5 Si1 Si6 C9 51.0(4) . . . . ? Si2 Si1 Si6 C9 169.9(4) . . . . ? Pb1 Si1 Si6 C9 -63.6(4) . . . . ? Si5 Si1 Si6 C8 -67.9(4) . . . . ? Si2 Si1 Si6 C8 50.9(4) . . . . ? Pb1 Si1 Si6 C8 177.5(4) . . . . ? C21 P1 C19 C20 -57.7(9) . . . . ? C17 P1 C19 C20 50.9(9) . . . . ? Pb1 P1 C19 C20 176.6(6) . . . . ? C19 P1 C17 C18 61.2(8) . . . . ? C21 P1 C17 C18 170.5(7) . . . . ? Pb1 P1 C17 C18 -75.1(7) . . . . ? C19 P1 C21 C22 171.5(8) . . . . ? C17 P1 C21 C22 62.2(9) . . . . ? Pb1 P1 C21 C22 -52.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 4.996 _refine_diff_density_min -4.551 _refine_diff_density_rms 0.232 #===END data_3_812j _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H48 B F15 Pb Si8' _chemical_formula_weight 1184.44 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.896(2) _cell_length_b 12.182(2) _cell_length_c 20.051(4) _cell_angle_alpha 81.96(3) _cell_angle_beta 74.89(3) _cell_angle_gamma 61.25(3) _cell_volume 2459.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9358 _cell_measurement_theta_min 4.954 _cell_measurement_theta_max 52.523 _exptl_crystal_description plates _exptl_crystal_colour green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 3.707 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3488 _exptl_absorpt_correction_T_max 0.6646 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19515 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9890 _reflns_number_gt 8754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution '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^)+(0.0688P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9890 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Pb1 Pb 0.454794(19) 0.093581(18) 0.259091(10) 0.01638(8) Uani 1 1 d . . . Si1 Si 0.53549(15) -0.15176(15) 0.27726(8) 0.0195(3) Uani 1 1 d . . . Si2 Si 0.73708(16) -0.23875(15) 0.19589(8) 0.0221(3) Uani 1 1 d . . . Si3 Si 0.73696(16) -0.08830(15) 0.10903(8) 0.0209(3) Uani 1 1 d . . . Si4 Si 0.65331(15) 0.10337(15) 0.16326(8) 0.0197(3) Uani 1 1 d . . . Si5 Si 0.37784(17) -0.19770(16) 0.25353(9) 0.0239(3) Uani 1 1 d . . . Si6 Si 0.56739(17) -0.22765(16) 0.38985(8) 0.0253(4) Uani 1 1 d . . . Si7 Si 0.80087(18) 0.11390(17) 0.21939(9) 0.0276(4) Uani 1 1 d . . . Si8 Si 0.59101(16) 0.26980(16) 0.08222(9) 0.0251(4) Uani 1 1 d . . . B1 B 0.2419(6) 0.2723(6) 0.2994(3) 0.0203(13) Uani 1 1 d . . . F1 F 0.4884(3) 0.2387(3) 0.33973(19) 0.0318(8) Uani 1 1 d . . . F2 F 0.4914(4) 0.3986(4) 0.4162(2) 0.0379(9) Uani 1 1 d . . . F3 F 0.2682(4) 0.6056(4) 0.4665(2) 0.0423(10) Uani 1 1 d . . . F4 F 0.0388(4) 0.6559(4) 0.4340(2) 0.0513(12) Uani 1 1 d . . . F5 F 0.0341(3) 0.5004(3) 0.3545(2) 0.0339(9) Uani 1 1 d . . . F6 F 0.3121(3) 0.1224(3) 0.41990(17) 0.0242(7) Uani 1 1 d . . . F7 F 0.1530(4) 0.0657(3) 0.52377(17) 0.0307(8) Uani 1 1 d . . . F8 F -0.0933(4) 0.1273(3) 0.51444(18) 0.0323(8) Uani 1 1 d . . . F9 F -0.1833(3) 0.2556(4) 0.40067(19) 0.0326(8) Uani 1 1 d . . . F10 F -0.0323(3) 0.3214(3) 0.29939(18) 0.0295(8) Uani 1 1 d . . . F11 F 0.1997(4) 0.1368(4) 0.21053(19) 0.0368(9) Uani 1 1 d . . . F12 F 0.1254(5) 0.2135(5) 0.0906(2) 0.0563(13) Uani 1 1 d . . . F13 F 0.1008(5) 0.4388(5) 0.0333(2) 0.0585(13) Uani 1 1 d . . . F14 F 0.1454(4) 0.5865(4) 0.1020(2) 0.0506(12) Uani 1 1 d . . . F15 F 0.2092(4) 0.5167(3) 0.22350(19) 0.0327(8) Uani 1 1 d . . . C1 C 0.7647(7) -0.3831(6) 0.1568(4) 0.0364(16) Uani 1 1 d . . . H48A H 0.8444 -0.4116 0.1196 0.055 Uiso 1 1 calc R . . H48B H 0.6891 -0.3642 0.1379 0.055 Uiso 1 1 calc R . . H48C H 0.7752 -0.4492 0.1923 0.055 Uiso 1 1 calc R . . C2 C 0.8767(6) -0.2815(6) 0.2388(3) 0.0305(14) Uani 1 1 d . . . H65A H 0.8952 -0.3603 0.2649 0.046 Uiso 1 1 calc R . . H65B H 0.8522 -0.2150 0.2703 0.046 Uiso 1 1 calc R . . H65C H 0.9554 -0.2915 0.2035 0.046 Uiso 1 1 calc R . . C3 C 0.6276(7) -0.0739(6) 0.0520(3) 0.0339(15) Uani 1 1 d . . . H47A H 0.6412 -0.0252 0.0102 0.051 Uiso 1 1 calc R . . H47B H 0.5354 -0.0313 0.0769 0.051 Uiso 1 1 calc R . . H47C H 0.6490 -0.1575 0.0390 0.051 Uiso 1 1 calc R . . C4 C 0.9063(6) -0.1399(6) 0.0536(3) 0.0317(15) Uani 1 1 d . . . H25A H 0.9356 -0.2192 0.0318 0.048 Uiso 1 1 calc R . . H25B H 0.9668 -0.1515 0.0822 0.048 Uiso 1 1 calc R . . H25C H 0.9053 -0.0761 0.0178 0.048 Uiso 1 1 calc R . . C5 C 0.3678(7) -0.1701(7) 0.1610(3) 0.0329(15) Uani 1 1 d . . . H49A H 0.3083 -0.1986 0.1528 0.049 Uiso 1 1 calc R . . H49B H 0.4555 -0.2168 0.1317 0.049 Uiso 1 1 calc R . . H49C H 0.3343 -0.0805 0.1498 0.049 Uiso 1 1 calc R . . C6 C 0.4352(7) -0.3692(6) 0.2743(4) 0.0383(16) Uani 1 1 d . . . H51A H 0.3746 -0.3944 0.2642 0.057 Uiso 1 1 calc R . . H51B H 0.4372 -0.3847 0.3234 0.057 Uiso 1 1 calc R . . H51C H 0.5237 -0.4179 0.2462 0.057 Uiso 1 1 calc R . . C7 C 0.2106(6) -0.1084(6) 0.3094(3) 0.0302(14) Uani 1 1 d . . . H50A H 0.1808 -0.0184 0.3015 0.045 Uiso 1 1 calc R . . H50B H 0.2143 -0.1293 0.3581 0.045 Uiso 1 1 calc R . . H50C H 0.1489 -0.1307 0.2980 0.045 Uiso 1 1 calc R . . C8 C 0.4072(7) -0.1973(6) 0.4503(3) 0.0337(15) Uani 1 1 d . . . H26A H 0.4219 -0.2289 0.4966 0.051 Uiso 1 1 calc R . . H26B H 0.3676 -0.2399 0.4340 0.051 Uiso 1 1 calc R . . H26C H 0.3478 -0.1070 0.4520 0.051 Uiso 1 1 calc R . . C9 C 0.6775(7) -0.4010(7) 0.3838(4) 0.0425(18) Uani 1 1 d . . . H28A H 0.7627 -0.4174 0.3530 0.064 Uiso 1 1 calc R . . H28B H 0.6369 -0.4400 0.3653 0.064 Uiso 1 1 calc R . . H28C H 0.6905 -0.4362 0.4298 0.064 Uiso 1 1 calc R . . C10 C 0.6450(8) -0.1533(8) 0.4244(4) 0.050(2) Uani 1 1 d . . . H27A H 0.5891 -0.0624 0.4259 0.074 Uiso 1 1 calc R . . H27B H 0.7316 -0.1726 0.3945 0.074 Uiso 1 1 calc R . . H27C H 0.6553 -0.1859 0.4712 0.074 Uiso 1 