# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_kt002twin _database_code_depnum_ccdc_archive 'CCDC 899513' #TrackingRef 'kt002twin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H39 B F12 P Si4' _chemical_formula_weight 781.75 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.0075(12) _cell_length_b 14.0075(12) _cell_length_c 34.296(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5827.7(10) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9976 _cell_measurement_theta_min 2.902 _cell_measurement_theta_max 27.284 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2418 _exptl_absorpt_coefficient_mu 0.272 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2998 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.45 _reflns_number_total 2998 _reflns_number_gt 2674 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+10.8148P] 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 2998 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.3333 0.6667 0.04210(5) 0.0150(3) Uani 1 3 d S . . Si1 Si 0.3333 0.6667 -0.02499(5) 0.0204(4) Uani 1 3 d S . . Si2 Si 0.25312(9) 0.48790(9) 0.06475(4) 0.0233(2) Uani 1 1 d . . . C19 C 0.4262(5) 0.8095(4) -0.04134(14) 0.0364(11) Uani 1 1 d . . . H19A H 0.4214 0.8136 -0.0692 0.055 Uiso 1 1 calc R . . H19B H 0.5006 0.8316 -0.0341 0.055 Uiso 1 1 calc R . . H19C H 0.4048 0.8578 -0.0292 0.055 Uiso 1 1 calc R . . C22 C 0.3567(5) 0.4424(4) 0.05865(16) 0.0383(11) Uani 1 1 d . . . H22A H 0.3233 0.3654 0.0648 0.057 Uiso 1 1 calc R . . H22B H 0.4178 0.4840 0.0759 0.057 Uiso 1 1 calc R . . H22C H 0.3824 0.4545 0.0322 0.057 Uiso 1 1 calc R . . C23 C 0.1271(4) 0.3989(4) 0.03523(16) 0.0387(11) Uani 1 1 d . . . H23A H 0.1483 0.3922 0.0092 0.058 Uiso 1 1 calc R . . H23B H 0.0811 0.4316 0.0344 0.058 Uiso 1 1 calc R . . H23C H 0.0872 0.3272 0.0469 0.058 Uiso 1 1 calc R . . C24 C 0.2187(5) 0.4887(4) 0.11740(13) 0.0350(11) Uani 1 1 d . . . H24A H 0.1669 0.5143 0.1199 0.052 Uiso 1 1 calc R . . H24B H 0.2846 0.5369 0.1316 0.052 Uiso 1 1 calc R . . H24C H 0.1869 0.4154 0.1277 0.052 Uiso 1 1 calc R . . F1 F 0.1395(2) -0.0673(2) 0.19678(8) 0.0331(6) Uani 1 1 d . . . F2 F 0.3440(2) -0.0132(3) 0.17967(9) 0.0382(7) Uani 1 1 d . . . F3 F 0.3359(3) 0.1866(3) 0.06989(10) 0.0496(9) Uani 1 1 d . . . F4 F 0.1327(3) 0.1369(3) 0.08718(9) 0.0443(8) Uani 1 1 d . . . C1 C 0.1247(3) 0.0327(3) 0.14344(11) 0.0215(7) Uani 1 1 d . . . C2 C 0.1847(3) -0.0034(3) 0.16497(12) 0.0237(8) Uani 1 1 d . . . C3 C 0.2919(4) 0.0234(4) 0.15606(13) 0.0256(9) Uani 1 1 d . . . C4 C 0.3460(4) 0.0876(4) 0.12481(14) 0.0274(9) Uani 1 1 d . . . H4 H 0.4182 0.1067 0.1190 0.033 Uiso 1 1 calc R . . C5 C 0.2877(4) 0.1233(4) 0.10205(14) 0.0296(9) Uani 1 1 d . . . C6 C 0.1816(4) 0.0969(4) 0.11172(13) 0.0270(9) Uani 1 1 d . . . B1 B 0.0000 0.0000 0.1573(2) 0.0230(15) Uani 1 3 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0154(5) 0.0154(5) 0.0141(8) 0.000 0.000 0.0077(2) Si1 0.0236(6) 0.0236(6) 0.0139(9) 0.000 0.000 0.0118(3) Si2 0.0267(6) 0.0172(5) 0.0232(6) 0.0041(4) 0.0037(4) 0.0089(4) C19 0.046(3) 0.033(2) 0.025(2) 0.0099(19) 0.0083(19) 0.015(2) C22 0.052(3) 0.033(3) 0.043(3) 0.008(2) 0.006(2) 0.030(2) C23 0.037(3) 0.026(2) 0.040(3) -0.004(2) -0.003(2) 0.006(2) C24 0.039(3) 0.036(3) 0.027(2) 0.0124(19) 0.0073(19) 0.016(2) F1 0.0371(15) 0.0383(15) 0.0270(13) 0.0100(11) 0.0027(11) 0.0212(13) F2 0.0408(16) 0.0481(17) 0.0379(16) -0.0014(13) -0.0099(12) 0.0315(14) F3 0.0444(18) 0.058(2) 0.053(2) 0.0314(16) 0.0264(15) 0.0311(16) F4 0.0439(17) 0.065(2) 0.0399(16) 0.0299(15) 0.0132(13) 0.0388(17) C1 0.0223(18) 0.0209(17) 0.0199(18) -0.0004(14) -0.0011(14) 0.0098(15) C2 0.026(2) 0.0211(18) 0.024(2) 0.0012(15) -0.0012(16) 0.0115(16) C3 0.030(2) 0.023(2) 0.030(2) -0.0068(16) -0.0057(17) 0.0183(18) C4 0.022(2) 0.024(2) 0.036(2) -0.0036(17) 0.0013(17) 0.0116(16) C5 0.030(2) 0.026(2) 0.034(2) 0.0050(17) 0.0074(18) 0.0153(18) C6 0.029(2) 0.028(2) 0.028(2) 0.0044(17) -0.0017(17) 0.0175(18) B1 0.023(2) 0.023(2) 0.022(4) 0.000 0.000 0.0117(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 Si1 2.301(3) . ? P1 Si2 2.3071(12) 3_565 ? P1 Si2 2.3071(12) 2_665 ? P1 Si2 2.3071(12) . ? Si1 C19 1.846(5) 2_665 ? Si1 C19 1.846(5) . ? Si1 C19 1.846(5) 3_565 ? Si2 C22 1.865(5) . ? Si2 C23 1.870(5) . ? Si2 C24 1.870(5) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? F1 C2 1.351(5) . ? F2 C3 1.350(5) . ? F3 C5 1.364(5) . ? F4 C6 1.369(5) . ? C1 C6 1.382(6) . ? C1 C2 1.390(5) . ? C1 B1 1.640(5) . ? C2 C3 1.388(6) . ? C3 C4 1.360(6) . ? C4 C5 1.390(7) . ? C4 H4 0.9300 . ? C5 C6 1.381(6) . ? B1 C1 1.640(5) 3 ? B1 C1 1.640(5) 2 ? 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 Si1 P1 Si2 109.68(5) . 