data_ki315_compound10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H52 B2 P2 Si4 Sn, C4 H10 O' _chemical_formula_sum 'C22 H62 B2 O P2 Si4 Sn' _chemical_formula_weight 657.33 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' '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' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y, -z+1/2' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z+1' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' '-x, y, z-1/2' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' _cell_length_a 16.220(4) _cell_length_b 20.048(7) _cell_length_c 21.707(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7059(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 290 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.5 _exptl_crystal_description lath _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23985 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4031 _reflns_number_gt 2563 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution SIR2002 _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0501P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4031 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Sn Sn 0.309412(18) 0.0000 0.2500 0.02077(11) Uani 1 2 d S . . P P 0.32076(5) -0.13814(5) 0.18971(4) 0.0242(2) Uani 1 1 d . . . Si1 Si 0.36590(6) -0.02299(6) 0.09738(4) 0.0282(3) Uani 1 1 d . . . Si2 Si 0.49621(6) -0.08437(6) 0.19178(4) 0.0268(3) Uani 1 1 d . . . B B 0.3053(3) -0.1499(3) 0.2791(2) 0.0297(10) Uani 1 1 d . . . H1 H 0.337(2) -0.1999(19) 0.2925(15) 0.030(10) Uiso 1 1 d . . . H2 H 0.334(2) -0.096(2) 0.3051(18) 0.051(12) Uiso 1 1 d . . . H3 H 0.235(2) -0.1413(18) 0.2877(16) 0.034(10) Uiso 1 1 d . . . C1 C 0.38350(19) -0.0645(2) 0.17585(15) 0.0252(9) Uani 1 1 d . . . C2 C 0.3608(2) -0.2128(2) 0.15222(16) 0.0325(9) Uani 1 1 d . . . H2A H 0.3625 -0.2057 0.1076 0.049 Uiso 1 1 calc R . . H2B H 0.3249 -0.2507 0.1615 0.049 Uiso 1 1 calc R . . H2C H 0.4166 -0.2220 0.1674 0.049 Uiso 1 1 calc R . . C3 C 0.2188(2) -0.1325(2) 0.15353(17) 0.0316(10) Uani 1 1 d . . . H3A H 0.2253 -0.1282 0.1088 0.047 Uiso 1 1 calc R . . H3B H 0.1895 -0.0935 0.1696 0.047 Uiso 1 1 calc R . . H3C H 0.1872 -0.1729 0.1628 0.047 Uiso 1 1 calc R . . C4 C 0.3695(2) -0.0847(2) 0.03152(15) 0.0369(11) Uani 1 1 d . . . H4A H 0.3221 -0.1148 0.0342 0.055 Uiso 1 1 calc R . . H4B H 0.4206 -0.1107 0.0339 0.055 Uiso 1 1 calc R . . H4C H 0.3677 -0.0606 -0.0077 0.055 Uiso 1 1 calc R . . C5 C 0.4456(2) 0.0432(2) 0.08166(18) 0.0420(11) Uani 1 1 d . . . H5A H 0.4352 0.0633 0.0413 0.063 Uiso 1 1 calc R . . H5B H 0.5007 0.0231 0.0820 0.063 Uiso 1 1 calc R . . H5C H 0.4425 0.0777 0.1136 0.063 Uiso 1 1 calc R . . C6 C 0.2630(2) 0.0217(2) 0.09228(17) 0.0323(10) Uani 1 1 d . . . H6A H 0.2182 -0.0109 0.0954 0.048 Uiso 1 1 calc R . . H6B H 0.2592 0.0452 0.0528 0.048 Uiso 1 1 calc