1 calc R . . C11 C 0.8003(7) 0.0419(7) 0.3083(4) 0.0385(16) Uani 1 1 d . . . H21A H 0.8750 0.0346 0.3241 0.058 Uiso 1 1 calc R . . H21B H 0.8074 -0.0414 0.3074 0.058 Uiso 1 1 calc R . . H21C H 0.7181 0.0950 0.3401 0.058 Uiso 1 1 calc R . . C12 C 0.9720(7) 0.0292(9) 0.1659(4) 0.049(2) Uani 1 1 d . . . H20A H 0.9730 0.0566 0.1175 0.074 Uiso 1 1 calc R . . H20B H 1.0013 -0.0612 0.1696 0.074 Uiso 1 1 calc R . . H20C H 1.0313 0.0478 0.1827 0.074 Uiso 1 1 calc R . . C13 C 0.7582(9) 0.2803(7) 0.2247(5) 0.055(2) Uani 1 1 d . . . H19A H 0.8145 0.2867 0.2503 0.082 Uiso 1 1 calc R . . H19B H 0.6659 0.3271 0.2485 0.082 Uiso 1 1 calc R . . H19C H 0.7716 0.3152 0.1779 0.082 Uiso 1 1 calc R . . C14 C 0.7433(7) 0.2474(8) 0.0155(4) 0.053(2) Uani 1 1 d . . . H23A H 0.7204 0.3136 -0.0201 0.079 Uiso 1 1 calc R . . H23B H 0.7835 0.1656 -0.0059 0.079 Uiso 1 1 calc R . . H23C H 0.8058 0.2514 0.0374 0.079 Uiso 1 1 calc R . . C15 C 0.5128(7) 0.4281(6) 0.1208(4) 0.0412(17) Uani 1 1 d . . . H22A H 0.4625 0.4916 0.0897 0.062 Uiso 1 1 calc R . . H22B H 0.5812 0.4458 0.1275 0.062 Uiso 1 1 calc R . . H22C H 0.4536 0.4299 0.1655 0.062 Uiso 1 1 calc R . . C16 C 0.4743(6) 0.2641(6) 0.0368(3) 0.0315(14) Uani 1 1 d . . . H24A H 0.4047 0.2528 0.0710 0.047 Uiso 1 1 calc R . . H24B H 0.5222 0.1938 0.0049 0.047 Uiso 1 1 calc R . . H24C H 0.4350 0.3426 0.0109 0.047 Uiso 1 1 calc R . . C17 C 0.2608(6) 0.3646(5) 0.3420(3) 0.0196(12) Uani 1 1 d . . . C18 C 0.3723(6) 0.3437(5) 0.3604(3) 0.0231(12) Uani 1 1 d . . . C19 C 0.3779(6) 0.4215(6) 0.4020(3) 0.0257(13) Uani 1 1 d . . . C20 C 0.2646(7) 0.5276(6) 0.4271(3) 0.0306(15) Uani 1 1 d . . . C21 C 0.1499(7) 0.5524(6) 0.4107(4) 0.0340(15) Uani 1 1 d . . . C22 C 0.1514(6) 0.4709(6) 0.3688(3) 0.0270(13) Uani 1 1 d . . . C23 C 0.1490(5) 0.2213(5) 0.3535(3) 0.0203(12) Uani 1 1 d . . . C24 C 0.1893(6) 0.1559(5) 0.4126(3) 0.0205(12) Uani 1 1 d . . . C25 C 0.1110(6) 0.1244(5) 0.4671(3) 0.0235(13) Uani 1 1 d . . . C26 C -0.0143(6) 0.1566(6) 0.4622(3) 0.0267(13) Uani 1 1 d . . . C27 C -0.0601(6) 0.2213(6) 0.4052(3) 0.0233(12) Uani 1 1 d . . . C28 C 0.0216(6) 0.2530(5) 0.3526(3) 0.0218(12) Uani 1 1 d . . . C29 C 0.2043(6) 0.3235(6) 0.2248(3) 0.0230(12) Uani 1 1 d . . . C30 C 0.1903(6) 0.4365(6) 0.1930(3) 0.0282(14) Uani 1 1 d . . . C31 C 0.1564(6) 0.4768(6) 0.1294(3) 0.0346(16) Uani 1 1 d . . . C32 C 0.1327(7) 0.4019(7) 0.0955(3) 0.0393(18) Uani 1 1 d . . . C33 C 0.1456(7) 0.2878(7) 0.1235(3) 0.0379(17) Uani 1 1 d . . . C34 C 0.1831(6) 0.2517(6) 0.1859(3) 0.0299(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 Pb1 0.01825(12) 0.01862(12) 0.01567(12) -0.00207(7) -0.00232(8) -0.01147(9) Si1 0.0230(8) 0.0202(8) 0.0178(8) -0.0012(6) -0.0022(6) -0.0128(7) Si2 0.0239(8) 0.0215(8) 0.0205(8) -0.0017(6) -0.0028(7) -0.0109(7) Si3 0.0211(8) 0.0260(9) 0.0180(8) -0.0013(6) -0.0034(6) -0.0132(7) Si4 0.0220(8) 0.0246(8) 0.0181(8) 0.0001(6) -0.0026(6) -0.0162(7) Si5 0.0272(9) 0.0275(9) 0.0231(8) -0.0040(7) -0.0032(7) -0.0178(7) Si6 0.0289(9) 0.0299(9) 0.0197(8) 0.0030(7) -0.0056(7) -0.0166(8) Si7 0.0321(9) 0.0345(10) 0.0288(9) 0.0020(7) -0.0116(8) -0.0235(8) Si8 0.0234(8) 0.0264(9) 0.0270(9) 0.0043(7) -0.0034(7) -0.0152(7) B1 0.021(3) 0.019(3) 0.023(3) -0.001(3) -0.005(3) -0.011(3) F1 0.0237(18) 0.035(2) 0.037(2) -0.0110(16) -0.0072(16) -0.0116(16) F2 0.044(2) 0.043(2) 0.042(2) -0.0022(18) -0.0215(19) -0.026(2) F3 0.064(3) 0.033(2) 0.043(2) -0.0121(18) -0.015(2) -0.029(2) F4 0.048(3) 0.033(2) 0.062(3) -0.027(2) -0.008(2) -0.006(2) F5 0.0235(19) 0.028(2) 0.044(2) -0.0125(17) -0.0075(16) -0.0048(16) F6 0.0251(18) 0.0285(18) 0.0230(17) 0.0010(14) -0.0073(14) -0.0149(15) F7 0.040(2) 0.034(2) 0.0191(18) 0.0046(15) -0.0038(15) -0.0203(18) F8 0.034(2) 0.032(2) 0.030(2) -0.0044(15) 0.0113(16) -0.0223(17) F9 0.0242(19) 0.043(2) 0.038(2) -0.0058(17) -0.0010(16) -0.0237(17) F10 0.0252(19) 0.040(2) 0.0279(19) 0.0020(16) -0.0090(15) -0.0178(17) F11 0.058(3) 0.041(2) 0.026(2) -0.0028(16) -0.0099(18) -0.033(2) F12 0.072(3) 0.093(4) 0.029(2) -0.009(2) -0.017(2) -0.053(3) F13 0.055(3) 0.086(4) 0.021(2) 0.012(2) -0.0182(19) -0.021(3) F14 0.047(3) 0.042(2) 0.039(2) 0.020(2) -0.004(2) -0.011(2) F15 0.039(2) 0.0251(19) 0.034(2) 0.0053(15) -0.0064(17) -0.0178(17) C1 0.042(4) 0.030(4) 0.034(4) -0.012(3) 0.003(3) -0.016(3) C2 0.022(3) 0.036(4) 0.028(3) -0.002(3) -0.004(3) -0.009(3) C3 0.044(4) 0.031(4) 0.035(4) -0.002(3) -0.019(3) -0.019(3) C4 0.022(3) 0.039(4) 0.029(3) -0.005(3) 0.002(3) -0.013(3) C5 0.035(4) 0.044(4) 0.026(3) -0.006(3) -0.007(3) -0.020(3) C6 0.045(4) 0.030(4) 0.050(4) -0.002(3) -0.009(3) -0.026(3) C7 0.028(3) 0.043(4) 0.023(3) 0.000(3) -0.004(3) -0.021(3) C8 0.037(4) 0.036(4) 0.024(3) -0.001(3) 0.004(3) -0.019(3) C9 0.046(4) 0.035(4) 0.038(4) 0.011(3) -0.007(3) -0.016(3) C10 0.067(5) 0.082(6) 0.032(4) 0.002(4) -0.017(4) -0.058(5) C11 0.048(4) 0.040(4) 0.033(4) 0.006(3) -0.017(3) -0.023(4) C12 0.034(4) 0.089(6) 0.037(4) -0.003(4) -0.008(3) -0.037(4) C13 0.086(6) 0.047(5) 0.064(6) 0.010(4) -0.047(5) -0.044(5) C14 0.038(4) 0.061(5) 0.054(5) 0.025(4) -0.002(4) -0.029(4) C15 0.042(4) 0.026(4) 0.061(5) -0.001(3) -0.019(4) -0.017(3) C16 0.034(4) 0.032(4) 0.025(3) 0.001(3) -0.010(3) -0.012(3) C17 0.024(3) 0.020(3) 0.019(3) 0.001(2) -0.006(2) -0.014(2) C18 0.029(3) 0.020(3) 0.024(3) 0.000(2) -0.004(2) -0.015(3) C19 0.037(4) 0.032(3) 0.022(3) 0.004(3) -0.011(3) -0.025(3) C20 0.049(4) 0.026(3) 0.029(3) -0.002(3) -0.008(3) -0.027(3) C21 0.038(4) 0.028(4) 0.035(4) -0.014(3) 0.000(3) -0.015(3) C22 0.029(3) 0.026(3) 0.032(3) 0.003(3) -0.010(3) -0.016(3) C23 0.021(3) 0.019(3) 0.022(3) -0.006(2) 0.000(2) -0.011(2) C24 0.023(3) 