3_565 ? Si1 P1 Si2 109.68(5) . 2_665 ? Si2 P1 Si2 109.26(5) 3_565 2_665 ? Si1 P1 Si2 109.68(5) . . ? Si2 P1 Si2 109.26(5) 3_565 . ? Si2 P1 Si2 109.26(5) 2_665 . ? C19 Si1 C19 111.20(15) 2_665 . ? C19 Si1 C19 111.20(15) 2_665 3_565 ? C19 Si1 C19 111.20(15) . 3_565 ? C19 Si1 P1 107.68(16) 2_665 . ? C19 Si1 P1 107.68(16) . . ? C19 Si1 P1 107.68(16) 3_565 . ? C22 Si2 C23 110.4(3) . . ? C22 Si2 C24 110.9(2) . . ? C23 Si2 C24 111.5(3) . . ? C22 Si2 P1 107.03(18) . . ? C23 Si2 P1 109.06(18) . . ? C24 Si2 P1 107.79(17) . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C6 C1 C2 113.5(4) . . ? C6 C1 B1 126.6(4) . . ? C2 C1 B1 119.8(4) . . ? F1 C2 C3 116.3(4) . . ? F1 C2 C1 120.1(4) . . ? C3 C2 C1 123.6(4) . . ? F2 C3 C4 119.7(4) . . ? F2 C3 C2 118.8(4) . . ? C4 C3 C2 121.4(4) . . ? C3 C4 C5 116.6(4) . . ? C3 C4 H4 121.7 . . ? C5 C4 H4 121.7 . . ? F3 C5 C6 119.0(4) . . ? F3 C5 C4 119.9(4) . . ? C6 C5 C4 121.0(4) . . ? F4 C6 C5 115.7(4) . . ? F4 C6 C1 120.5(4) . . ? C5 C6 C1 123.8(4) . . ? C1 B1 C1 111.9(3) 3 . ? C1 B1 C1 111.9(3) 3 2 ? C1 B1 C1 111.9(3) . 2 ? 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 Si2 P1 Si1 C19 -46.80(19) 3_565 . . 2_665 ? Si2 P1 Si1 C19 -166.80(19) 2_665 . . 2_665 ? Si2 P1 Si1 C19 73.20(19) . . . 2_665 ? Si2 P1 Si1 C19 73.20(19) 3_565 . . . ? Si2 P1 Si1 C19 -46.80(19) 2_665 . . . ? Si2 P1 Si1 C19 -166.80(19) . . . . ? Si2 P1 Si1 C19 -166.80(19) 3_565 . . 3_565 ? Si2 P1 Si1 C19 73.20(19) 2_665 . . 3_565 ? Si2 P1 Si1 C19 -46.80(19) . . . 3_565 ? Si1 P1 Si2 C22 76.5(2) . . . . ? Si2 P1 Si2 C22 -163.30(19) 3_565 . . . ? Si2 P1 Si2 C22 -43.8(2) 2_665 . . . ? Si1 P1 Si2 C23 -42.93(19) . . . . ? Si2 P1 Si2 C23 77.3(2) 3_565 . . . ? Si2 P1 Si2 C23 -163.2(2) 2_665 . . . ? Si1 P1 Si2 C24 -164.15(18) . . . . ? Si2 P1 Si2 C24 -43.9(2) 3_565 . . . ? Si2 P1 Si2 C24 75.60(19) 2_665 . . . ? C6 C1 C2 F1 -179.8(4) . . . . ? B1 C1 C2 F1 1.4(6) . . . . ? C6 C1 C2 C3 1.0(6) . . . . ? B1 C1 C2 C3 -177.8(4) . . . . ? F1 C2 C3 F2 -1.4(6) . . . . ? C1 C2 C3 F2 177.8(4) . . . . ? F1 C2 C3 C4 -179.7(4) . . . . ? C1 C2 C3 C4 -0.5(7) . . . . ? F2 C3 C4 C5 -179.3(4) . . . . ? C2 C3 C4 C5 -1.0(7) . . . . ? C3 C4 C5 F3 -179.0(4) . . . . ? C3 C4 C5 C6 1.8(7) . . . . ? F3 C5 C6 F4 0.6(7) . . . . ? C4 C5 C6 F4 179.8(4) . . . . ? F3 C5 C6 C1 179.4(4) . . . . ? C4 C5 C6 C1 -1.4(7) . . . . ? C2 C1 C6 F4 178.7(4) . . . . ? B1 C1 C6 F4 -2.7(7) . . . . ? C2 C1 C6 C5 -0.1(7) . . . . ? B1 C1 C6 C5 178.6(4) . . . . ? C6 C1 B1 C1 100.2(4) . . . 3 ? C2 C1 B1 C1 -81.2(7) . . . 3 ? C6 C1 B1 C1 -26.4(7) . . . 2 ? C2 C1 B1 C1 152.2(4) . . . 2 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.291 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.081 data_kt003_0m _database_code_depnum_ccdc_archive 'CCDC 899514' #TrackingRef 'kt003_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H30 B F12 O2 P Si3' _chemical_formula_weight 752.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(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 9.5675(4) _cell_length_b 19.0878(8) _cell_length_c 18.8223(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.567(2) _cell_angle_gamma 90.00 _cell_volume 3430.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9924 _cell_measurement_theta_min 2.168 _cell_measurement_theta_max 26.848 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.276 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9809 _exptl_absorpt_correction_T_max 0.9890 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56358 _diffrn_reflns_av_R_equivalents 0.0878 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7863 _reflns_number_gt 4756 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+1.2068P] 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 7863 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 C1 C 0.6998(2) 0.67453(12) 0.75583(13) 0.0163(5) Uani 1 1 d . . . P1 P 0.65854(6) 0.59652(3) 0.80643(3) 0.01820(15) Uani 1 1 d . . . B1 B 0.8043(3) 0.79722(14) 0.75234(15) 0.0187(6) Uani 1 1 d . . . O1 O 0.77144(15) 0.72371(8) 0.78556(8) 0.0167(4) Uani 1 1 d . . . O2 O 0.65882(16) 0.68140(8) 0.68873(8) 0.0192(4) Uani 1 1 d . . . Si1 Si 0.79179(7) 0.61094(4) 0.91051(4) 0.02067(17) Uani 1 1 d . . . C2 C 0.9714(3) 0.58649(14) 0.88654(15) 0.0308(7) Uani 1 1 d . . . H1 H 1.0059 0.6215 0.8537 0.046 Uiso 1 1 calc . . . H2 H 0.9688 0.5404 0.8635 0.046 Uiso 1 1 calc . . . H3 H 1.0340 0.5847 0.9297 0.046 Uiso 1 1 calc . . . C3 C 0.7881(3) 0.69923(13) 0.95218(13) 0.0258(6) Uani 1 1 d . . . H4 H 0.8245 0.7340 0.9197 0.039 Uiso 1 1 calc . . . H5 H 0.8463 0.6990 0.9969 0.039 Uiso 1 1 calc . . . H6 H 0.6915 0.7113 0.9618 0.039 Uiso 1 1 calc . . . C4 C 0.7220(3) 0.54494(13) 0.97168(14) 0.0279(6) Uani 1 1 