R . . H6C H 0.2585 0.0539 0.1260 0.048 Uiso 1 1 calc R . . C7 C 0.5482(2) -0.1190(2) 0.12001(17) 0.0362(10) Uani 1 1 d . . . H7A H 0.5151 -0.1557 0.1034 0.054 Uiso 1 1 calc R . . H7B H 0.6033 -0.1354 0.1307 0.054 Uiso 1 1 calc R . . H7C H 0.5529 -0.0837 0.0890 0.054 Uiso 1 1 calc R . . C8 C 0.5122(2) -0.1485(2) 0.25431(17) 0.0351(9) Uani 1 1 d . . . H8A H 0.4803 -0.1887 0.2447 0.053 Uiso 1 1 calc R . . H8B H 0.4939 -0.1303 0.2939 0.053 Uiso 1 1 calc R . . H8C H 0.5709 -0.1600 0.2568 0.053 Uiso 1 1 calc R . . C9 C 0.5605(2) -0.0105(2) 0.21520(18) 0.0335(10) Uani 1 1 d . . . H9A H 0.6182 -0.0197 0.2031 0.040 Uiso 1 1 calc R . . H9B H 0.5418 0.0284 0.1907 0.040 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 Sn 0.01062(16) 0.0358(2) 0.01592(16) 0.00024(17) 0.000 0.000 P 0.0163(5) 0.0376(6) 0.0188(4) -0.0023(4) 0.0012(4) -0.0009(4) Si1 0.0201(5) 0.0480(8) 0.0166(5) 0.0018(5) 0.0009(4) -0.0027(5) Si2 0.0124(5) 0.0462(7) 0.0219(5) -0.0044(5) -0.0002(4) 0.0002(5) B 0.032(3) 0.035(3) 0.022(2) 0.005(2) 0.012(2) 0.000(2) C1 0.0125(17) 0.044(3) 0.0194(18) -0.0052(17) 0.0030(13) -0.0028(16) C2 0.028(2) 0.041(3) 0.029(2) -0.0087(19) 0.0010(16) 0.0018(18) C3 0.0183(18) 0.046(3) 0.031(2) -0.0072(19) 0.0009(15) -0.0046(17) C4 0.029(2) 0.065(3) 0.0169(19) -0.0005(19) -0.0008(16) 0.001(2) C5 0.040(2) 0.062(3) 0.024(2) 0.009(2) 0.0061(18) -0.008(2) C6 0.032(2) 0.043(3) 0.0225(19) 0.0021(17) -0.0045(16) -0.0005(18) C7 0.0157(19) 0.060(3) 0.033(2) -0.009(2) 0.0012(16) 0.0050(19) C8 0.023(2) 0.050(3) 0.032(2) -0.003(2) -0.0075(17) 0.0030(18) C9 0.0091(16) 0.053(3) 0.038(2) -0.007(2) 0.0033(15) -0.0014(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn C1 2.389(3) . ? Sn C1 2.389(3) 3 ? P B 1.971(5) . ? P C1 1.818(4) . ? P C2 1.823(4) . ? P C3 1.834(3) . ? Si1 C1 1.917(4) . ? Si1 C4 1.891(4) . ? Si1 C5 1.885(4) . ? Si1 C6 1.898(4) . ? Si2 C1 1.903(3) . ? Si2 C7 1.902(4) . ? Si2 C8 1.888(4) . ? Si2 C9 1.881(4) . ? B H1 1.16(4) . ? B H2 1.30(4) . ? B H3 1.16(3) . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 C9 1.568(8) 3 ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? 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 Sn C1 119.60(15) . 3 ? B P C1 109.37(18) . . ? B P C2 112.7(2) . . ? B P C3 108.32(19) . . ? C1 P C2 113.15(17) . . ? C1 P C3 112.58(18) . . ? C2 P C3 100.40(18) . . ? C1 Si1 C4 112.53(18) . . ? C1 Si1 C5 111.38(16) . . ? C1 Si1 C6 112.82(15) . . ? C4 Si1 C5 107.63(19) . . ? C4 Si1 C6 106.97(17) . . ? C5 Si1 C6 105.1(2) . . ? C1 Si2 C7 110.68(15) . . ? C1 Si2 C8 113.94(16) . . ? C1 Si2 C9 114.62(18) . . ? C7 Si2 C8 106.21(19) . . ? C7 Si2 C9 105.26(17) . . ? C8 Si2 C9 105.41(18) . . ? P B H1 107.1(16) . . ? P B H2 106.3(18) . . ? P B H3 105.3(18) . . ? H1 B H2 117(2) . . ? H1 B H3 121(2) . . ? H2 B H3 99(2) . . ? Sn C1 P 92.66(13) . . ? Sn C1 Si1 106.78(17) . . ? Sn C1 Si2 118.30(15) . . ? P C1 Si1 114.59(17) . . ? P C1 Si2 109.7(2) . . ? Si1 C1 Si2 113.30(16) . . ? P C2 H2A 109.5 . . ? P C2 H2B 109.5 . . ? P C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P C3 H3A 109.5 . . ? P C3 H3B 109.5 . . ? P C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 C9 118.1(3) . 