0.023(3) 0.018(3) -0.006(2) 0.000(2) -0.014(3) C25 0.035(3) 0.019(3) 0.016(3) -0.002(2) -0.002(2) -0.013(3) C26 0.031(3) 0.023(3) 0.024(3) -0.008(2) 0.006(3) -0.015(3) C27 0.023(3) 0.025(3) 0.024(3) -0.009(2) 0.001(2) -0.014(3) C28 0.028(3) 0.023(3) 0.020(3) -0.006(2) -0.002(2) -0.017(3) C29 0.021(3) 0.031(3) 0.017(3) 0.000(2) 0.001(2) -0.015(3) C30 0.021(3) 0.024(3) 0.033(3) -0.001(3) -0.002(3) -0.007(3) C31 0.025(3) 0.034(4) 0.029(4) 0.009(3) -0.002(3) -0.006(3) C32 0.028(4) 0.058(5) 0.017(3) 0.008(3) -0.007(3) -0.009(3) C33 0.031(4) 0.060(5) 0.026(3) -0.004(3) -0.007(3) -0.023(4) C34 0.031(3) 0.041(4) 0.022(3) -0.002(3) -0.002(3) -0.022(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 Pb1 B1 2.434(7) . ? Pb1 Si1 2.6654(17) . ? Pb1 Si4 2.6691(18) . ? Si1 Si2 2.353(2) . ? Si1 Si5 2.368(2) . ? Si1 Si6 2.371(2) . ? Si2 C1 1.874(7) . ? Si2 C2 1.887(6) . ? Si2 Si3 2.345(2) . ? Si3 C4 1.870(6) . ? Si3 C3 1.879(6) . ? Si3 Si4 2.353(2) . ? Si4 Si8 2.358(2) . ? Si4 Si7 2.377(2) . ? Si5 C5 1.864(6) . ? Si5 C7 1.870(6) . ? Si5 C6 1.881(7) . ? Si6 C10 1.862(7) . ? Si6 C8 1.866(6) . ? Si6 C9 1.876(7) . ? Si7 C13 1.849(8) . ? Si7 C12 1.873(8) . ? Si7 C11 1.874(7) . ? Si8 C15 1.871(7) . ? Si8 C14 1.874(7) . ? Si8 C16 1.880(7) . ? B1 C23 1.622(8) . ? B1 C29 1.626(9) . ? B1 C17 1.630(8) . ? F1 C18 1.366(7) . ? F2 C19 1.342(7) . ? F3 C20 1.340(7) . ? F4 C21 1.340(8) . ? F5 C22 1.363(7) . ? F6 C24 1.359(6) . ? F7 C25 1.332(7) . ? F8 C26 1.347(7) . ? F9 C27 1.342(7) . ? F10 C28 1.355(7) . ? F11 C34 1.355(7) . ? F12 C33 1.331(8) . ? F13 C32 1.351(7) . ? F14 C31 1.329(8) . ? F15 C30 1.352(7) . ? C17 C18 1.365(8) . ? C17 C22 1.367(8) . ? C18 C19 1.381(8) . ? C19 C20 1.376(9) . ? C20 C21 1.368(10) . ? C21 C22 1.378(9) . ? C23 C28 1.377(8) . ? C23 C24 1.390(8) . ? C24 C25 1.381(8) . ? C25 C26 1.375(9) . ? C26 C27 1.372(9) . ? C27 C28 1.386(8) . ? C29 C30 1.385(8) . ? C29 C34 1.395(9) . ? C30 C31 1.390(9) . ? C31 C32 1.378(11) . ? C32 C33 1.375(11) . ? C33 C34 1.380(9) . ? 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 B1 Pb1 Si1 131.06(16) . . ? B1 Pb1 Si4 125.26(16) . . ? Si1 Pb1 Si4 102.80(6) . . ? Si2 Si1 Si5 112.36(9) . . ? Si2 Si1 Si6 110.21(9) . . ? Si5 Si1 Si6 108.73(9) . . ? Si2 Si1 Pb1 102.77(8) . . ? Si5 Si1 Pb1 108.57(8) . . ? Si6 Si1 Pb1 114.17(8) . . ? C1 Si2 C2 108.5(3) . . ? C1 Si2 Si3 109.8(2) . . ? C2 Si2 Si3 108.4(2) . . ? C1 Si2 Si1 111.6(2) . . ? C2 Si2 Si1 109.9(2) . . ? Si3 Si2 Si1 108.63(9) . . ? C4 Si3 C3 107.4(3) . . ? C4 Si3 Si2 110.1(2) . . ? C3 Si3 Si2 108.9(2) . . ? C4 Si3 Si4 113.0(2) . . ? C3 Si3 Si4 109.9(2) . . ? Si2 Si3 Si4 107.62(8) . . ? Si3 Si4 Si8 109.93(9) . . ? Si3 Si4 Si7 114.05(9) . . ? Si8 Si4 Si7 109.53(9) . . ? Si3 Si4 Pb1 99.23(7) . . ? Si8 Si4 Pb1 115.13(8) . . ? Si7 Si4 Pb1 108.78(7) . . ? C5 Si5 C7 109.5(3) . . ? C5 Si5 C6 108.4(3) . . ? C7 Si5 C6 108.0(3) . . ? C5 Si5 Si1 112.6(2) . . ? C7 Si5 Si1 112.3(2) . . ? C6 Si5 Si1 105.8(2) . . ? C10 Si6 C8 108.7(3) . . ? C10 Si6 C9 109.5(4) . . ? C8 Si6 C9 109.1(3) . . ? C10 Si6 Si1 111.8(3) . . ? C8 Si6 Si1 110.4(2) . . ? C9 Si6 Si1 107.2(2) . . ? C13 Si7 C12 108.9(4) . . ? C13 Si7 C11 108.9(4) . . ? C12 Si7 C11 107.5(4) . . ? C13 Si7 Si4 108.4(3) . . ? C12 Si7 Si4 108.5(2) . . ? C11 Si7 Si4 114.5(2) . . ? C15 Si8 C14 109.1(4) . . ? C15 Si8 C16 108.5(3) . . ? C14 Si8 C16 107.4(4) . . ? C15 Si8 Si4 113.7(3) . . ? C14 Si8 Si4 107.3(3) . . ? C16 Si8 Si4 110.6(2) . . ? C23 B1 C29 116.7(5) . . ? C23 B1 C17 106.9(5) . . ? C29 B1 C17 116.9(5) . . ? C23 B1 Pb1 108.2(4) . . ? C29 B1 Pb1 98.2(4) . . ? C17 B1 Pb1 109.2(4) . . ? C18 C17 C22 114.2(5) . . ? C18 C17 B1 127.7(5) . . ? C22 C17 B1 117.9(5) . . ? C17 C18 F1 121.0(5) . . ? C17 C18 C19 124.3(6) . . ? F1 C18 C19 114.7(5) . . ? F2 C19 C20 119.4(5) . . ? F2 C19 C18 121.7(6) . . ? C20 C19 C18 118.8(6) . . ? F3 C20 C21 121.0(6) . . ? F3 C20 C19 119.9(6) . . ? C21 C20 C19 119.1(6) . . ? F4 C21 C20 120.1(6) . . ? F4 C21 C22 120.8(6) . . ? C20 C21 C22 119.0(6) . . ? F5 C22 C17 119.2(5) . . ? F5 C22 C21 116.3(6) . . ? C17 C22 C21 124.5(6) . . ? C28 C23 C24 114.4(5) . . ? C28 C23 B1 125.6(5) . . ? C24 C23 B1 119.2(5) . . ? F6 C24 C25 115.9(5) . . ? F6 C24 C23 119.5(5) . . ? C25 C24 C23 124.5(5) . . ? F7 C25 C26 119.9(5) . . ? F7 C25 C24 122.1(6) . . ? C26 C25 C24 118.0(5) . . ? F8 C26 C27 120.0(6) . . ? F8 C26 C25 119.6(6) . . ? C27 C26 C25 120.3(5) . . ? F9 C27 C26 120.7(5) . . ? F9 C27 C28 120.1(5) . . ? C26 C27 C28 119.3(6) . . ? F10 C28 C23 120.7(5) . . ? F10 C28 C27 115.9(5) . . ? C23 C28 C27 123.4(6) . . ? C30 C29 C34 113.0(5) . . ? C30 C29 B1 126.4(5) . . ? C34 C29 B1 120.6(5) . . ? F15 C30 C29 120.6(6) . . ? F15 C30 C31 115.1(6) . . ? C29 C30 C31 124.3(6) . . ? F14 C31 C32 120.4(6) . . ? F14 C31 C30 120.8(7) . . ? C32 C31 C30 118.8(6) . . ? F13 C32 C33 119.8(7) . . ? F13 C32 C31 119.8(7) . . ? C33 C32 C31 120.4(6) . . ? F12 C33 C32 120.9(6) . . ? F12 C33 C34 121.1(7) . . ? C32 C33 C34 117.9(7) . . ? F11 C34 C33 116.2(6) . . ? F11 C34 C29 118.3(5) . . ? C33 C34 C29 125.5(6) . . ? 