d . . . H7 H 0.6280 0.5589 0.9840 0.042 Uiso 1 1 calc . . . H8 H 0.7839 0.5420 1.0151 0.042 Uiso 1 1 calc . . . H9 H 0.7173 0.4991 0.9482 0.042 Uiso 1 1 calc . . . Si2 Si 0.43082(7) 0.62046(4) 0.83054(4) 0.02116(17) Uani 1 1 d . . . C5 C 0.4163(3) 0.67739(14) 0.90959(15) 0.0333(7) Uani 1 1 d . . . H10 H 0.4555 0.7236 0.9001 0.050 Uiso 1 1 calc . . . H11 H 0.4682 0.6563 0.9507 0.050 Uiso 1 1 calc . . . H12 H 0.3176 0.6823 0.9197 0.050 Uiso 1 1 calc . . . C6 C 0.3373(3) 0.66366(15) 0.75262(15) 0.0351(7) Uani 1 1 d . . . H13 H 0.3785 0.7099 0.7452 0.053 Uiso 1 1 calc . . . H14 H 0.2381 0.6690 0.7616 0.053 Uiso 1 1 calc . . . H15 H 0.3463 0.6348 0.7100 0.053 Uiso 1 1 calc . . . C7 C 0.3592(3) 0.53238(14) 0.84737(15) 0.0340(7) Uani 1 1 d . . . H16 H 0.3672 0.5030 0.8051 0.051 Uiso 1 1 calc . . . H17 H 0.2604 0.5365 0.8578 0.051 Uiso 1 1 calc . . . H18 H 0.4120 0.5110 0.8881 0.051 Uiso 1 1 calc . . . Si3 Si 0.61156(7) 0.63089(4) 0.61478(4) 0.02356(17) Uani 1 1 d . . . C8 C 0.5464(3) 0.54305(15) 0.63714(16) 0.0453(8) Uani 1 1 d . . . H19 H 0.6215 0.5165 0.6626 0.068 Uiso 1 1 calc . . . H20 H 0.5159 0.5183 0.5933 0.068 Uiso 1 1 calc . . . H21 H 0.4671 0.5478 0.6674 0.068 Uiso 1 1 calc . . . C9 C 0.4778(3) 0.68509(15) 0.56639(14) 0.0355(7) Uani 1 1 d . . . H22 H 0.5178 0.7309 0.5559 0.053 Uiso 1 1 calc . . . H23 H 0.3977 0.6914 0.5958 0.053 Uiso 1 1 calc . . . H24 H 0.4468 0.6618 0.5217 0.053 Uiso 1 1 calc . . . C10 C 0.7701(3) 0.62295(16) 0.56429(15) 0.0414(8) Uani 1 1 d . . . H25 H 0.8039 0.6698 0.5526 0.062 Uiso 1 1 calc . . . H26 H 0.7477 0.5968 0.5202 0.062 Uiso 1 1 calc . . . H27 H 0.8430 0.5981 0.5932 0.062 Uiso 1 1 calc . . . C11 C 0.9110(2) 0.78894(12) 0.68873(12) 0.0165(5) Uani 1 1 d . . . C12 C 0.9808(2) 0.72854(12) 0.66952(13) 0.0186(6) Uani 1 1 d . . . C13 C 1.0753(2) 0.72718(12) 0.61678(13) 0.0198(6) Uani 1 1 d . . . C14 C 1.1107(2) 0.78691(13) 0.58155(13) 0.0221(6) Uani 1 1 d . . . H28 H 1.1760 0.7862 0.5456 0.027 Uiso 1 1 calc . . . C15 C 1.0468(2) 0.84794(13) 0.60098(13) 0.0209(6) Uani 1 1 d . . . C16 C 0.9516(2) 0.84829(12) 0.65247(13) 0.0185(5) Uani 1 1 d . . . F1 F 0.95837(13) 0.66650(7) 0.70220(7) 0.0233(3) Uani 1 1 d . . . F2 F 1.13293(14) 0.66505(7) 0.60031(7) 0.0286(4) Uani 1 1 d . . . F3 F 1.07716(15) 0.90903(7) 0.56841(8) 0.0326(4) Uani 1 1 d . . . F4 F 0.89324(14) 0.91097(7) 0.66865(7) 0.0256(3) Uani 1 1 d . . . C17 C 0.6489(2) 0.82947(11) 0.73164(13) 0.0170(5) Uani 1 1 d . . . C18 C 0.5900(2) 0.84333(12) 0.66419(13) 0.0192(6) Uani 1 1 d . . . C19 C 0.4552(3) 0.86750(13) 0.65132(14) 0.0241(6) Uani 1 1 d . . . C20 C 0.3690(3) 0.87924(13) 0.70522(16) 0.0292(6) Uani 1 1 d . . . H29 H 0.2763 0.8964 0.6962 0.035 Uiso 1 1 calc . . . C21 C 0.4225(3) 0.86518(13) 0.77288(14) 0.0257(6) Uani 1 1 d . . . C22 C 0.5570(2) 0.84100(12) 0.78500(13) 0.0211(6) Uani 1 1 d . . . F5 F 0.66480(14) 0.83266(7) 0.60641(7) 0.0266(3) Uani 1 1 d . . . F6 F 0.40812(15) 0.87969(8) 0.58294(8) 0.0372(4) Uani 1 1 d . . . F7 F 0.34206(15) 0.87486(8) 0.82880(8) 0.0395(4) Uani 1 1 d . . . F8 F 0.60098(14) 0.82832(7) 0.85412(7) 0.0290(4) Uani 1 1 d . . . C23 C 0.8916(2) 0.83971(12) 0.81682(12) 0.0178(5) Uani 1 1 d . . . C24 C 1.0066(2) 0.80979(12) 0.85311(13) 0.0185(5) Uani 1 1 d . . . C25 C 1.0839(2) 0.84113(13) 0.90825(13) 0.0224(6) Uani 1 1 d . . . C26 C 1.0529(3) 0.90764(14) 0.93007(14) 0.0289(6) Uani 1 1 d . . . H30 H 1.1051 0.9299 0.9683 0.035 Uiso 1 1 calc . . . C27 C 0.9425(3) 0.94024(13) 0.89368(14) 0.0283(6) Uani 1 1 d . . . C28 C 0.8654(2) 0.90787(13) 0.83886(13) 0.0215(6) Uani 1 1 d . . . F9 F 1.04718(14) 0.74408(7) 0.83442(7) 0.0261(3) Uani 1 1 d . . . F10 F 1.19250(14) 0.80606(8) 0.94118(7) 0.0311(4) Uani 1 1 d . . . F11 F 0.90650(17) 1.00637(8) 0.91244(9) 0.0454(5) Uani 1 1 d . . . F12 F 0.75951(15) 0.94600(7) 0.80719(8) 0.0305(4) 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 C1 0.0126(11) 0.0175(13) 0.0188(15) -0.0016(11) 0.0013(10) 0.0030(10) P1 0.0191(3) 0.0163(3) 0.0193(4) 0.0016(3) 0.0021(3) -0.0009(3) B1 0.0228(15) 0.0151(14) 0.0181(17) 0.0015(12) 0.0011(12) -0.0013(12) O1 0.0178(8) 0.0157(9) 0.0164(9) 0.0000(7) 0.0007(7) -0.0011(7) O2 0.0234(9) 0.0174(9) 0.0164(10) 0.0009(7) -0.0018(7) -0.0021(7) Si1 0.0205(4) 0.0223(4) 0.0191(4) 0.0040(3) 0.0006(3) 0.0009(3) C2 0.0240(14) 0.0359(16) 0.0321(17) 0.0034(13) -0.0014(12) 0.0019(12) C3 0.0271(14) 0.0283(15) 0.0217(16) 0.0018(12) -0.0016(12) -0.0016(12) C4 0.0319(15) 0.0274(15) 0.0242(16) 0.0043(12) -0.0006(12) 0.0028(12) Si2 0.0191(3) 0.0226(4) 0.0221(4) 0.0019(3) 0.0041(3) 0.0001(3) C5 0.0320(16) 0.0319(16) 0.0368(18) -0.0038(13) 0.0083(13) 0.0071(12) C6 0.0241(14) 0.0462(18) 0.0351(18) 0.0084(14) 0.0015(13) 0.0092(13) C7 