3 ? Si2 C9 H9A 107.8 . . ? Si2 C9 H9B 107.8 . . ? C9 C9 H9A 107.8 3 . ? C9 C9 H9B 107.8 3 . ? H9A C9 H9B 107.1 . . ? 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 B P C1 Sn -44.0(2) . . . . ? B P C1 Si1 -153.8(2) . . . . ? B P C1 Si2 77.4(2) . . . . ? C2 P C1 Sn -170.57(14) . . . . ? C2 P C1 Si1 79.6(2) . . . . ? C2 P C1 Si2 -49.2(2) . . . . ? C3 P C1 Sn 76.45(17) . . . . ? C3 P C1 Si1 -33.4(2) . . . . ? C3 P C1 Si2 -162.15(17) . . . . ? C7 Si2 C1 Sn -167.65(19) . . . . ? C7 Si2 C1 P 87.9(2) . . . . ? C7 Si2 C1 Si1 -41.6(3) . . . . ? C8 Si2 C1 Sn 72.8(2) . . . . ? C8 Si2 C1 P -31.7(2) . . . . ? C8 Si2 C1 Si1 -161.17(19) . . . . ? C9 Si2 C1 Sn -48.8(2) . . . . ? C9 Si2 C1 P -153.24(18) . . . . ? C9 Si2 C1 Si1 77.3(2) . . . . ? C4 Si1 C1 Sn -150.30(15) . . . . ? C4 Si1 C1 P -49.3(2) . . . . ? C4 Si1 C1 Si2 77.7(2) . . . . ? C5 Si1 C1 Sn 88.7(2) . . . . ? C5 Si1 C1 P -170.2(2) . . . . ? C5 Si1 C1 Si2 -43.2(3) . . . . ? C6 Si1 C1 Sn -29.2(2) . . . . ? C6 Si1 C1 P 71.9(2) . . . . ? C6 Si1 C1 Si2 -161.15(19) . . . . ? C1 Sn C1 P 132.49(16) 3 . . . ? C1 Sn C1 Si1 -110.83(17) 3 . . . ? C1 Sn C1 Si2 18.34(14) 3 . . . ? C1 Si2 C9 C9 84.4(3) . . . 3 ? C7 Si2 C9 C9 -153.7(3) . . . 3 ? C8 Si2 C9 C9 -41.7(3) . . . 3 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.761 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.103 #===END data_ki318_compound11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H52 B2 P2 Pb Si4, C4 H10 O' _chemical_formula_sum 'C22 H62 B2 O P2 Pb Si4' _chemical_formula_weight 745.83 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.168(3) _cell_length_b 20.182(7) _cell_length_c 21.656(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7066(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 206 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 27.50 _exptl_crystal_description lath _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 5.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.280 _exptl_absorpt_correction_T_max 0.634 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44824 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.92 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6188 _reflns_number_gt 3770 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0093P)^2^+31.7020P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6188 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0623 _refine_ls_wR_factor_gt 0.0493 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 Pb Pb 0.305901(10) 0.006568(8) 0.749520(15) 0.01661(6) Uani 1 1 d . . . Si1 Si 0.36815(10) 0.03338(8) 0.59632(8) 0.0237(4) Uani 1 1 d . . . Si2 Si 0.49741(10) 0.09321(8) 0.69206(8) 0.0221(4) Uani 1 1 d . . . Si3 Si 0.49661(10) -0.07676(8) 0.80910(8) 0.0196(4) Uani 1 1 d . . . Si4 Si 0.36448(10) -0.01836(8) 0.90389(7) 0.0219(4) Uani 1 1 d . . . P1 P 0.32108(10) 0.14717(8) 0.68875(8) 0.0226(4) Uani 1 1 d . . . P2 P 0.32158(9) -0.13352(7) 0.81169(7) 0.0185(3) Uani 1 1 d . . . B1 B 0.3018(5) 0.1581(4) 0.7781(4) 0.0266(16) Uani 1 1 d . . . H1A H 0.331(4) 0.203(3) 0.795(3) 0.05(2) Uiso 1 1 d . . . H1B H 0.232(3) 0.156(3) 0.783(2) 0.022(15) Uiso 1 1 d . . . H1C H 0.332(4) 0.118(3) 0.806(3) 0.041(19) Uiso 1 1 d . . . B2 B 0.3040(5) -0.1450(4) 0.7235(3) 0.0238(16) Uani 1 1 d . . . H2A H 0.326(3) -0.194(3) 0.709(3) 0.038(18) Uiso 1 1 d . . . H2B H 0.241(4) -0.139(3) 0.714(2) 0.026(16) Uiso 1 1 d . . . H2C H 0.336(3) -0.108(3) 0.702(2) 0.011(14) Uiso 1 1 d . . . O1 O 0.3480(4) -0.2575(3) 1.0175(3) 0.0738(18) Uani 1 1 d . . . C1 C 0.3844(3) 0.0749(3) 0.6737(3) 0.0162(13) Uani 1 1 d . . . C2 C 0.2193(3) 0.1407(3) 0.6516(3) 0.0296(16) Uani 1 1 d . . . H2D H 0.1882 0.1817 0.6584 0.044 Uiso 1 1 calc R . . H2E H 0.1888 0.1033 0.6694 0.044 Uiso 1 1 calc R . . H2F H 0.2266 0.1335 0.6071 0.044 Uiso 1 1 calc R . . C3 C 0.3615(4) 0.2217(3) 0.6521(3) 0.0300(16) Uani 1 1 d . . . H3A H 0.3245 0.2590 0.6606 0.045 Uiso 1 1 calc R . . H3B H 0.3652 0.2147 0.6074 0.045 Uiso 1 1 calc R . . H3C H 0.4167 0.2314 0.6686 0.045 Uiso 1 1 calc R . . C4 C 0.4496(4) -0.0315(3) 0.5802(3) 0.0360(16) Uani 1 1 d . . . H4A H 0.4382 -0.0526 0.5403 0.054 Uiso 1 1 calc R . . H4B H 0.4486 -0.0651 0.6129 0.054 Uiso 1 1 calc R . . H4C H 0.5042 -0.0105 0.5790 0.054 Uiso 1 1 calc R . . C5 C 0.3696(4) 0.0939(3) 0.5300(3) 0.0306(15) Uani 1 1 d . . . H5A H 0.3219 0.1236 0.5331 0.046 Uiso 1 1 calc R . . H5B H 0.3669 0.0695 0.4909 0.046 Uiso 1 1 calc R . . H5C H 0.4208 0.1199 0.5314 0.046 Uiso 1 1 calc R . . C6 C 0.2669(4) -0.0129(3) 0.5923(3) 0.0293(16) Uani 1 1 d . . . H6A H 0.2214 0.0173 0.6025 0.044 Uiso 1 1 calc R . . H6B H 0.2677 -0.0497 0.6218 0.044 Uiso 1 1 calc R . . H6C H 0.2590 -0.0302 0.5504 0.044 Uiso 1 1 calc R . . C7 C 0.5522(4) 0.1268(3) 0.6216(3) 0.0285(14) Uani 1 1 d . . . H7A H 0.5547 0.0924 0.5897 0.043 Uiso 1 1 calc R . . H7B H 0.6085 0.1403 0.6328 0.043 Uiso 1 1 calc R . . H7C H 0.5219 0.1652 0.6056 0.043 Uiso 1 1 calc R . . C8 C 0.5116(3) 0.1566(3) 0.7558(3) 0.0278(14) Uani 1 1 d . . . H8A H 0.5707 0.1647 0.7622 0.042 Uiso 1 1 calc R . . H8B H 0.4872 0.1397 0.7941 0.042 Uiso 1 1 calc R . . H8C H 0.4842 0.1980 0.7442 0.042 Uiso 1 1 calc R . . C9 C 0.5598(4) 0.0193(3) 0.7172(3) 0.0287(16) Uani 1 1 d . . . H9A H 0.5412 -0.0191 0.6924 0.034 Uiso 1 1 calc R . . H9B H 0.6182 0.0279 0.7058 0.034 Uiso 1 1 calc R . . C10 C 0.5584(4) -0.0018(3) 0.7858(3) 0.0237(16) Uani 1 1 d . . . H10A H 0.5375 0.0363 