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 B1 Pb1 Si1 Si2 166.7(2) . . . . ? Si4 Pb1 Si1 Si2 -2.75(8) . . . . ? B1 Pb1 Si1 Si5 47.6(2) . . . . ? Si4 Pb1 Si1 Si5 -121.93(7) . . . . ? B1 Pb1 Si1 Si6 -73.9(2) . . . . ? Si4 Pb1 Si1 Si6 116.60(8) . . . . ? Si5 Si1 Si2 C1 -27.6(3) . . . . ? Si6 Si1 Si2 C1 93.8(3) . . . . ? Pb1 Si1 Si2 C1 -144.1(3) . . . . ? Si5 Si1 Si2 C2 -147.9(2) . . . . ? Si6 Si1 Si2 C2 -26.5(2) . . . . ? Pb1 Si1 Si2 C2 95.6(2) . . . . ? Si5 Si1 Si2 Si3 93.62(10) . . . . ? Si6 Si1 Si2 Si3 -144.96(9) . . . . ? Pb1 Si1 Si2 Si3 -22.89(9) . . . . ? C1 Si2 Si3 C4 -69.6(3) . . . . ? C2 Si2 Si3 C4 48.8(3) . . . . ? Si1 Si2 Si3 C4 168.1(2) . . . . ? C1 Si2 Si3 C3 47.9(3) . . . . ? C2 Si2 Si3 C3 166.2(3) . . . . ? Si1 Si2 Si3 C3 -74.4(3) . . . . ? C1 Si2 Si3 Si4 166.9(3) . . . . ? C2 Si2 Si3 Si4 -74.8(2) . . . . ? Si1 Si2 Si3 Si4 44.58(11) . . . . ? C4 Si3 Si4 Si8 74.8(2) . . . . ? C3 Si3 Si4 Si8 -45.0(3) . . . . ? Si2 Si3 Si4 Si8 -163.41(8) . . . . ? C4 Si3 Si4 Si7 -48.7(3) . . . . ? C3 Si3 Si4 Si7 -168.5(2) . . . . ? Si2 Si3 Si4 Si7 73.14(11) . . . . ? C4 Si3 Si4 Pb1 -164.1(2) . . . . ? C3 Si3 Si4 Pb1 76.1(2) . . . . ? Si2 Si3 Si4 Pb1 -42.31(9) . . . . ? B1 Pb1 Si4 Si3 -144.0(2) . . . . ? Si1 Pb1 Si4 Si3 26.33(7) . . . . ? B1 Pb1 Si4 Si8 -26.7(2) . . . . ? Si1 Pb1 Si4 Si8 143.56(8) . . . . ? B1 Pb1 Si4 Si7 96.6(2) . . . . ? Si1 Pb1 Si4 Si7 -93.10(8) . . . . ? Si2 Si1 Si5 C5 -46.8(3) . . . . ? Si6 Si1 Si5 C5 -169.1(2) . . . . ? Pb1 Si1 Si5 C5 66.2(3) . . . . ? Si2 Si1 Si5 C7 -171.0(2) . . . . ? Si6 Si1 Si5 C7 66.7(2) . . . . ? Pb1 Si1 Si5 C7 -58.0(2) . . . . ? Si2 Si1 Si5 C6 71.4(3) . . . . ? Si6 Si1 Si5 C6 -50.9(3) . . . . ? Pb1 Si1 Si5 C6 -175.6(2) . . . . ? Si2 Si1 Si6 C10 74.9(3) . . . . ? Si5 Si1 Si6 C10 -161.5(3) . . . . ? Pb1 Si1 Si6 C10 -40.1(3) . . . . ? Si2 Si1 Si6 C8 -163.9(2) . . . . ? Si5 Si1 Si6 C8 -40.3(3) . . . . ? Pb1 Si1 Si6 C8 81.1(3) . . . . ? Si2 Si1 Si6 C9 -45.1(3) . . . . ? Si5 Si1 Si6 C9 78.5(3) . . . . ? Pb1 Si1 Si6 C9 -160.1(3) . . . . ? Si3 Si4 Si7 C13 155.3(3) . . . . ? Si8 Si4 Si7 C13 31.6(3) . . . . ? Pb1 Si4 Si7 C13 -95.0(3) . . . . ? Si3 Si4 Si7 C12 37.1(3) . . . . ? Si8 Si4 Si7 C12 -86.5(3) . . . . ? Pb1 Si4 Si7 C12 146.8(3) . . . . ? Si3 Si4 Si7 C11 -82.9(3) . . . . ? Si8 Si4 Si7 C11 153.4(3) . . . . ? Pb1 Si4 Si7 C11 26.8(3) . . . . ? Si3 Si4 Si8 C15 176.3(3) . . . . ? Si7 Si4 Si8 C15 -57.7(3) . . . . ? Pb1 Si4 Si8 C15 65.3(3) . . . . ? Si3 Si4 Si8 C14 -63.0(3) . . . . ? Si7 Si4 Si8 C14 63.0(3) . . . . ? Pb1 Si4 Si8 C14 -174.0(3) . . . . ? Si3 Si4 Si8 C16 53.9(2) . . . . ? Si7 Si4 Si8 C16 180.0(2) . . . . ? Pb1 Si4 Si8 C16 -57.1(2) . . . . ? Si1 Pb1 B1 C23 8.6(5) . . . . ? Si4 Pb1 B1 C23 176.1(3) . . . . ? Si1 Pb1 B1 C29 -113.0(3) . . . . ? Si4 Pb1 B1 C29 54.4(4) . . . . ? Si1 Pb1 B1 C17 124.7(3) . . . . ? Si4 Pb1 B1 C17 -67.9(4) . . . . ? C23 B1 C17 C18 110.2(6) . . . . ? C29 B1 C17 C18 -116.9(6) . . . . ? Pb1 B1 C17 C18 -6.7(7) . . . . ? C23 B1 C17 C22 -63.2(7) . . . . ? C29 B1 C17 C22 69.7(7) . . . . ? Pb1 B1 C17 C22 179.9(4) . . . . ? C22 C17 C18 F1 177.5(5) . . . . ? B1 C17 C18 F1 4.0(9) . . . . ? C22 C17 C18 C19 -0.3(9) . . . . ? B1 C17 C18 C19 -173.9(6) . . . . ? C17 C18 C19 F2 -177.5(5) . . . . ? F1 C18 C19 F2 4.6(8) . . . . ? C17 C18 C19 C20 0.0(9) . . . . ? F1 C18 C19 C20 -177.9(5) . . . . ? F2 C19 C20 F3 -1.2(9) . . . . ? C18 C19 C20 F3 -178.8(5) . . . . ? F2 C19 C20 C21 178.0(6) . . . . ? C18 C19 C20 C21 0.4(9) . . . . ? F3 C20 C21 F4 -0.1(10) . . . . ? C19 C20 C21 F4 -179.3(6) . . . . ? F3 C20 C21 C22 178.6(6) . . . . ? C19 C20 C21 C22 -0.5(10) . . . . ? C18 C17 C22 F5 -179.3(5) . . . . ? B1 C17 C22 F5 -5.1(8) . . . . ? C18 C17 C22 C21 0.2(9) . . . . ? B1 C17 C22 C21 174.4(6) . . . . ? F4 C21 C22 F5 -1.5(9) . . . . ? C20 C21 C22 F5 179.7(6) . . . . ? F4 C21 C22 C17 178.9(6) . . . . ? C20 C21 C22 C17 0.2(10) . . . . ? C29 B1 C23 C28 -22.4(8) . . . . ? C17 B1 C23 C28 110.6(6) . . . . ? Pb1 B1 C23 C28 -131.8(5) . . . . ? C29 B1 C23 C24 168.4(5) . . . . ? C17 B1 C23 C24 -58.5(6) . . . . ? Pb1 B1 C23 C24 59.1(6) . . . . ? C28 C23 C24 F6 -178.4(5) . . . . ? B1 C23 C24 F6 -8.1(8) . . . . ? C28 C23 C24 C25 -0.5(8) . . . . ? B1 C23 C24 C25 169.8(5) . . . . ? F6 C24 C25 F7 0.6(8) . . . . ? C23 C24 C25 F7 -177.4(5) . . . . ? F6 C24 C25 C26 179.9(5) . . . . ? C23 C24 C25 C26 1.9(9) . . . . ? F7 C25 C26 F8 -0.7(8) . . . . ? C24 C25 C26 F8 180.0(5) . . . . ? F7 C25 C26 C27 177.5(5) . . . . ? C24 C25 C26 C27 -1.8(9) . . . . ? F8 C26 C27 F9 -0.3(8) . . . . ? C25 C26 C27 F9 -178.5(5) . . . . ? F8 C26 C27 C28 178.7(5) . . . . ? C25 C26 C27 C28 0.5(9) . . . . ? C24 C23 C28 F10 177.2(5) . . . . ? B1 C23 C28 F10 7.7(9) . . . . ? C24 C23 C28 C27 -1.0(8) . . . . ? B1 C23 C28 C27 -170.5(5) . . . . ? F9 C27 C28 F10 1.7(8) . . . . ? C26 C27 C28 F10 -177.3(5) . . . . ? F9 C27 C28 C23 180.0(5) . . . . ? C26 C27 C28 C23 1.0(9) . . . . ? C23 B1 C29 C30 130.3(6) . . . . ? C17 B1 C29 C30 1.9(9) . . . . ? Pb1 B1 C29 C30 -114.6(6) . . . . ? C23 B1 C29 C34 -50.0(8) . . . . ? C17 B1 C29 C34 -178.3(5) . . . . ? Pb1 B1 C29 C34 65.2(6) . . . . ? C34 C29 C30 F15 -179.2(5) . . . . ? B1 C29 C30 F15 0.6(9) . . . . ? C34 C29 C30 C31 1.0(9) . . . . ? B1 C29 C30 C31 -179.2(6) . . . . ? F15 C30 C31 F14 0.5(9) . . . . ? C29 C30 C31 F14 -179.7(6) . . . . ? F15 C30 C31 C32 -178.6(6) . . . . ? C29 C30 C31 C32 1.2(10) . . . . ? F14 C31 C32 F13 1.4(10) . . . . ? C30 C31 C32 F13 -179.4(6) . . . . ? F14 C31 C32 C33 179.3(6) . . . . ? C30 C31 C32 C33 -1.6(10) . . . . ? F13 C32 C33 F12 -0.8(10) . . . . ? C31 C32 C33 F12 -178.7(6) . . . . ? F13 C32 C33 C34 177.6(6) . . . . ? C31 C32 C33 C34 -0.2(10) . . . . ? F12 C33 C34 F11 0.8(10) . . . . ? C32 C33 C34 F11 -177.6(6) . . . . ? F12 C33 C34 C29 -178.8(6) . . . . ? C32 C33 C34 C29 2.8(10) . . . . ? C30 C29 C34 F11 177.3(5) . . . . ? B1 C29 C34 F11 -2.5(8) . . . . ? C30 C29 C34 C33 -3.1(9) . . . . ? B1 C29 C34 C33 177.