0.0266(15) 0.0336(16) 0.0424(19) 0.0034(14) 0.0080(13) -0.0048(12) Si3 0.0270(4) 0.0240(4) 0.0194(4) -0.0028(3) -0.0009(3) -0.0034(3) C8 0.072(2) 0.0308(17) 0.0326(19) -0.0055(14) -0.0041(16) -0.0140(16) C9 0.0359(16) 0.0446(18) 0.0251(17) 0.0039(14) -0.0059(13) -0.0046(14) C10 0.0368(17) 0.058(2) 0.0292(18) -0.0182(16) 0.0010(14) 0.0021(15) C11 0.0162(12) 0.0180(13) 0.0147(14) -0.0024(10) -0.0033(10) -0.0021(10) C12 0.0187(12) 0.0165(13) 0.0203(15) 0.0021(11) -0.0009(11) -0.0015(10) C13 0.0164(12) 0.0217(14) 0.0213(15) -0.0056(11) 0.0000(11) 0.0031(10) C14 0.0169(12) 0.0308(15) 0.0187(15) -0.0028(12) 0.0025(11) -0.0042(11) C15 0.0217(13) 0.0214(14) 0.0196(15) 0.0027(11) 0.0013(11) -0.0069(11) C16 0.0170(12) 0.0174(13) 0.0209(15) 0.0000(11) -0.0006(11) 0.0002(10) F1 0.0265(8) 0.0169(7) 0.0272(9) 0.0026(6) 0.0061(6) 0.0025(6) F2 0.0280(8) 0.0274(8) 0.0313(9) -0.0063(7) 0.0092(7) 0.0064(7) F3 0.0368(9) 0.0270(8) 0.0353(10) 0.0080(7) 0.0120(7) -0.0071(7) F4 0.0300(8) 0.0156(7) 0.0319(9) 0.0007(6) 0.0077(7) 0.0016(6) C17 0.0194(12) 0.0110(12) 0.0208(15) -0.0010(10) 0.0031(11) -0.0025(10) C18 0.0220(13) 0.0173(13) 0.0190(15) -0.0019(11) 0.0059(11) 0.0002(10) C19 0.0228(13) 0.0229(14) 0.0257(16) 0.0028(12) -0.0059(12) -0.0007(11) C20 0.0180(13) 0.0264(15) 0.0431(19) -0.0018(14) 0.0020(13) 0.0025(11) C21 0.0241(14) 0.0256(15) 0.0287(17) -0.0040(13) 0.0125(12) -0.0012(11) C22 0.0243(14) 0.0197(13) 0.0194(16) 0.0001(11) 0.0010(11) -0.0019(11) F5 0.0264(8) 0.0364(9) 0.0171(8) 0.0016(7) 0.0021(6) 0.0025(7) F6 0.0321(9) 0.0453(10) 0.0326(10) 0.0051(8) -0.0098(7) 0.0078(7) F7 0.0276(8) 0.0489(10) 0.0439(10) -0.0054(8) 0.0174(7) 0.0037(8) F8 0.0294(8) 0.0367(9) 0.0216(9) 0.0013(7) 0.0073(7) 0.0023(7) C23 0.0199(12) 0.0174(13) 0.0166(14) 0.0011(11) 0.0062(10) -0.0014(10) C24 0.0216(13) 0.0165(13) 0.0179(14) -0.0011(11) 0.0053(11) -0.0015(10) C25 0.0206(13) 0.0284(15) 0.0179(15) 0.0016(12) -0.0002(11) -0.0030(11) C26 0.0321(15) 0.0333(16) 0.0212(16) -0.0084(13) 0.0000(12) -0.0064(13) C27 0.0390(16) 0.0184(14) 0.0280(17) -0.0074(12) 0.0052(13) 0.0000(12) C28 0.0214(13) 0.0213(13) 0.0217(15) 0.0010(12) 0.0001(11) 0.0019(11) F9 0.0252(8) 0.0208(8) 0.0318(9) -0.0048(7) -0.0010(7) 0.0045(6) F10 0.0258(8) 0.0386(9) 0.0277(9) 0.0006(7) -0.0081(7) 0.0018(7) F11 0.0570(11) 0.0260(9) 0.0516(12) -0.0209(8) -0.0078(9) 0.0059(8) F12 0.0349(9) 0.0200(8) 0.0357(10) -0.0042(7) -0.0055(7) 0.0071(7) _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 C1 O1 1.271(3) . ? C1 O2 1.306(3) . ? C1 P1 1.824(2) . ? P1 Si1 2.2865(9) . ? P1 Si2 2.2989(9) . ? B1 O1 1.576(3) . ? B1 C11 1.628(4) . ? B1 C17 1.634(4) . ? B1 C23 1.644(4) . ? O2 Si3 1.7300(17) . ? Si1 C4 1.859(3) . ? Si1 C3 1.860(3) . ? Si1 C2 1.863(3) . ? C2 H1 0.9800 . ? C2 H2 0.9800 . ? C2 H3 0.9800 . ? C3 H4 0.9800 . ? C3 H5 0.9800 . ? C3 H6 0.9800 . ? C4 H7 0.9800 . ? C4 H8 0.9800 . ? C4 H9 0.9800 . ? Si2 C7 1.850(3) . ? Si2 C5 1.855(3) . ? Si2 C6 1.862(3) . ? C5 H10 0.9800 . ? C5 H11 0.9800 . ? C5 H12 0.9800 . ? C6 H13 0.9800 . ? C6 H14 0.9800 . ? C6 H15 0.9800 . ? C7 H16 0.9800 . ? C7 H17 0.9800 . ? C7 H18 0.9800 . ? Si3 C9 1.842(3) . ? Si3 C10 1.846(3) . ? Si3 C8 1.847(3) . ? C8 H19 0.9800 . ? C8 H20 0.9800 . ? C8 H21 0.9800 . ? C9 H22 0.9800 . ? C9 H23 0.9800 . ? C9 H24 0.9800 . ? C10 H25 0.9800 . ? C10 H26 0.9800 . ? C10 H27 0.9800 . ? C11 C16 1.390(3) . ? C11 C12 1.391(3) . ? C12 F1 1.358(3) . ? C12 C13 1.384(3) . ? C13 F2 1.352(3) . ? C13 C14 1.372(3) . ? C14 C15 1.375(3) . ? C14 H28 0.9500 . ? C15 F3 1.357(3) . ? C15 C16 1.371(3) . ? C16 F4 1.363(3) . ? C17 C18 1.382(3) . ? C17 C22 1.393(3) . ? C18 F5 1.354(3) . ? C18 C19 1.377(3) . ? C19 F6 1.357(3) . ? C19 C20 1.365(4) . ? C20 C21 1.369(4) . ? C20 H29 0.9500 . ? C21 F7 1.354(3) . ? C21 C22 1.373(3) . ? C22 F8 1.364(3) . ? C23 C24 1.382(3) . ? C23 C28 1.393(3) . ? C24 F9 1.366(3) . ? C24 C25 1.374(3) . ? C25 F10 1.353(3) . ? C25 C26 1.373(3) . ? C26 C27 1.372(4) . ? C26 H30 0.9500 . ? C27 F11 1.361(3) . ? C27 C28 1.377(3) . ? C28 F12 1.355(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 118.2(2) . . ? O1 C1 P1 120.08(18) . . ? O2 C1 P1 121.69(17) . . ? C1 P1 Si1 102.82(8) . . ? C1 P1 Si2 100.35(7) . . ? Si1 P1 Si2 106.96(4) . . ? O1 B1 C11 110.80(19) . . ? O1 B1 C17 103.21(18) . . ? C11 B1 C17 117.6(2) . . ? O1 B1 C23 104.55(19) . . ? C11 B1 C23 106.16(19) . . ? C17 B1 C23 113.8(2) . . ? C1 O1 B1 126.75(19) . . ? C1 O2 Si3 140.36(15) . . ? C4 Si1 C3 109.63(12) . . ? C4 Si1 C2 110.65(12) . . ? C3 Si1 C2 111.78(12) . . ? C4 Si1 P1 104.27(9) . . ? C3 Si1 P1 116.49(8) . . ? C2 Si1 P1 103.64(9) . . ? Si1 C2 H1 109.5 . . ? Si1 C2 H2 109.5 . . ? H1 C2 H2 109.5 . . ? Si1 C2 H3 109.5 . . ? H1 C2 H3 109.5 . . ? H2 C2 H3 109.5 . . ? Si1 C3 H4 109.5 . . ? Si1 C3 H5 109.5 . . ? H4 C3 H5 109.5 . . ? Si1 C3 H6 109.5 . . ? H4 C3 H6 109.5 . . ? H5 C3 H6 109.5 . . ? Si1 C4 H7 109.5 . . ? Si1 C4 H8 109.5 . . ? H7 C4 H8 109.5 . . ? Si1 C4 H9 109.5 . . ? H7 C4 H9 109.5 . . ? H8 C4 H9 109.5 . . ? C7 Si2 C5 110.37(13) . . ? C7 Si2 C6 111.86(13) . . ? C5 Si2 C6 108.44(13) . . ? C7 Si2 P1 102.64(9) . . ? C5 Si2 P1 113.20(9) . . ? C6 Si2 P1 110.31(9) . . ? Si2 C5 H10 109.5 . . ? Si2 C5 H11 109.5 . . ? H10 C5 H11 109.5 . . ? Si2 C5 H12 109.5 . . ? H10 C5 H12 109.5 . . ? H11 C5 H12 109.5 . . ? Si2 C6 H13 109.5 . . ? Si2 C6 H14 109.5 . . ? H13 C6 H14 109.5 . . ? Si2 C6 H15 109.5 . . ? H13 C6 H15 109.5 . . ? H14 C6 H15 109.5 . . ? Si2 C7 H16 109.5 . . ? Si2 C7 H17 109.5 . . ? H16 C7 H17 109.5 . . ? Si2 C7 H18 109.5 . . ? H16 C7 H18 109.5 . . ? H17 C7 H18 109.5 . . ? O2 Si3 C9 102.92(11) . . ? O2 Si3 C10 106.14(11) . . ? C9 Si3 C10 111.07(13) . . ? O2 Si3 C8 113.44(11) . . ? C9 Si3 C8 112.86(14) . . ? C10 Si3 C8 110.06(14) . . ? Si3 C8 H19 109.5 . . ? Si3 C8 H20 109.5 . . ? H19 C8 H20 109.5 . . ? Si3 C8 H21 109.5 . . ? H19 C8 H21 109.5 . . ? H20 C8 H21 109.5 . . ? Si3 C9 H22 109.5 . . ? Si3 C9 H23 109.5 . . ? H22 C9 H23 109.5 . . ? Si3 C9 H24 109.5 . . ? H22 C9 H24 109.5 . . ? H23 C9 H24 109.5 . . ? Si3 C10 H25 109.5 . . ? Si3 C10 H26 109.5 . . ? H25 C10 H26 109.5 . . ? Si3 C10 H27 109.5 . . ? H25 C10 H27 109.5 . . ? H26 C10 H27 109.5 . . ? C16 C11 C12 113.2(2) . . ? C16 C11 B1 119.3(2) . . ? C12 C11 B1 127.2(2) . . ? F1 C12 C13 115.9(2) . . ? F1 C12 C11 120.9(2) . . ? C13 C12 C11 123.2(2) . . ? F2 C13 C14 120.1(2) . . ? F2 C13 C12 118.4(2) . . ? C14 C13 C12 121.5(2) . . ? C13 C14 C15 116.6(2) . . ? C13 C14 H28 121.7 . . ? C15 C14 H28 121.7 . . ? F3 C15 C16 119.0(2) . . ? F3 C15 C14 119.8(2) . . ? C16 C15 C14 121.2(2) . . ? F4 C16 C15 117.5(2) . . ? F4 C16 C11 118.3(2) . . ? C15 C16 C11 124.1(2) . . ? C18 C17 C22 113.1(2) . . ? C18 C17 B1 127.2(2) . . ? C22 C17 B1 119.6(2) . . ? F5 C18 C19 116.4(2) . . ? F5 C18 C17 120.2(2) . . ? C19 C18 C17 123.3(2) . . ? F6 C19 C20 119.8(2) . . ? F6 C19 C18 118.4(2) . . ? C20 C19 C18 121.8(2) . . ? C19 C20 C21 116.8(2) . . ? C19 C20 H29 121.6 . . ? C21 C20 H29 121.6 . . ? F7 C21 C20 119.9(2) . . ? F7 C21 C22 119.3(2) . . ? C20 C21 C22 120.8(2) . . ? F8 C22 C21 116.6(2) . . ? F8 C22 C17 119.3(2) . . ? C21 C22 C17 124.1(2) . . ? C24 C23 C28 113.0(2) . . ? C24 C23 B1 120.9(2) . . ? C28 C23 B1 126.0(2) . . ? F9 C24 C25 116.5(2) . . ? F9 C24 C23 118.9(2) . . ? C25 C24 C23 124.6(2) . . ? F10 C25 C26 119.7(2) . . ? F10 C25 C24 119.5(2) . . ? C26 C25 C24 120.8(2) . . ? C27 C26 C25 116.4(2) . . ? C27 C26 H30 121.8 . . ? C25 C26 H30 121.8 . . ? F11 C27 C26 119.4(2) . . ? F11 C27 C28 118.6(2) . . ? C26 C27 C28 122.1(2) . . ? F12 C28 C27 116.1(2) . . ? F12 C28 C23 120.9(2) . . ? C27 C28 C23 123.0(2) . . ? 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 O1 C1 P1 Si1 -8.86(19) . . . . ? O2 C1 P1 Si1 170.45(16) . . . . ? O1 C1 P1 Si2 101.36(17) . . . . ? O2 C1 P1 Si2 -79.33(18) . . . . ? O2 C1 O1 B1 6.9(3) . . . . ? P1 C1 O1 B1 -173.76(16) . . . . ? C11 B1 O1 C1 -69.5(3) . . . . ? C17 B1 O1 C1 57.3(3) . . . . ? C23 B1 O1 C1 176.58(19) . . . . ? O1 C1 O2 Si3 154.70(17) . . . . ? P1 C1 O2 Si3 -24.6(3) . . . . ? C1 P1 Si1 C4 166.78(11) . . . . ? Si2 P1 Si1 C4 61.60(9) . . . . ? C1 P1 Si1 C3 45.84(12) . . . . ? Si2 P1 Si1 C3 -59.34(10) . . . . ? C1 P1 Si1 C2 -77.36(12) . . . . ? Si2 P1 Si1 C2 177.45(9) . . . . ? C1 P1 Si2 C7 157.43(12) . . . . ? Si1 P1 Si2 C7 -95.63(10) . . . . ? C1 P1 Si2 C5 -83.61(13) . . . . ? Si1 P1 Si2 C5 23.33(10) . . . . ? C1 P1 Si2 C6 38.09(13) . . . . ? Si1 P1 Si2 C6 145.04(10) . . . . ? C1 O2 Si3 C9 146.8(2) . . . . ? C1 O2 Si3 C10 -96.4(3) . . . . ? C1 O2 Si3 C8 24.5(3) . . . . ? O1 B1 C11 C16 179.52(19) . . . . ? C17 B1 C11 C16 61.2(3) . . . . ? C23 B1 C11 C16 -67.5(3) . . . . ? O1 B1 C11 C12 -7.6(3) . . . . ? C17 B1 C11 C12 -125.9(2) . . . . ? C23 B1 C11 C12 105.4(3) . . . . ? C16 C11 C12 F1 176.9(2) . . . . ? B1 C11 C12 F1 3.7(4) . . . . ? C16 C11 C12 C13 -3.4(3) . . . . ? B1 C11 C12 C13 -176.7(2) . . . . ? F1 C12 C13 F2 2.4(3) . . . . ? C11 C12 C13 F2 -177.3(2) . . . . ? F1 C12 C13 C14 -177.6(2) . . . . ? C11 C12 C13 C14 2.7(4) . . . . ? F2 C13 C14 C15 179.5(2) . . . . ? C12 C13 C14 C15 -0.5(4) . . . . ? C13 C14 C15 F3 179.9(2) . . . . ? C13 C14 C15 C16 -0.7(4) . . . . ? F3 C15 C16 F4 -0.6(3) . . . . ? C14 C15 C16 F4 179.9(2) . . . . ? F3 C15 C16 C11 179.2(2) . . . . ? C14 C15 C16 C11 -0.3(4) . . . . ? C12 C11 C16 F4 -177.95(19) . . . . ? B1 C11 C16 F4 -4.1(3) . . . . ? C12 C11 C16 C15 2.3(3) . . . . ? B1 C11 C16 C15 176.1(2) . . . . ? O1 B1 C17 C18 -114.1(2) . . . . ? C11 B1 C17 C18 8.2(3) . . . . ? C23 B1 C17 C18 133.2(2) . . . . ? O1 B1 C17 C22 61.1(3) . . . . ? C11 B1 C17 C22 -176.6(2) . . . . ? C23 B1 C17 C22 -51.5(3) . . . . ? C22 C17 C18 F5 -178.1(2) . . . . ? B1 C17 C18 F5 -2.6(4) . . . . ? C22 C17 C18 C19 1.3(3) . . . . ? B1 C17 C18 C19 176.8(2) . . . . ? F5 C18 C19 F6 -0.9(3) . . . . ? C17 C18 C19 F6 179.7(2) . . . . ? F5 C18 C19 C20 179.0(2) . . . . ? C17 C18 C19 C20 -0.4(4) . . . . ? F6 C19 C20 C21 179.3(2) . . . . ? C18 C19 C20 C21 -0.6(4) . . . . ? C19 C20 C21 F7 -179.2(2) . . . . ? C19 C20 C21 C22 0.5(4) . . . . ? F7 C21 C22 F8 -0.1(3) . . . . ? C20 C21 C22 F8 -179.9(2) . . . . ? F7 C21 C22 C17 -179.7(2) . . . . ? C20 C21 C22 C17 0.5(4) . . . . ? C18 C17 C22 F8 179.0(2) . . . . ? B1 C17 C22 F8 3.2(3) . . . . ? C18 C17 C22 C21 -1.4(3) . . . . ? B1 C17 C22 C21 -177.3(2) . . . . ? O1 B1 C23 C24 51.2(3) . . . . ? C11 B1 C23 C24 -66.0(3) . . . . ? C17 B1 C23 C24 163.1(2) . . . . ? O1 B1 C23 C28 -131.8(2) . . . . ? C11 B1 C23 C28 111.0(3) . . . . ? C17 B1 C23 C28 -19.9(3) . . . . ? C28 C23 C24 F9 -177.2(2) . . . . ? B1 C23 C24 F9 0.2(3) . . . . ? C28 C23 C24 C25 3.7(3) . . . . ? B1 C23 C24 C25 -179.0(2) . . . . ? F9 C24 C25 F10 -0.9(3) . . . . ? C23 C24 C25 F10 178.3(2) . . . . ? F9 C24 C25 C26 178.8(2) . . . . ? C23 C24 C25 C26 -2.1(4) . . . . ? F10 C25 C26 C27 179.3(2) . . . . ? C24 C25 C26 C27 -0.4(4) . . . . ? C25 C26 C27 F11 -179.8(2) . . . . ? C25 C26 C27 C28 0.9(4) . . . . ? F11 C27 C28 F12 0.9(3) . . . . ? C26 C27 C28 F12 -179.7(2) . . . . ? F11 C27 C28 C23 -178.4(2) . . . . ? C26 C27 C28 C23 1.0(4) . . . . ? C24 C23 C28 F12 177.6(2) . . . . ? B1 C23 C28 F12 0.4(4) . . . . ? C24 C23 C28 C27 -3.1(3) . . . . ? B1 C23 C28 C27 179.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.296 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.069 data_kt004_0m _database_code_depnum_ccdc_archive 'CCDC 899515' #TrackingRef 'kt004_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H30 B F12 O4 P Si3' _chemical_formula_weight 796.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8454(4) _cell_length_b 11.2438(4) _cell_length_c 15.4120(6) _cell_angle_alpha 84.657(2) _cell_angle_beta 87.6520(10) _cell_angle_gamma 85.639(2) _cell_volume 1864.72(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9885 _cell_measurement_theta_min 2.650 _cell_measurement_theta_max 27.461 _exptl_crystal_description Plate _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9494 _exptl_absorpt_correction_T_max 0.9494 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32663 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8451 _reflns_number_gt 6312 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+1.1322P] 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 8451 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1021 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.18147(5) 0.45763(5) 0.15666(4) 0.02801(13) Uani 1 1 d . . . C1 C 0.11265(16) 0.38080(17) 0.25274(13) 0.0229(4) Uani 1 1 d . . . C2 C 0.08794(17) 0.59120(17) 0.14753(13) 0.0234(4) Uani 1 1 d . . . O1 O 0.17364(11) 0.29643(11) 0.29711(8) 0.0203(3) Uani 1 1 d . . . O2 O -0.00301(12) 0.39967(13) 0.27567(9) 0.0309(3) Uani 1 1 d . . . O3 O 0.00295(13) 0.62671(12) 0.20308(9) 0.0294(3) Uani 1 1 d . . . O4 O 0.10667(13) 0.67039(12) 0.08054(9) 0.0284(3) Uani 1 1 d . . . Si1 Si -0.08622(5) 0.31724(5) 0.35591(4) 0.02680(14) Uani 1 1 d . . . C3 C -0.01339(19) 0.3168(2) 0.46180(14) 0.0320(5) Uani 1 1 d . . . H1 H -0.0145 0.3991 0.4782 0.048 Uiso 1 1 calc . . . H2 H 0.0724 0.2830 0.4573 0.048 Uiso 1 1 calc . . . H3 H -0.0593 0.2682 0.5063 0.048 Uiso 1 1 calc . . . C4 C -0.0910(2) 0.1672(2) 0.31720(15) 0.0429(6) Uani 1 1 d . . . H4 H -0.1304 0.1745 0.2607 0.064 Uiso 1 1 calc . . . H5 H -0.1386 0.1168 0.3595 0.064 Uiso 1 1 calc . . . H6 H -0.0065 0.1307 0.3109 0.064 Uiso 1 1 calc . . . C5 C -0.2383(2) 0.4023(3) 0.35290(17) 0.0509(7) Uani 1 1 d . . . H7 H -0.2737 0.3996 0.2957 0.076 Uiso 1 1 calc . . . H8 H -0.2284 0.4857 0.3631 0.076 Uiso 1 1 calc . . . H9 H -0.2938 0.3668 0.3983 0.076 Uiso 1 1 calc . . . Si2 Si -0.07393(6) 0.76702(6) 0.20197(4) 0.03841(16) Uani 1 1 d . . . C6 C -0.1713(3) 0.7516(3) 0.30298(18) 0.0605(8) Uani 1 1 d . . . H10 H -0.1183 0.7367 0.3534 0.091 Uiso 1 1 calc . . . H11 H -0.2233 0.6844 0.3010 0.091 Uiso 1 1 calc . . . H12 H -0.2240 0.8256 0.3081 0.091 Uiso 1 1 calc . . . C7 C -0.1682(3) 0.7918(2) 0.10453(18) 0.0512(7) Uani 1 1 d . . . H13 H -0.2279 0.7304 0.1065 0.077 Uiso 1 1 calc . . . H14 H -0.1143 0.7870 0.0522 0.077 Uiso 1 1 calc . . . H15 H -0.2126 0.8712 0.1030 0.077 Uiso 1 1 calc . . . C8 C 0.0415(3) 0.8775(3) 0.2064(2) 0.0782(10) Uani 1 1 