0.8100 0.028 Uiso 1 1 calc R . . H10B H 0.6163 -0.0094 0.7988 0.028 Uiso 1 1 calc R . . C11 C 0.5140(3) -0.1393(2) 0.7465(4) 0.0274(13) Uani 1 1 d . . . H11A H 0.5733 -0.1486 0.7428 0.041 Uiso 1 1 calc R . . H11B H 0.4933 -0.1218 0.7072 0.041 Uiso 1 1 calc R . . H11C H 0.4845 -0.1803 0.7566 0.041 Uiso 1 1 calc R . . C12 C 0.5521(4) -0.1100(3) 0.8793(3) 0.0279(14) Uani 1 1 d . . . H12A H 0.6085 -0.1231 0.8679 0.042 Uiso 1 1 calc R . . H12B H 0.5223 -0.1486 0.8954 0.042 Uiso 1 1 calc R . . H12C H 0.5545 -0.0756 0.9112 0.042 Uiso 1 1 calc R . . C14 C 0.3698(4) -0.0777(3) 0.9705(3) 0.0305(16) Uani 1 1 d . . . H14A H 0.4241 -0.0993 0.9710 0.046 Uiso 1 1 calc R . . H14B H 0.3265 -0.1114 0.9660 0.046 Uiso 1 1 calc R . . H14C H 0.3616 -0.0535 1.0092 0.046 Uiso 1 1 calc R . . C15 C 0.4421(4) 0.0488(3) 0.9189(3) 0.0309(14) Uani 1 1 d . . . H15A H 0.4980 0.0303 0.9168 0.046 Uiso 1 1 calc R . . H15B H 0.4327 0.0676 0.9600 0.046 Uiso 1 1 calc R . . H15C H 0.4361 0.0837 0.8877 0.046 Uiso 1 1 calc R . . C13 C 0.2602(4) 0.0243(3) 0.9082(3) 0.0270(15) Uani 1 1 d . . . H13A H 0.2561 0.0489 0.9471 0.041 Uiso 1 1 calc R . . H13B H 0.2162 -0.0090 0.9064 0.041 Uiso 1 1 calc R . . H13C H 0.2545 0.0550 0.8735 0.041 Uiso 1 1 calc R . . C16 C 0.3634(4) -0.2071(3) 0.8491(3) 0.0277(15) Uani 1 1 d . . . H16A H 0.3317 -0.2461 0.8361 0.042 Uiso 1 1 calc R . . H16B H 0.3594 -0.2021 0.8940 0.042 Uiso 1 1 calc R . . H16C H 0.4215 -0.2126 0.8373 0.042 Uiso 1 1 calc R . . C17 C 0.2203(3) -0.1295(3) 0.8484(3) 0.0289(16) Uani 1 1 d . . . H17A H 0.1881 -0.1688 0.8371 0.043 Uiso 1 1 calc R . . H17B H 0.1913 -0.0896 0.8344 0.043 Uiso 1 1 calc R . . H17C H 0.2272 -0.1279 0.8933 0.043 Uiso 1 1 calc R . . C18 C 0.3833(3) -0.0600(3) 0.8265(2) 0.0157(13) Uani 1 1 d . . . C19 C 0.4755(7) -0.2256(6) 1.0569(6) 0.127(5) Uani 1 1 d . . . H19A H 0.5209 -0.2393 1.0841 0.190 Uiso 1 1 calc R . . H19B H 0.4493 -0.1857 1.0736 0.190 Uiso 1 1 calc R . . H19C H 0.4973 -0.2163 1.0156 0.190 Uiso 1 1 calc R . . C20 C 0.4170(8) -0.2765(5) 1.0532(6) 0.107(4) Uani 1 1 d . . . H20A H 0.3984 -0.2883 1.0954 0.128 Uiso 1 1 calc R . . H20B H 0.4429 -0.3162 1.0346 0.128 Uiso 1 1 calc R . . C21 C 0.2878(7) -0.3083(4) 1.0183(5) 0.078(3) Uani 1 1 d . . . H21A H 0.2690 -0.3160 1.0613 0.093 Uiso 1 1 calc R . . H21B H 0.3122 -0.3500 1.0026 0.093 Uiso 1 1 calc R . . C22 C 0.2174(7) -0.2893(5) 0.9799(5) 0.089(3) Uani 1 1 d . . . H22A H 0.1741 -0.3231 0.9831 0.134 Uiso 1 1 calc R . . H22B H 0.2353 -0.2854 0.9368 0.134 Uiso 1 1 calc R . . H22C H 0.1956 -0.2466 0.9940 0.134 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 Pb 0.01345(9) 0.01905(10) 0.01732(9) 0.00130(12) -0.00023(15) 0.00028(8) Si1 0.0261(10) 0.0247(10) 0.0202(9) -0.0014(7) -0.0002(7) -0.0002(7) Si2 0.0198(10) 0.0215(9) 0.0250(10) 0.0015(7) 0.0002(7) 0.0001(7) Si3 0.0158(9) 0.0193(9) 0.0238(9) 0.0020(7) -0.0005(7) 