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 4.361 _refine_diff_density_min -1.771 _refine_diff_density_rms 0.182 #===END data_4_790j _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H96 Pb2 Si16' _chemical_formula_weight 1344.91 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.913(3) _cell_length_b 18.062(4) _cell_length_c 23.793(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.49(3) _cell_angle_gamma 90.00 _cell_volume 6764(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7158 _cell_measurement_theta_min 4.797 _cell_measurement_theta_max 52.335 _exptl_crystal_description blocks _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 5.274 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2391 _exptl_absorpt_correction_T_max 0.4185 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20045 _diffrn_reflns_av_R_equivalents 0.1259 _diffrn_reflns_av_sigmaI/netI 0.1530 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11463 _reflns_number_gt 7114 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution '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^)+(0.0951P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11463 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1609 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.017 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 Pb1 Pb 0.14963(3) 0.32087(2) 0.15562(2) 0.03910(16) Uani 1 1 d . . . Pb2 Pb -0.01287(2) 0.23261(2) 0.16279(2) 0.03286(15) Uani 1 1 d . . . Si1 Si 0.2722(2) 0.22693(19) 0.20677(18) 0.0452(9) Uani 1 1 d . . . Si2 Si 0.3206(2) 0.1568(2) 0.1357(2) 0.0535(11) Uani 1 1 d . . . Si3 Si 0.3174(2) 0.2318(3) 0.0536(2) 0.0707(14) Uani 1 1 d . . . Si4 Si 0.1944(2) 0.3049(3) 0.05078(19) 0.0652(13) Uani 1 1 d . . . Si5 Si 0.2379(2) 0.1446(3) 0.2770(2) 0.0669(13) Uani 1 1 d . . . Si6 Si 0.3794(3) 0.3071(4) 0.2513(2) 0.0901(18) Uani 1 1 d . . . Si7 Si 0.2208(4) 0.4293(4) 0.0272(3) 0.127(3) Uani 1 1 d . . . Si8 Si 0.0876(3) 0.2543(6) -0.0150(3) 0.161(4) Uani 1 1 d . . . Si9 Si -0.1578(2) 0.1568(2) 0.12162(17) 0.0464(9) Uani 1 1 d . . . Si10 Si -0.2618(2) 0.1897(2) 0.17796(16) 0.0446(9) Uani 1 1 d . . . Si11 Si -0.1958(3) 0.2384(3) 0.26513(17) 0.0632(13) Uani 1 1 d . . . Si12 Si -0.07733(19) 0.30492(18) 0.24595(14) 0.0335(7) Uani 1 1 d . . . Si13 Si -0.1124(3) 0.0347(2) 0.1391(3) 0.106(2) Uani 1 1 d . . . Si14 Si -0.2246(2) 0.1647(3) 0.0252(2) 0.0754(16) Uani 1 1 d . . . Si15 Si -0.11941(19) 0.41045(18) 0.18960(15) 0.0347(8) Uani 1 1 d . . . Si16 Si 0.0083(2) 0.3405(2) 0.33060(15) 0.0391(8) Uani 1 1 d . . . C1 C 0.4297(9) 0.1170(8) 0.1561(8) 0.075(5) Uani 1 1 d . . . H1A H 0.4308 0.0866 0.1903 0.112 Uiso 1 1 calc R . . H1B H 0.4710 0.1573 0.1637 0.112 Uiso 1 1 calc R . . H1C H 0.4442 0.0863 0.1250 0.112 Uiso 1 1 calc R . . C2 C 0.2454(9) 0.0769(8) 0.1179(9) 0.087(6) Uani 1 1 d . . . H2A H 0.2488 0.0597 0.0792 0.131 Uiso 1 1 calc R . . H2B H 0.1873 0.0930 0.1203 0.131 Uiso 1 1 calc R . . H2C H 0.2611 0.0364 0.1448 0.131 Uiso 1 1 calc R . . C3 C 0.4176(10) 0.2910(12) 0.0555(11) 0.132(10) Uani 1 1 d . . . H3A H 0.4679 0.2591 0.0622 0.198 Uiso 1 1 calc R . . H3B H 0.4199 0.3274 0.0862 0.198 Uiso 1 1 calc R . . H3C H 0.4162 0.3167 0.0191 0.198 Uiso 1 1 calc R . . C4 C 0.3208(12) 0.1718(13) -0.0103(9) 0.133(10) Uani 1 1 d . . . H4A H 0.3789 0.1537 -0.0103 0.200 Uiso 1 1 calc R . . H4B H 0.3032 0.2008 -0.0449 0.200 Uiso 1 1 calc R . . H4C H 0.2823 0.1297 -0.0092 0.200 Uiso 1 1 calc R . . C5 C 0.1262(8) 0.1097(8) 0.2574(7) 0.068(5) Uani 1 1 d . . . H5A H 0.1157 0.0697 0.2833 0.103 Uiso 1 1 calc R . . H5B H 0.1185 0.0909 0.2183 0.103 Uiso 1 1 calc R . . H5C H 0.0861 0.1502 0.2602 0.103 Uiso 1 1 calc R . . C6 C 0.2439(12) 0.1846(13) 0.3469(7) 0.111(8) Uani 1 1 d . . . H6A H 0.2193 0.1502 0.3718 0.167 Uiso 1 1 calc R . . H6B H 0.2123 0.2313 0.3445 0.167 Uiso 1 1 calc R . . H6C H 0.3035 0.1940 0.3624 0.167 Uiso 1 1 calc R . . C7 C 0.3148(10) 0.0649(10) 0.2851(9) 0.104(8) Uani 1 1 d . . . H7A H 0.3731 0.0840 0.2926 0.156 Uiso 1 1 calc R . . H7B H 0.3077 0.0357 0.2500 0.156 Uiso 1 1 calc R . . H7C H 0.3038 0.0335 0.3168 0.156 Uiso 1 1 calc R . . C8 C 0.4417(16) 0.354(2) 0.1942(10) 0.190(16) Uani 1 1 d . . . H8A H 0.4018 0.3828 0.1672 0.285 Uiso 1 1 calc R . . H8B H 0.4685 0.3160 0.1738 0.285 Uiso 1 1 calc R . . H8C H 0.4854 0.3875 0.2135 0.285 Uiso 1 1 calc R . . C9 C 0.4761(13) 0.258(2) 0.2777(13) 0.24(2) Uani 1 1 d . . . H9A H 0.5091 0.2870 0.3082 0.365 Uiso 1 1 calc R . . H9B H 0.5096 0.2509 0.2468 0.365 Uiso 1 1 calc R . . H9C H 0.4619 0.2098 0.2926 0.365 Uiso 1 1 calc R . . C10 C 0.3538(15) 0.359(2) 0.3019(18) 0.36(4) Uani 1 1 d . . . H10A H 0.3465 0.3285 0.3347 0.547 Uiso 1 1 calc R . . H10B H 0.3005 0.3851 0.2884 0.547 Uiso 1 1 calc R . . H10C H 0.3989 0.3956 0.3130 0.547 Uiso 1 1 calc R . . C11 C 0.1155(15) 0.4817(16) 0.0204(13) 0.25(2) Uani 1 1 d . . . H11A H 0.0788 0.4658 -0.0143 0.382 Uiso 1 1 calc R . . H11B H 0.1263 0.5350 0.0184 0.382 Uiso 1 1 calc R . . H11C H 0.0875 0.4711 0.0535 0.382 Uiso 1 1 calc R . . C12 C 0.3015(13) 0.4793(11) 0.0827(10) 0.119(8) Uani 1 1 d . . . H12A H 0.3588 0.4607 0.0805 0.178 Uiso 1 1 calc R . . H12B H 0.2873 0.4702 0.1208 0.178 Uiso 1 1 calc R . . H12C H 0.2995 0.5327 0.0750 0.178 Uiso 1 1 calc R . . C13 C 0.2621(14) 0.4330(16) -0.0449(10) 0.180(15) Uani 1 1 d . . . H13A H 0.3190 0.4112 -0.0409 0.270 Uiso 1 1 calc R . . H13B H 0.2646 0.4847 -0.0571 0.270 Uiso 1 1 calc R . . H13C H 0.2236 0.4052 -0.0732 0.270 Uiso 1 1 calc R . . C14 C 0.0765(14) 0.1475(18) 0.0007(16) 0.27(3) Uani 1 1 d . . . H14A H 0.0203 0.1378 0.0114 0.407 Uiso 1 1 calc R . . H14B H 0.1206 0.1328 0.0319 0.407 Uiso 1 1 calc R . . H14C H 0.0830 0.1189 -0.0334 0.407 Uiso 1 1 calc R . . C15 C 0.1147(18) 0.263(2) -0.0879(9) 0.25(2) Uani 1 1 d . . . H15A H 0.0685 0.2422 -0.1152 0.380 Uiso 1 1 calc R . . H15B H 0.1673 0.2358 -0.0904 0.380 Uiso 1 1 calc R . . H15C H 0.1225 0.3153 -0.0966 0.380 Uiso 1 1 calc