d . . . H16 H 0.0892 0.8583 0.2592 0.117 Uiso 1 1 calc . . . H17 H -0.0005 0.9577 0.2076 0.117 Uiso 1 1 calc . . . H18 H 0.0974 0.8755 0.1549 0.117 Uiso 1 1 calc . . . Si3 Si 0.20360(6) 0.67879(6) -0.00962(4) 0.03212(15) Uani 1 1 d . . . C9 C 0.1408(3) 0.8211(3) -0.06649(18) 0.0598(8) Uani 1 1 d . . . H19 H 0.1516 0.8871 -0.0309 0.090 Uiso 1 1 calc . . . H20 H 0.0525 0.8165 -0.0759 0.090 Uiso 1 1 calc . . . H21 H 0.1848 0.8352 -0.1229 0.090 Uiso 1 1 calc . . . C10 C 0.3619(2) 0.6861(3) 0.02731(18) 0.0516(7) Uani 1 1 d . . . H22 H 0.3652 0.7562 0.0603 0.077 Uiso 1 1 calc . . . H23 H 0.4193 0.6928 -0.0234 0.077 Uiso 1 1 calc . . . H24 H 0.3855 0.6133 0.0647 0.077 Uiso 1 1 calc . . . C11 C 0.1856(3) 0.5498(3) -0.07173(17) 0.0528(7) Uani 1 1 d . . . H25 H 0.0998 0.5512 -0.0897 0.079 Uiso 1 1 calc . . . H26 H 0.2062 0.4755 -0.0351 0.079 Uiso 1 1 calc . . . H27 H 0.2411 0.5538 -0.1235 0.079 Uiso 1 1 calc . . . B1 B 0.31638(18) 0.26962(19) 0.30440(14) 0.0199(4) Uani 1 1 d . . . C12 C 0.37484(16) 0.39881(16) 0.30625(13) 0.0215(4) Uani 1 1 d . . . C13 C 0.46132(16) 0.44806(17) 0.24769(13) 0.0234(4) Uani 1 1 d . . . C14 C 0.49742(18) 0.56261(18) 0.24919(15) 0.0301(5) Uani 1 1 d . . . C15 C 0.4487(2) 0.63651(19) 0.30924(17) 0.0387(6) Uani 1 1 d . . . H28 H 0.4734 0.7157 0.3098 0.046 Uiso 1 1 calc . . . C16 C 0.36221(19) 0.59132(19) 0.36908(16) 0.0361(5) Uani 1 1 d . . . C17 C 0.32815(17) 0.47639(18) 0.36715(14) 0.0277(4) Uani 1 1 d . . . F1 F 0.51262(10) 0.38554(10) 0.18231(8) 0.0302(3) Uani 1 1 d . . . F2 F 0.58243(11) 0.60299(11) 0.18862(9) 0.0414(3) Uani 1 1 d . . . F3 F 0.31000(13) 0.65981(12) 0.42961(11) 0.0556(4) Uani 1 1 d . . . F4 F 0.24247(11) 0.43879(11) 0.42793(8) 0.0360(3) Uani 1 1 d . . . C18 C 0.32467(16) 0.18169(16) 0.39604(12) 0.0201(4) Uani 1 1 d . . . C19 C 0.39564(17) 0.19349(18) 0.46713(13) 0.0235(4) Uani 1 1 d . . . C20 C 0.39858(18) 0.11171(19) 0.53985(13) 0.0277(4) Uani 1 1 d . . . C21 C 0.3318(2) 0.01225(19) 0.54591(13) 0.0313(5) Uani 1 1 d . . . H29 H 0.3339 -0.0436 0.5961 0.038 Uiso 1 1 calc . . . C22 C 0.26222(19) -0.00269(18) 0.47626(14) 0.0282(4) Uani 1 1 d . . . C23 C 0.25953(17) 0.07897(17) 0.40411(12) 0.0230(4) Uani 1 1 d . . . F5 F 0.46746(11) 0.28628(11) 0.46738(8) 0.0345(3) Uani 1 1 d . . . F6 F 0.47136(12) 0.12833(12) 0.60634(8) 0.0421(3) Uani 1 1 d . . . F7 F 0.19604(13) -0.10005(11) 0.47717(9) 0.0452(3) Uani 1 1 d . . . F8 F 0.19101(11) 0.05431(10) 0.33745(8) 0.0326(3) Uani 1 1 d . . . C24 C 0.37300(16) 0.18505(16) 0.22924(12) 0.0196(4) Uani 1 1 d . . . C25 C 0.49555(17) 0.13950(17) 0.23633(12) 0.0223(4) Uani 1 1 d . . . C26 C 0.54959(18) 0.05320(18) 0.18756(14) 0.0285(5) Uani 1 1 d . . . C27 C 0.4851(2) 0.00657(19) 0.12522(14) 0.0333(5) Uani 1 1 d . . . H30 H 0.5220 -0.0532 0.0908 0.040 Uiso 1 1 calc . . . C28 C 0.3647(2) 0.05074(19) 0.11537(13) 0.0314(5) Uani 1 1 d . . . C29 C 0.31066(17) 0.13695(17) 0.16598(13) 0.0244(4) Uani 1 1 d . . . F9 F 0.56579(9) 0.18042(10) 0.29649(7) 0.0274(3) Uani 1 1 d . . . F10 F 0.66887(11) 0.01227(11) 0.20210(9) 0.0417(3) Uani 1 1 d . . . F11 F 0.29606(14) 0.00807(13) 0.05534(9) 0.0479(4) Uani 1 1 d . . . F12 F 0.18969(10) 0.17082(11) 0.15240(8) 0.0333(3) 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 P1 0.0215(2) 0.0294(3) 0.0288(3) 0.0098(2) 0.0077(2) 0.0061(2) C1 0.0172(9) 0.0258(10) 0.0245(10) 0.0019(8) 0.0007(8) 0.0007(8) C2 0.0236(9) 0.0261(10) 0.0202(10) -0.0005(8) -0.0009(8) -0.0020(8) O1 0.0162(6) 0.0208(7) 0.0230(7) 0.0033(5) -0.0012(5) -0.0006(5) O2 0.0167(6) 0.0402(9) 0.0311(8) 0.0137(7) 0.0044(6) 0.0045(6) O3 0.0344(8) 0.0267(8) 0.0249(8) -0.0010(6) 0.0061(6) 0.0060(6) O4 0.0363(8) 0.0232(7) 0.0235(7) 0.0046(6) 0.0025(6) 0.0015(6) Si1 0.0174(2) 0.0383(3) 0.0234(3) 0.0038(2) 0.0024(2) -0.0036(2) C3 0.0306(11) 0.0401(13) 0.0260(11) -0.0038(9) 0.0049(9) -0.0090(9) C4 0.0389(12) 0.0615(16) 0.0326(13) -0.0138(12) 0.0065(10) -0.0233(12) C5 0.0213(10) 0.0771(19) 0.0485(16) 0.0173(14) 0.0071(10) 0.0029(11) Si2 0.0508(4) 0.0261(3) 0.0375(4) -0.0097(3) 0.0070(3) 0.0064(3) C6 0.0723(19) 0.0612(18) 0.0433(16) -0.0132(14) 0.0150(14) 0.0266(15) C7 0.0546(15) 0.0427(15) 0.0508(16) 0.0010(12) 0.0018(13) 0.0237(12) C8 0.096(3) 0.0495(18) 0.096(3) -0.0367(18) 0.010(2) -0.0222(17) Si3 0.0352(3) 0.0413(4) 0.0206(3) 0.0027(3) -0.0001(2) -0.0152(3) C9 0.0754(19) 0.0607(18) 0.0413(16) 0.0257(13) -0.0119(14) -0.0239(15) C10 0.0386(13) 0.0718(19) 0.0460(16) 0.0009(14) -0.0028(12) -0.0215(13) C11 0.0547(16) 0.0726(19) 0.0355(14) -0.0225(13) 0.0076(12) -0.0167(14) B1 0.0158(9) 0.0213(11) 0.0223(11) -0.0011(9) -0.0027(8) -0.0001(8) C12 0.0161(8) 0.0211(10) 0.0272(10) -0.0023(8) -0.0017(7) -0.0002(7) C13 0.0183(9) 0.0220(10) 