0.0012(6) Si4 0.0249(10) 0.0230(10) 0.0179(9) -0.0021(7) -0.0021(7) 0.0026(7) P1 0.0239(10) 0.0197(8) 0.0242(9) 0.0005(7) 0.0012(7) 0.0032(6) P2 0.0183(9) 0.0182(8) 0.0188(8) 0.0006(7) -0.0006(7) -0.0014(6) B1 0.034(5) 0.021(4) 0.024(4) 0.001(3) 0.004(4) 0.003(3) B2 0.028(4) 0.025(4) 0.019(4) 0.001(3) -0.007(4) -0.005(3) O1 0.100(5) 0.053(4) 0.068(4) 0.000(3) -0.014(4) 0.002(4) C1 0.012(3) 0.016(3) 0.021(3) 0.001(2) -0.001(2) 0.004(2) C2 0.022(4) 0.035(4) 0.032(4) 0.006(3) 0.001(3) 0.008(3) C3 0.031(4) 0.022(4) 0.037(4) 0.006(3) 0.009(3) 0.000(3) C4 0.048(4) 0.029(4) 0.031(4) -0.005(3) 0.006(3) 0.001(3) C5 0.034(4) 0.038(4) 0.020(4) 0.003(3) -0.001(3) -0.004(3) C6 0.035(4) 0.029(4) 0.024(4) -0.001(3) -0.009(3) -0.002(3) C7 0.023(3) 0.031(4) 0.032(4) 0.005(3) 0.005(3) 0.000(3) C8 0.029(3) 0.023(3) 0.032(4) -0.001(3) -0.010(3) -0.002(2) C9 0.017(4) 0.024(4) 0.045(4) 0.001(3) 0.016(3) 0.002(3) C10 0.017(4) 0.026(4) 0.028(4) 0.002(3) 0.001(3) 0.001(3) C11 0.026(3) 0.022(3) 0.035(4) 0.001(4) 0.007(4) 0.003(2) C12 0.025(4) 0.028(3) 0.031(4) 0.006(3) 0.004(3) 0.007(3) C14 0.034(4) 0.031(4) 0.026(4) -0.003(3) -0.001(3) 0.007(3) C15 0.033(4) 0.034(4) 0.026(3) -0.008(3) -0.007(3) -0.002(3) C13 0.034(4) 0.035(4) 0.013(3) -0.003(3) 0.003(3) 0.006(3) C16 0.032(4) 0.023(3) 0.028(4) 0.002(3) 0.002(3) -0.003(3) C17 0.026(4) 0.025(4) 0.035(4) -0.001(3) 0.001(3) -0.008(3) C18 0.014(3) 0.010(3) 0.023(3) 0.003(2) -0.005(2) -0.004(2) C19 0.107(10) 0.082(9) 0.191(14) 0.009(9) -0.041(9) -0.008(7) C20 0.134(11) 0.069(8) 0.116(10) 0.015(7) -0.006(8) 0.011(7) C21 0.114(8) 0.038(5) 0.082(7) 0.002(5) 0.044(7) -0.007(6) C22 0.111(9) 0.053(6) 0.103(8) -0.026(6) 0.031(7) -0.025(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 Pb C1 2.492(5) . ? Pb C18 2.480(5) . ? Si1 C1 1.892(6) . ? Si1 C4 1.890(6) . ? Si1 C5 1.886(6) . ? Si1 C6 1.887(6) . ? Si2 C1 1.906(5) . ? Si2 C7 1.891(6) . ? Si2 C8 1.896(6) . ? Si2 C9 1.881(6) . ? Si3 C10 1.882(6) . ? Si3 C11 1.874(7) . ? Si3 C12 1.889(6) . ? Si3 C18 1.900(5) . ? Si4 C14 1.877(6) . ? Si4 C15 1.876(6) . ? Si4 C13 1.895(6) . ? Si4 C18 1.901(6) . ? P1 B1 1.971(8) . ? P1 C1 1.812(5) . ? P1 C2 1.837(6) . ? P1 C3 1.822(6) . ? P2 B2 1.945(7) . ? P2 C16 1.821(6) . ? P2 C17 1.821(6) . ? P2 C18 1.816(5) . ? B1 H1A 1.09(6) . ? B1 H1B 1.14(5) . ? B1 H1C 1.12(6) . ? B2 H2A 1.10(6) . ? B2 H2B 1.05(6) . ? B2 H2C 1.03(5) . ? O1 C20 1.412(11) . ? O1 C21 1.414(10) . ? C2 H2D 0.980 . ? C2 H2E 0.980 . ? C2 H2F 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C9 C10 1.546(7) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C13 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C19 H19A 0.980 . ? C19 H19B 0.980 . ? C19 H19C 0.980 . ? C19 C20 1.397(13) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.461(12) . ? C22 H22A 0.980 . ? C22 H22B 0.980 . ? C22 H22C 0.980 . ? 