R . . C16 C -0.0187(10) 0.2968(14) -0.0097(6) 0.106(8) Uani 1 1 d . . . H16A H -0.0484 0.3073 -0.0480 0.159 Uiso 1 1 calc R . . H16B H -0.0106 0.3429 0.0121 0.159 Uiso 1 1 calc R . . H16C H -0.0525 0.2622 0.0094 0.159 Uiso 1 1 calc R . . C17 C -0.3350(7) 0.2614(7) 0.1419(6) 0.044(3) Uani 1 1 d . . . H17A H -0.3620 0.2425 0.1050 0.067 Uiso 1 1 calc R . . H17B H -0.3028 0.3063 0.1362 0.067 Uiso 1 1 calc R . . H17C H -0.3788 0.2729 0.1655 0.067 Uiso 1 1 calc R . . C18 C -0.3310(9) 0.1085(9) 0.1906(7) 0.081(5) Uani 1 1 d . . . H18A H -0.3761 0.1250 0.2116 0.121 Uiso 1 1 calc R . . H18B H -0.2965 0.0707 0.2127 0.121 Uiso 1 1 calc R . . H18C H -0.3565 0.0876 0.1540 0.121 Uiso 1 1 calc R . . C19 C -0.1603(15) 0.1590(13) 0.3152(8) 0.155(13) Uani 1 1 d . . . H19A H -0.1419 0.1784 0.3535 0.233 Uiso 1 1 calc R . . H19B H -0.1129 0.1329 0.3019 0.233 Uiso 1 1 calc R . . H19C H -0.2077 0.1246 0.3160 0.233 Uiso 1 1 calc R . . C20 C -0.2740(10) 0.2950(14) 0.2985(7) 0.132(11) Uani 1 1 d . . . H20A H -0.3171 0.2624 0.3107 0.198 Uiso 1 1 calc R . . H20B H -0.3014 0.3309 0.2708 0.198 Uiso 1 1 calc R . . H20C H -0.2442 0.3215 0.3316 0.198 Uiso 1 1 calc R . . C21 C -0.0158(9) 0.0162(8) 0.1035(10) 0.111(8) Uani 1 1 d . . . H21A H -0.0179 0.0477 0.0698 0.166 Uiso 1 1 calc R . . H21B H -0.0153 -0.0360 0.0922 0.166 Uiso 1 1 calc R . . H21C H 0.0358 0.0273 0.1301 0.166 Uiso 1 1 calc R . . C22 C -0.0870(11) 0.0144(11) 0.2177(11) 0.171(14) Uani 1 1 d . . . H22A H -0.0520 -0.0303 0.2235 0.257 Uiso 1 1 calc R . . H22B H -0.1399 0.0068 0.2334 0.257 Uiso 1 1 calc R . . H22C H -0.0559 0.0563 0.2370 0.257 Uiso 1 1 calc R . . C23 C -0.1992(12) -0.0332(10) 0.1050(14) 0.195(16) Uani 1 1 d . . . H23A H -0.1883 -0.0467 0.0668 0.293 Uiso 1 1 calc R . . H23B H -0.2550 -0.0094 0.1024 0.293 Uiso 1 1 calc R . . H23C H -0.1984 -0.0778 0.1285 0.293 Uiso 1 1 calc R . . C24 C -0.1617(10) 0.1174(13) -0.0252(8) 0.117(9) Uani 1 1 d . . . H24A H -0.1504 0.0661 -0.0130 0.175 Uiso 1 1 calc R . . H24B H -0.1078 0.1435 -0.0254 0.175 Uiso 1 1 calc R . . H24C H -0.1942 0.1179 -0.0635 0.175 Uiso 1 1 calc R . . C25 C -0.3276(9) 0.1141(11) 0.0212(8) 0.098(7) Uani 1 1 d . . . H25A H -0.3643 0.1397 0.0447 0.146 Uiso 1 1 calc R . . H25B H -0.3170 0.0635 0.0352 0.146 Uiso 1 1 calc R . . H25C H -0.3557 0.1127 -0.0183 0.146 Uiso 1 1 calc R . . C26 C -0.2513(9) 0.2625(10) 0.0023(6) 0.077(5) Uani 1 1 d . . . H26A H -0.2774 0.2628 -0.0377 0.115 Uiso 1 1 calc R . . H26B H -0.1993 0.2923 0.0068 0.115 Uiso 1 1 calc R . . H26C H -0.2912 0.2833 0.0257 0.115 Uiso 1 1 calc R . . C27 C -0.1266(8) 0.3879(7) 0.1123(5) 0.048(3) Uani 1 1 d . . . H27A H -0.1582 0.4270 0.0898 0.072 Uiso 1 1 calc R . . H27B H -0.1562 0.3405 0.1046 0.072 Uiso 1 1 calc R . . H27C H -0.0693 0.3842 0.1021 0.072 Uiso 1 1 calc R . . C28 C -0.2261(7) 0.4461(7) 0.2021(6) 0.052(4) Uani 1 1 d . . . H28A H -0.2250 0.4560 0.2427 0.078 Uiso 1 1 calc R . . H28B H -0.2697 0.4090 0.1895 0.078 Uiso 1 1 calc R . . H28C H -0.2391 0.4920 0.1805 0.078 Uiso 1 1 calc R . . C29 C -0.0407(8) 0.4855(7) 0.2044(6) 0.052(4) Uani 1 1 d . . . H29A H 0.0148 0.4680 0.1968 0.078 Uiso 1 1 calc R . . H29B H -0.0366 0.5004 0.2443 0.078 Uiso 1 1 calc R . . H29C H -0.0585 0.5280 0.1799 0.078 Uiso 1 1 calc R . . C30 C -0.0496(8) 0.4134(8) 0.3669(6) 0.056(4) Uani 1 1 d . . . H30A H -0.0144 0.4286 0.4023 0.084 Uiso 1 1 calc R . . H30B H -0.1034 0.3930 0.3754 0.084 Uiso 1 1 calc R . . H30C H -0.0612 0.4563 0.3418 0.084 Uiso 1 1 calc R . . C31 C 0.1132(7) 0.3804(8) 0.3188(6) 0.055(4) Uani 1 1 d . . . H31A H 0.1042 0.4296 0.3016 0.082 Uiso 1 1 calc R . . H31B H 0.1394 0.3480 0.2932 0.082 Uiso 1 1 calc R . . H31C H 0.1506 0.3843 0.3552 0.082 Uiso 1 1 calc R . . C32 C 0.0276(9) 0.2599(8) 0.3799(6) 0.060(4) Uani 1 1 d . . . H32A H 0.0533 0.2194 0.3609 0.090 Uiso 1 1 calc R . . H32B H -0.0265 0.2432 0.3906 0.090 Uiso 1 1 calc R . . H32C H 0.0660 0.2747 0.4140 0.090 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 Pb1 0.0241(2) 0.0299(2) 0.0644(4) 0.0031(2) 0.0103(2) 0.00472(18) Pb2 0.0208(2) 0.0272(2) 0.0478(3) -0.0010(2) -0.00394(18) 0.00092(17) Si1 0.0201(15) 0.039(2) 0.073(3) 0.0041(19) -0.0022(16) 0.0004(14) Si2 0.0232(16) 0.0335(19) 0.104(3) 0.000(2) 0.0100(19) 0.0052(14) Si3 0.0271(19) 0.084(3) 0.105(4) 0.013(3) 0.023(2) 0.021(2) Si4 0.0335(19) 0.096(3) 0.071(3) 0.022(3) 0.022(2) 0.036(2) Si5 0.0300(19) 0.080(3) 0.091(3) 0.032(3) 0.009(2) 0.023(2) Si6 0.039(2) 0.129(5) 0.097(4) -0.015(4) -0.011(2) -0.043(3) Si7 0.105(4) 0.147(5) 0.153(6) 0.122(5) 0.101(5) 0.100(4) Si8 0.048(3) 0.348(13) 0.086(4) -0.093(6) 0.006(3) 0.071(5) Si9 0.0254(16) 0.040(2) 0.068(3) -0.0138(19) -0.0135(16) -0.0025(15) Si10 0.0270(16) 0.044(2) 0.059(2) 0.0069(18) -0.0071(16) -0.0137(15) Si11 0.050(2) 0.089(3) 0.047(2) 0.016(2) -0.0047(19) -0.046(2) Si12 0.0237(15) 0.0374(18) 0.0394(19) 0.0053(15) 0.0042(14) -0.0066(13) Si13 0.030(2) 0.031(2) 0.246(8) 0.005(3) -0.017(3) -0.0067(17) Si14 0.0280(19) 0.122(4) 0.070(3) -0.053(3) -0.0137(19) 0.013(2) Si15 0.0236(15) 0.0318(17) 0.050(2) -0.0003(16) 0.0088(15) 0.0004(13) Si16 0.0285(16) 0.046(2) 0.041(2) -0.0005(16) 0.0006(15) -0.0076(15) C1 0.041(8) 0.056(9) 0.128(15) 0.028(10) 0.017(9) 0.033(7) C2 0.053(9) 0.044(9) 0.171(19) -0.031(11) 0.035(11) -0.010(7) C3 0.041(10) 0.138(18) 0.23(3) 0.059(19) 0.050(14) 0.039(11) C4 0.093(15) 0.21(3) 0.118(17) -0.001(17) 0.071(14) 0.076(16) C5 0.039(8) 0.074(11) 0.099(12) 0.038(10) 0.030(8) 0.013(7) C6 0.084(14) 0.17(2) 0.070(13) 0.020(14) -0.008(10) 0.051(15) C7 0.069(11) 0.105(14) 0.150(18) 0.078(14) 0.051(12) 0.060(11) C8 0.12(2) 0.33(4) 0.13(2) -0.08(3) 0.042(17) -0.12(3) C9 0.042(12) 0.44(6) 0.23(3) -0.20(4) -0.057(15) 0.05(2) C10 0.079(17) 0.52(6) 0.52(6) -0.48(6) 0.12(3) -0.14(3) C11 0.16(2) 0.27(3) 0.39(4) 0.29(3) 0.21(3) 0.18(2) C12 0.101(16) 0.087(15) 0.17(2) -0.003(15) 0.034(16) -0.026(13) C13 0.107(17) 0.29(3) 0.16(2) 0.18(2) 0.084(16) 0.12(2) C14 0.051(13) 0.29(4) 0.47(6) -0.28(4) 0.01(2) 0.04(2) C15 0.15(3) 0.56(7) 0.056(14) -0.04(3) 0.029(16) 0.10(4) C16 0.056(10) 0.22(2) 0.037(9) -0.006(12) -0.013(7) 0.056(13) C17 0.035(6) 0.046(7) 0.054(8) -0.015(6) 0.010(6) -0.014(6) C18 0.038(8) 0.092(12) 0.103(13) 0.039(11) -0.018(8) -0.038(8) C19 0.17(2) 0.18(2) 0.091(15) 0.089(16) -0.064(14) -0.13(2) C20 0.070(11) 0.27(3) 0.064(11) -0.079(15) 0.051(10) -0.120(16) C21 0.032(8) 0.036(8) 0.26(3) -0.044(12) 0.003(12) 0.006(6) C22 0.045(10) 0.121(17) 0.34(4) 0.18(2) -0.009(15) 0.001(10) C23 0.061(13) 0.053(12) 0.46(5) -0.08(2) -0.01(2) -0.030(10) C24 0.050(10) 0.19(2) 0.107(15) -0.108(16) -0.011(9) 0.016(12) C25 0.035(8) 0.114(15) 0.130(16) -0.064(13) -0.036(9) 0.011(9) C26 0.033(7) 0.138(16) 0.054(9) -0.023(10) -0.011(7) 0.023(9) C27 0.046(7) 0.058(9) 0.039(7) -0.002(7) 0.004(6) 0.008(7) C28 0.028(6) 0.046(8) 0.082(10) -0.003(7) 0.007(7) 0.006(6) C29 0.041(7) 0.044(8) 0.075(10) -0.008(7) 0.020(7) -0.012(6) C30 0.047(8) 0.067(9) 0.054(9) 0.006(8) 0.008(7) 0.000(7) C31 0.030(6) 0.070(10) 0.064(9) -0.004(8) 0.005(6) -0.015(7) C32 0.053(8) 0.076(10) 0.046(8) 0.005(8) -0.009(7) -0.001(8) _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 Pb1 Si4 2.709(4) . ? Pb1 Si1 2.732(3) . ? Pb1 Pb2 3.0640(8) . ? Pb2 Si12 2.697(3) . ? Pb2 Si9 2.737(3) . ? Si1 Si2 2.334(6) . ? Si1 Si5 2.361(6) . ? Si1 Si6 2.366(6) . ? Si2 C1 1.875(13) . ? Si2 C2 1.883(14) . ? Si2 Si3 2.371(7) . ? Si3 C4 1.87(2) . ? Si3 C3 1.91(2) . ? Si3 Si4 2.353(5) . ? Si4 Si8 2.321(9) . ? Si4 Si7 2.368(8) . ? Si5 C6 1.802(19) . ? Si5 C7 1.882(14) . ? Si5 C5 1.878(15) . ? Si6 C10 1.63(2) . ? Si6 C9 1.80(3) . ? Si6 C8 1.99(2) . ? Si7 C11 1.910(17) . ? Si7 C12 1.93(2) . ? Si7 C13 1.925(18) . ? Si8 C15 1.85(2) . ? Si8 C16 1.879(16) . ? Si8 C14 1.98(4) . ? Si9 Si13 2.340(6) . ? Si9 Si10 2.353(5) . ? Si9 Si14 2.385(6) . ? Si10 C17 1.864(13) . ? Si10 C18 1.885(13) . ? Si10 Si11 2.352(6) . ? Si11 C20 1.88(2) . ? Si11 C19 1.897(19) . ? Si11 Si12 2.337(5) . ? Si12 Si16 2.348(5) . ? Si12 Si15 2.370(5) . ? Si13 C22 1.89(2) . ? Si13 C21 1.891(17) . ? Si13 C23 1.934(17) . ? Si14 C25 1.868(17) . ? Si14 C24 1.876(15) . ? Si14 C26 1.878(18) . ? Si15 C29 1.844(12) . ? Si15 C27 1.870(12) . ? Si15 C28 1.880(11) . ? Si16 C32 1.866(14) . ? Si16 C31 1.877(12) . ? Si16 C30 1.888(14) . ? 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 Si4 Pb1 Si1 94.38(12) . . ? Si4 Pb1 Pb2 109.54(11) . . ? Si1 Pb1 Pb2 101.83(7) . . ? Si12 Pb2 Si9 96.49(10) . . ? Si12 Pb2 Pb1 101.80(7) . . ? Si9 Pb2 Pb1 156.09(9) . . ? Si2 Si1 Si5 107.9(2) . . ? Si2 Si1 Si6 111.3(2) . . ? Si5 Si1 Si6 107.2(2) . . ? Si2 Si1 Pb1 107.74(18) . . ? Si5 Si1 Pb1 118.81(15) . . ? Si6 Si1 Pb1 103.9(2) . . ? C1 Si2 C2 107.3(7) . . ? C1 Si2 Si1 114.3(6) . . ? C2 Si2 Si1 108.2(5) . . ? C1 Si2 Si3 109.8(5) . . ? C2 Si2 Si3 108.5(7) . . ? Si1 Si2 Si3 108.5(2) . . ? C4 Si3 C3 102.6(10) . . ? C4 Si3 Si4 115.2(7) . . ? C3 Si3 Si4 111.9(6) . . ? C4 Si3 Si2 109.8(7) . . ? C3 Si3 Si2 112.5(7) . . ? Si4 Si3 Si2 105.1(2) . . ? Si8 Si4 Si3 108.7(3) . . ? Si8 Si4 Si7 110.6(4) . . ? Si3 Si4 Si7 111.3(2) . . ? Si8 Si4 Pb1 113.4(2) . . ? Si3 Si4 Pb1 111.4(2) . . ? Si7 Si4 Pb1 101.4(2) . . ? C6 Si5 C7 105.5(9) . . ? C6 Si5 C5 106.5(8) . . ? C7 Si5 C5 110.2(8) . . ? C6 Si5 Si1 114.5(8) . . ? C7 Si5 Si1 109.8(5) . . ? C5 Si5 Si1 110.1(5) . . ? C10 Si6 C9 108.6(19) . . ? C10 Si6 C8 117.5(19) . . ? C9 Si6 C8 87.9(15) . . ? C10 Si6 Si1 116.2(8) . . ? C9 Si6 Si1 112.2(11) . . ? C8 Si6 Si1 110.9(7) . . ? C11 Si7 C12 108.2(14) . . ? C11 Si7 C13 108.5(9) . . ? C12 Si7 C13 108.2(12) . . ? C11 Si7 Si4 107.8(9) . . ? C12 Si7 Si4 114.0(7) . . ? C13 Si7 Si4 109.9(10) . . ? C15 Si8 C16 111.3(11) . . ? C15 Si8 C14 107.4(16) . . ? C16 Si8 C14 106.2(10) . . ? C15 Si8 Si4 110.5(11) . . ? C16 Si8 Si4 111.8(7) . . ? C14 Si8 Si4 109.5(10) . . ? Si13 Si9 Si10 111.2(2) . . ? Si13 Si9 Si14 108.0(3) . . ? Si10 Si9 Si14 106.39(18) . . ? Si13 Si9 Pb2 100.70(15) . . ? Si10 Si9 Pb2 107.22(15) . . ? Si14 Si9 Pb2 123.1(2) . . ? C17 Si10 C18 105.8(6) . . ? C17 Si10 Si11 108.3(4) . . ? C18 Si10 Si11 110.2(6) . . ? C17 Si10 Si9 110.9(4) . . ? C18 Si10 Si9 111.8(6) . . ? Si11 Si10 Si9 109.70(19) . . ? C20 Si11 C19 107.5(11) . . ? C20 Si11 Si12 114.0(6) . . ? C19 Si11 Si12 109.7(7) . . ? C20 Si11 Si10 109.9(6) . . ? C19 Si11 Si10 108.9(7) . . ? Si12 Si11 Si10 106.72(19) . . ? Si11 Si12 Si16 110.84(18) . . ? Si11 Si12 Si15 110.82(18) . . ? Si16 Si12 Si15 110.19(18) . . ? Si11 Si12 Pb2 107.42(17) . . ? Si16 Si12 Pb2 121.76(14) . . ? Si15 Si12 Pb2 94.63(13) . . ? C22 Si13 C21 109.9(9) . . ? C22 Si13 C23 109.2(12) . . ? C21 Si13 C23 106.1(10) . . ? C22 Si13 Si9 112.0(8) . . ? C21 Si13 Si9 109.7(6) . . ? C23 Si13 Si9 109.8(7) . . ? C25 Si14 C24 106.9(8) . . ? C25 Si14 C26 106.6(7) . . ? C24 Si14 C26 111.2(9) . . ? C25 Si14 Si9 106.4(7) . . ? C24 Si14 Si9 112.6(6) . . ? C26 Si14 Si9 112.7(5) . . ? C29 Si15 C27 106.9(6) . . ? C29 Si15 C28 108.7(6) . . ? C27 Si15 C28 107.7(6) . . ? C29 Si15 Si12 110.9(5) . . ? C27 Si15 Si12 110.6(4) . . ? C28 Si15 Si12 111.9(4) . . ? C32 Si16 C31 109.0(7) . . ? C32 Si16 C30 107.6(6) . . ? C31 Si16 C30 107.8(6) . . ? C32 Si16 Si12 110.3(5) . . ? C31 Si16 Si12 113.1(5) . . ? C30 Si16 Si12 108.