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 Pb C18 119.04(15) . . ? C1 Si1 C4 111.9(3) . . ? C1 Si1 C5 112.7(3) . . ? C1 Si1 C6 112.4(3) . . ? C4 Si1 C5 107.4(3) . . ? C4 Si1 C6 104.7(3) . . ? C5 Si1 C6 107.2(3) . . ? C1 Si2 C7 110.5(3) . . ? C1 Si2 C8 113.5(2) . . ? C1 Si2 C9 114.9(3) . . ? C7 Si2 C8 106.8(3) . . ? C7 Si2 C9 105.4(3) . . ? C8 Si2 C9 105.0(3) . . ? C10 Si3 C11 105.5(3) . . ? C10 Si3 C12 104.4(3) . . ? C10 Si3 C18 114.9(3) . . ? C11 Si3 C12 105.8(3) . . ? C11 Si3 C18 114.0(2) . . ? C12 Si3 C18 111.2(3) . . ? C14 Si4 C15 107.3(3) . . ? C14 Si4 C13 107.0(3) . . ? C14 Si4 C18 112.8(3) . . ? C15 Si4 C13 104.9(3) . . ? C15 Si4 C18 111.4(3) . . ? C13 Si4 C18 112.8(2) . . ? B1 P1 C1 110.8(3) . . ? B1 P1 C2 107.2(3) . . ? B1 P1 C3 113.1(3) . . ? C1 P1 C2 111.7(3) . . ? C1 P1 C3 112.5(3) . . ? C2 P1 C3 100.9(3) . . ? B2 P2 C16 113.2(3) . . ? B2 P2 C17 107.6(3) . . ? B2 P2 C18 110.5(3) . . ? C16 P2 C17 100.1(3) . . ? C16 P2 C18 112.5(3) . . ? C17 P2 C18 112.4(3) . . ? P1 B1 H1A 111(3) . . ? P1 B1 H1B 104(3) . . ? P1 B1 H1C 112(3) . . ? H1A B1 H1B 115(4) . . ? H1A B1 H1C 104(5) . . ? H1B B1 H1C 111(4) . . ? P2 B2 H2A 110(3) . . ? P2 B2 H2B 108(3) . . ? P2 B2 H2C 107(3) . . ? H2A B2 H2B 112(4) . . ? H2A B2 H2C 111(4) . . ? H2B B2 H2C 109(4) . . ? C20 O1 C21 109.9(8) . . ? Pb C1 Si1 105.5(2) . . ? Pb C1 Si2 117.3(2) . . ? Pb C1 P1 92.2(2) . . ? Si1 C1 Si2 113.8(3) . . ? Si1 C1 P1 115.9(3) . . ? Si2 C1 P1 110.4(3) . . ? P1 C2 H2D 109.5 . . ? P1 C2 H2E 109.5 . . ? P1 C2 H2F 109.5 . . ? H2D C2 H2E 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 107.5 . . ? Si2 C9 H9B 107.5 . . ? Si2 C9 C10 119.2(4) . . ? H9A C9 H9B 107.0 . . ? H9A C9 C10 107.5 . . ? H9B C9 C10 107.5 . . ? Si3 C10 C9 119.2(5) . . ? Si3 C10 H10A 107.5 . . ? Si3 C10 H10B 107.5 . . ? C9 C10 H10A 107.5 . . ? C9 C10 H10B 107.5 . . ? H10A C10 H10B 107.0 . . ? Si3 C11 H11A 109.5 . . ? Si3 C11 H11B 109.5 . . ? Si3 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si3 C12 H12A 109.5 . . ? Si3 C12 H12B 109.5 . . ? Si3 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si4 C14 H14A 109.5 . . ? Si4 C14 H14B 109.5 . . ? Si4 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si4 C15 H15A 109.5 . . ? Si4 C15 H15B 109.5 . . ? Si4 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si4 C13 H13A 109.5 . . ? Si4 C13 H13B 109.5 . . ? Si4 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C16 H16A 109.5 . . ? P2 C16 H16B 109.5 . . ? P2 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P2 C17 H17A 109.5 . . ? P2 C17 H17B 109.5 . . ? P2 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Pb C18 Si3 116.7(2) . . ? Pb C18 Si4 105.8(2) . . ? Pb C18 P2 92.7(2) . . ? Si3 C18 Si4 114.1(3) . . ? Si3 C18 P2 110.5(3) . . ? Si4 C18 P2 115.4(3) . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19A C19 C20 109.5 . . ? H19B C19 H19C 109.5 . . ? H19B C19 C20 109.5 . . ? H19C C19 C20 109.5 . . ? O1 C20 C19 111.5(9) . . ? O1 C20 H20A 109.3 . . ? O1 C20 H20B 109.3 . . ? C19 C20 H20A 109.3 . . ? C19 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? O1 C21 H21A 109.7 . . ? O1 C21 H21B 109.7 . . ? O1 C21 C22 109.7(8) . . ? H21A C21 H21B 108.2 . . ? H21A C21 C22 109.7 . . ? H21B C21 C22 109.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? 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 B1 P1 C1 Pb 43.3(3) . . . . ? B1 P1 C1 Si1 151.8(3) . . . . ? B1 P1 C1 Si2 -76.9(4) . . . . ? C2 P1 C1 Pb -76.2(3) . . . . ? C2 P1 C1 Si1 32.3(4) . . . . ? C2 P1 C1 Si2 163.6(3) . . . . ? C3 P1 C1 Pb 171.1(2) . . . . ? C3 P1 C1 Si1 -80.4(4) . . . . ? C3 P1 C1 Si2 50.8(4) . . . . ? C4 Si1 C1 Pb -89.6(3) . . . . ? C4 Si1 C1 Si2 40.4(4) . . . . ? C4 Si1 C1 P1 170.0(3) . . . . ? C5 Si1 C1 Pb 149.2(2) . . . . ? C5 Si1 C1 Si2 -80.8(3) . . . . ? C5 Si1 C1 P1 48.8(4) . . . . ? C6 Si1 C1 Pb 27.9(3) . . . . ? C6 Si1 C1 Si2 157.9(3) . . . . ? C6 Si1 C1 P1 -72.5(4) . . . . ? C7 Si2 C1 Pb 166.3(3) . . . . ? C7 Si2 C1 Si1 42.4(4) . . . . ? C7 Si2 C1 P1 -89.9(3) . . . . ? C8 Si2 C1 Pb -73.8(3) . . . . ? C8 Si2 C1 Si1 162.4(3) . . . . ? C8 Si2 C1 P1 30.0(4) . . . . ? C9 Si2 C1 Pb 47.1(4) . . . . ? C9 Si2 C1 Si1 -76.7(4) . . . . ? C9 Si2 C1 P1 150.9(3) . . . . ? C18 Pb C1 Si1 110.5(2) . . . . ? C18 Pb C1 Si2 -17.4(4) . . . . ? C18 Pb C1 P1 -131.77(19) . . . . ? C1 Si2 C9 C10 -84.7(6) . . . . ? C7 Si2 C9 C10 153.3(5) . . . . ? C8 Si2 C9 C10 40.7(6) . . . . ? Si2 C9 C10 Si3 104.6(4) . . . . ? C11 Si3 C10 C9 40.2(6) . . . . ? C12 Si3 C10 C9 151.4(5) . . . . ? C18 Si3 C10 C9 -86.4(6) . . . . ? B2 P2 C18 Pb 42.9(3) . . . . ? B2 P2 C18 Si3 -77.0(4) . . . . ? B2 P2 C18 Si4 151.8(3) . . . . ? C16 P2 C18 Pb 170.5(2) . . . . ? C16 P2 C18 Si3 50.6(4) . . . . ? C16 P2 C18 Si4 -80.6(4) . . . . ? C17 P2 C18 Pb -77.3(3) . . . . ? C17 P2 C18 Si3 162.8(3) . . . . ? C17 P2 C18 Si4 31.5(4) . . . . ? C10 Si3 C18 Pb 48.4(4) . . . . ? C10 Si3 C18 Si4 -75.6(4) . . . . ? C10 Si3 C18 P2 152.5(3) . . . . ? C11 Si3 C18 Pb -73.7(3) . . . . ? C11 Si3 C18 Si4 162.3(3) . . . . ? C11 Si3 C18 P2 30.4(4) . . . . ? C12 Si3 C18 Pb 166.8(3) . . . . ? C12 Si3 C18 Si4 42.8(4) . . . . ? C12 Si3 C18 P2 -89.1(3) . . . . ? C14 Si4 C18 Pb 151.6(2) . . . . ? C14 Si4 C18 Si3 -78.8(3) . . . . ? C14 Si4 C18 P2 50.8(4) . . . . ? C15 Si4 C18 Pb -87.6(3) . . . . ? C15 Si4 C18 Si3 42.0(4) . . . . ? C15 Si4 C18 P2 171.6(3) . . . . ? C13 Si4 C18 Pb 30.1(3) . . . . ? C13 Si4 C18 Si3 159.8(3) . . . . ? C13 Si4 C18 P2 -70.7(4) . . . . ? C1 Pb C18 Si3 -18.2(3) . . . . ? C1 Pb C18 Si4 109.9(2) . . . . ? C1 Pb C18 P2 -132.79(19) . . . . ? C21 O1 C20 C19 -176.0(10) . . . . ? C20 O1 C21 C22 -178.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.179 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.120 #===END