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si4 Pb1 Pb2 Si12 -155.46(12) . . . . ? Si1 Pb1 Pb2 Si12 105.49(11) . . . . ? Si4 Pb1 Pb2 Si9 -16.3(2) . . . . ? Si1 Pb1 Pb2 Si9 -115.4(2) . . . . ? Si4 Pb1 Si1 Si2 -16.91(18) . . . . ? Pb2 Pb1 Si1 Si2 94.12(14) . . . . ? Si4 Pb1 Si1 Si5 -139.9(2) . . . . ? Pb2 Pb1 Si1 Si5 -28.8(2) . . . . ? Si4 Pb1 Si1 Si6 101.2(2) . . . . ? Pb2 Pb1 Si1 Si6 -147.73(18) . . . . ? Si5 Si1 Si2 C1 -73.3(6) . . . . ? Si6 Si1 Si2 C1 44.0(6) . . . . ? Pb1 Si1 Si2 C1 157.3(5) . . . . ? Si5 Si1 Si2 C2 46.2(7) . . . . ? Si6 Si1 Si2 C2 163.6(7) . . . . ? Pb1 Si1 Si2 C2 -83.2(7) . . . . ? Si5 Si1 Si2 Si3 163.7(2) . . . . ? Si6 Si1 Si2 Si3 -78.9(3) . . . . ? Pb1 Si1 Si2 Si3 34.3(2) . . . . ? C1 Si2 Si3 C4 72.7(9) . . . . ? C2 Si2 Si3 C4 -44.3(8) . . . . ? Si1 Si2 Si3 C4 -161.6(7) . . . . ? C1 Si2 Si3 C3 -40.8(9) . . . . ? C2 Si2 Si3 C3 -157.8(9) . . . . ? Si1 Si2 Si3 C3 84.8(7) . . . . ? C1 Si2 Si3 Si4 -162.8(6) . . . . ? C2 Si2 Si3 Si4 80.1(5) . . . . ? Si1 Si2 Si3 Si4 -37.2(3) . . . . ? C4 Si3 Si4 Si8 20.1(9) . . . . ? C3 Si3 Si4 Si8 136.8(9) . . . . ? Si2 Si3 Si4 Si8 -100.9(4) . . . . ? C4 Si3 Si4 Si7 -101.9(8) . . . . ? C3 Si3 Si4 Si7 14.8(9) . . . . ? Si2 Si3 Si4 Si7 137.2(3) . . . . ? C4 Si3 Si4 Pb1 145.8(8) . . . . ? C3 Si3 Si4 Pb1 -97.6(9) . . . . ? Si2 Si3 Si4 Pb1 24.8(3) . . . . ? Si1 Pb1 Si4 Si8 118.0(3) . . . . ? Pb2 Pb1 Si4 Si8 13.8(3) . . . . ? Si1 Pb1 Si4 Si3 -5.1(2) . . . . ? Pb2 Pb1 Si4 Si3 -109.3(2) . . . . ? Si1 Pb1 Si4 Si7 -123.5(2) . . . . ? Pb2 Pb1 Si4 Si7 132.3(2) . . . . ? Si2 Si1 Si5 C6 154.3(7) . . . . ? Si6 Si1 Si5 C6 34.4(7) . . . . ? Pb1 Si1 Si5 C6 -82.8(7) . . . . ? Si2 Si1 Si5 C7 35.9(8) . . . . ? Si6 Si1 Si5 C7 -84.1(8) . . . . ? Pb1 Si1 Si5 C7 158.8(8) . . . . ? Si2 Si1 Si5 C5 -85.7(6) . . . . ? Si6 Si1 Si5 C5 154.4(6) . . . . ? Pb1 Si1 Si5 C5 37.2(6) . . . . ? Si2 Si1 Si6 C10 -180(2) . . . . ? Si5 Si1 Si6 C10 -62(2) . . . . ? Pb1 Si1 Si6 C10 64(2) . . . . ? Si2 Si1 Si6 C9 -54.1(12) . . . . ? Si5 Si1 Si6 C9 63.6(12) . . . . ? Pb1 Si1 Si6 C9 -169.8(12) . . . . ? Si2 Si1 Si6 C8 42.4(12) . . . . ? Si5 Si1 Si6 C8 160.2(12) . . . . ? Pb1 Si1 Si6 C8 -73.3(12) . . . . ? Si8 Si4 Si7 C11 54.7(12) . . . . ? Si3 Si4 Si7 C11 175.6(12) . . . . ? Pb1 Si4 Si7 C11 -65.9(12) . . . . ? Si8 Si4 Si7 C12 174.9(7) . . . . ? Si3 Si4 Si7 C12 -64.2(8) . . . . ? Pb1 Si4 Si7 C12 54.4(7) . . . . ? Si8 Si4 Si7 C13 -63.4(8) . . . . ? Si3 Si4 Si7 C13 57.5(8) . . . . ? Pb1 Si4 Si7 C13 176.1(8) . . . . ? Si3 Si4 Si8 C15 -67.1(13) . . . . ? Si7 Si4 Si8 C15 55.4(13) . . . . ? Pb1 Si4 Si8 C15 168.4(13) . . . . ? Si3 Si4 Si8 C16 168.4(8) . . . . ? Si7 Si4 Si8 C16 -69.2(9) . . . . ? Pb1 Si4 Si8 C16 43.9(9) . . . . ? Si3 Si4 Si8 C14 51.0(9) . . . . ? Si7 Si4 Si8 C14 173.5(8) . . . . ? Pb1 Si4 Si8 C14 -73.5(9) . . . . ? Si12 Pb2 Si9 Si13 -117.2(2) . . . . ? Pb1 Pb2 Si9 Si13 103.0(3) . . . . ? Si12 Pb2 Si9 Si10 -0.86(18) . . . . ? Pb1 Pb2 Si9 Si10 -140.71(15) . . . . ? Si12 Pb2 Si9 Si14 122.8(2) . . . . ? Pb1 Pb2 Si9 Si14 -17.0(3) . . . . ? Si13 Si9 Si10 C17 -151.2(4) . . . . ? Si14 Si9 Si10 C17 -33.8(5) . . . . ? Pb2 Si9 Si10 C17 99.6(4) . . . . ? Si13 Si9 Si10 C18 -33.4(6) . . . . ? Si14 Si9 Si10 C18 84.0(6) . . . . ? Pb2 Si9 Si10 C18 -142.5(5) . . . . ? Si13 Si9 Si10 Si11 89.2(3) . . . . ? Si14 Si9 Si10 Si11 -153.4(2) . . . . ? Pb2 Si9 Si10 Si11 -20.0(2) . . . . ? C17 Si10 Si11 C20 38.4(8) . . . . ? C18 Si10 Si11 C20 -76.9(9) . . . . ? Si9 Si10 Si11 C20 159.6(7) . . . . ? C17 Si10 Si11 C19 156.0(9) . . . . ? C18 Si10 Si11 C19 40.7(10) . . . . ? Si9 Si10 Si11 C19 -82.8(9) . . . . ? C17 Si10 Si11 Si12 -85.6(4) . . . . ? C18 Si10 Si11 Si12 159.1(6) . . . . ? Si9 Si10 Si11 Si12 35.6(3) . . . . ? C20 Si11 Si12 Si16 68.0(7) . . . . ? C19 Si11 Si12 Si16 -52.7(9) . . . . ? Si10 Si11 Si12 Si16 -170.5(2) . . . . ? C20 Si11 Si12 Si15 -54.7(7) . . . . ? C19 Si11 Si12 Si15 -175.4(9) . . . . ? Si10 Si11 Si12 Si15 66.8(3) . . . . ? C20 Si11 Si12 Pb2 -156.8(7) . . . . ? C19 Si11 Si12 Pb2 82.5(9) . . . . ? Si10 Si11 Si12 Pb2 -35.3(2) . . . . ? Si9 Pb2 Si12 Si11 21.34(18) . . . . ? Pb1 Pb2 Si12 Si11 -174.15(14) . . . . ? Si9 Pb2 Si12 Si16 150.59(18) . . . . ? Pb1 Pb2 Si12 Si16 -44.89(17) . . . . ? Si9 Pb2 Si12 Si15 -92.19(14) . . . . ? Pb1 Pb2 Si12 Si15 72.33(12) . . . . ? Si10 Si9 Si13 C22 -47.5(6) . . . . ? Si14 Si9 Si13 C22 -163.9(6) . . . . ? Pb2 Si9 Si13 C22 65.9(6) . . . . ? Si10 Si9 Si13 C21 -169.8(7) . . . . ? Si14 Si9 Si13 C21 73.8(7) . . . . ? Pb2 Si9 Si13 C21 -56.4(7) . . . . ? Si10 Si9 Si13 C23 74.0(11) . . . . ? Si14 Si9 Si13 C23 -42.4(11) . . . . ? Pb2 Si9 Si13 C23 -172.7(11) . . . . ? Si13 Si9 Si14 C25 71.2(6) . . . . ? Si10 Si9 Si14 C25 -48.2(6) . . . . ? Pb2 Si9 Si14 C25 -172.3(6) . . . . ? Si13 Si9 Si14 C24 -45.6(8) . . . . ? Si10 Si9 Si14 C24 -165.1(8) . . . . ? Pb2 Si9 Si14 C24 70.9(8) . . . . ? Si13 Si9 Si14 C26 -172.3(5) . . . . ? Si10 Si9 Si14 C26 68.2(5) . . . . ? Pb2 Si9 Si14 C26 -55.9(5) . . . . ? Si11 Si12 Si15 C29 150.3(5) . . . . ? Si16 Si12 Si15 C29 27.3(5) . . . . ? Pb2 Si12 Si15 C29 -99.0(5) . . . . ? Si11 Si12 Si15 C27 -91.3(5) . . . . ? Si16 Si12 Si15 C27 145.6(5) . . . . ? Pb2 Si12 Si15 C27 19.3(5) . . . . ? Si11 Si12 Si15 C28 28.8(5) . . . . ? Si16 Si12 Si15 C28 -94.3(5) . . . . ? Pb2 Si12 Si15 C28 139.4(5) . . . . ? Si11 Si12 Si16 C32 48.2(5) . . . . ? Si15 Si12 Si16 C32 171.2(5) . . . . ? Pb2 Si12 Si16 C32 -79.6(5) . . . . ? Si11 Si12 Si16 C31 170.6(5) . . . . ? Si15 Si12 Si16 C31 -66.4(5) . . . . ? Pb2 Si12 Si16 C31 42.8(5) . . . . ? Si11 Si12 Si16 C30 -69.6(5) . . . . ? Si15 Si12 Si16 C30 53.4(5) . . . . ? Pb2 Si12 Si16 C30 162.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 2.211 _refine_diff_density_min -1.964 _refine_diff_density_rms 0.211 #===END