0.0299(11) -0.0053(8) -0.0002(8) 0.0015(7) C14 0.0215(9) 0.0272(11) 0.0415(13) -0.0006(10) 0.0028(9) -0.0068(8) C15 0.0326(11) 0.0229(11) 0.0628(16) -0.0123(11) 0.0043(11) -0.0090(9) C16 0.0291(11) 0.0298(12) 0.0516(15) -0.0186(11) 0.0046(10) -0.0021(9) C17 0.0203(9) 0.0275(11) 0.0356(12) -0.0064(9) 0.0043(8) -0.0021(8) F1 0.0304(6) 0.0274(6) 0.0326(7) -0.0044(5) 0.0095(5) -0.0050(5) F2 0.0341(7) 0.0331(7) 0.0568(9) 0.0001(6) 0.0134(6) -0.0144(5) F3 0.0519(8) 0.0403(8) 0.0795(11) -0.0375(8) 0.0243(8) -0.0106(7) F4 0.0317(6) 0.0359(7) 0.0421(8) -0.0144(6) 0.0155(6) -0.0081(5) C18 0.0190(8) 0.0203(9) 0.0204(10) -0.0030(8) 0.0006(7) 0.0036(7) C19 0.0194(9) 0.0266(10) 0.0248(10) -0.0051(8) -0.0007(8) 0.0001(8) C20 0.0256(10) 0.0400(12) 0.0169(10) -0.0053(9) -0.0036(8) 0.0072(9) C21 0.0363(11) 0.0323(12) 0.0217(11) 0.0060(9) 0.0023(9) 0.0078(9) C22 0.0334(11) 0.0218(10) 0.0282(11) 0.0013(9) 0.0029(9) -0.0009(8) C23 0.0243(9) 0.0235(10) 0.0213(10) -0.0027(8) -0.0026(8) 0.0000(8) F5 0.0321(6) 0.0399(7) 0.0337(7) -0.0043(6) -0.0103(5) -0.0114(5) F6 0.0444(7) 0.0574(9) 0.0246(7) -0.0032(6) -0.0137(6) 0.0015(6) F7 0.0653(9) 0.0297(7) 0.0407(8) 0.0090(6) -0.0006(7) -0.0184(6) F8 0.0411(7) 0.0289(6) 0.0294(7) 0.0026(5) -0.0116(5) -0.0140(5) C24 0.0222(9) 0.0159(9) 0.0199(10) 0.0036(7) -0.0009(7) -0.0014(7) C25 0.0242(9) 0.0216(10) 0.0209(10) 0.0002(8) -0.0018(8) -0.0020(8) C26 0.0260(10) 0.0256(11) 0.0315(12) 0.0025(9) 0.0055(9) 0.0041(8) C27 0.0425(12) 0.0283(11) 0.0286(12) -0.0078(9) 0.0075(10) 0.0027(9) C28 0.0448(12) 0.0293(11) 0.0218(11) -0.0062(9) -0.0042(9) -0.0072(10) C29 0.0259(10) 0.0240(10) 0.0228(10) 0.0014(8) -0.0030(8) -0.0015(8) F9 0.0207(5) 0.0301(6) 0.0314(6) -0.0034(5) -0.0060(5) 0.0025(5) F10 0.0292(6) 0.0397(8) 0.0538(9) -0.0069(6) 0.0054(6) 0.0120(6) F11 0.0613(9) 0.0512(9) 0.0355(8) -0.0214(7) -0.0111(7) -0.0067(7) F12 0.0283(6) 0.0381(7) 0.0349(7) -0.0069(6) -0.0127(5) -0.0003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C2 1.745(2) . ? P1 C1 1.8070(19) . ? C1 O1 1.275(2) . ? C1 O2 1.296(2) . ? C2 O3 1.298(2) . ? C2 O4 1.319(2) . ? O1 B1 1.561(2) . ? O2 Si1 1.7393(14) . ? O3 Si2 1.7264(15) . ? O4 Si3 1.7076(15) . ? Si1 C3 1.841(2) . ? Si1 C5 1.843(2) . ? Si1 C4 1.846(3) . ? C3 H1 0.9800 . ? C3 H2 0.9800 . ? C3 H3 0.9800 . ? C4 H4 0.9800 . ? C4 H5 0.9800 . ? C4 H6 0.9800 . ? C5 H7 0.9800 . ? C5 H8 0.9800 . ? C5 H9 0.9800 . ? Si2 C8 1.837(3) . ? Si2 C7 1.839(3) . ? Si2 C6 1.847(3) . ? C6 H10 0.9800 . ? C6 H11 0.9800 . ? C6 H12 0.9800 . ? C7 H13 0.9800 . ? C7 H14 0.9800 . ? C7 H15 0.9800 . ? C8 H16 0.9800 . ? C8 H17 0.9800 . ? C8 H18 0.9800 . ? Si3 C11 1.837(3) . ? Si3 C10 1.841(2) . ? Si3 C9 1.848(3) . ? C9 H19 0.9800 . ? C9 H20 0.9800 . ? C9 H21 0.9800 . ? C10 H22 0.9800 . ? C10 H23 0.9800 . ? C10 H24 0.9800 . ? C11 H25 0.9800 . ? C11 H26 0.9800 . ? C11 H27 0.9800 . ? B1 C12 1.632(3) . ? B1 C24 1.637(3) . ? B1 C18 1.648(3) . ? C12 C13 1.385(3) . ? C12 C17 1.394(3) . ? C13 F1 1.359(2) . ? C13 C14 1.377(3) . ? C14 F2 1.357(2) . ? C14 C15 1.365(3) . ? C15 C16 1.380(3) . ? C15 H28 0.9500 . ? C16 F3 1.345(2) . ? C16 C17 1.374(3) . ? C17 F4 1.354(2) . ? C18 C19 1.386(3) . ? C18 C23 1.392(3) . ? C19 F5 1.349(2) . ? C19 C20 1.382(3) . ? C20 F6 1.354(2) . ? C20 C21 1.372(3) . ? C21 C22 1.367(3) . ? C21 H29 0.9500 . ? C22 F7 1.353(2) . ? C22 C23 1.374(3) . ? C23 F8 1.353(2) . ? C24 C29 1.381(3) . ? C24 C25 1.392(3) . ? C25 F9 1.357(2) . ? C25 C26 1.365(3) . ? C26 F10 1.360(2) . ? C26 C27 1.376(3) . ? C27 C28 1.370(3) . ? C27 H30 0.9500 . ? C28 F11 1.354(2) . ? C28 C29 1.381(3) . ? C29 F12 1.357(2) . ? 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 C2 P1 C1 101.08(9) . . ? O1 C1 O2 116.26(16) . . ? O1 C1 P1 120.87(13) . . ? O2 C1 P1 122.55(14) . . ? O3 C2 O4 113.89(17) . . ? O3 C2 P1 126.97(15) . . ? O4 C2 P1 119.03(14) . . ? C1 O1 B1 129.91(14) . . ? C1 O2 Si1 127.21(13) . . ? C2 O3 Si2 126.86(13) . . ? C2 O4 Si3 136.17(13) . . ? O2 Si1 C3 109.94(8) . . ? O2 Si1 C5 101.30(9) . . ? C3 Si1 C5 112.37(12) . . ? O2 Si1 C4 105.69(9) . . ? C3 Si1 C4 114.08(11) . . ? C5 Si1 C4 112.44(12) . . ? Si1 C3 H1 109.5 . . ? Si1 C3 H2 109.5 . . ? H1 C3 H2 109.5 . . ? Si1 C3 H3 109.5 . . ? H1 C3 H3 109.5 . . ? H2 C3 H3 109.5 . . ? Si1 C4 H4 109.5 . . ? Si1 C4 H5 109.5 . . ? H4 C4 H5 109.5 . . ? Si1 C4 H6 109.5 . . ? H4 C4 H6 109.5 . . ? H5 C4 H6 109.5 . . ? Si1 C5 H7 109.5 . . ? Si1 C5 H8 109.5 . . ? H7 C5 H8 109.5 . . ? Si1 C5 H9 109.5 . . ? H7 C5 H9 109.5 . . ? H8 C5 H9 109.5 . . ? O3 Si2 C8 108.21(13) . . ? O3 Si2 C7 108.51(10) . . ? C8 Si2 C7 113.73(16) . . ? O3 Si2 C6 101.61(10) . . ? C8 Si2 C6 112.35(16) . . ? C7 Si2 C6 111.60(14) . . ? Si2 C6 H10 109.5 . . ? Si2 C6 H11 109.5 . . ? H10 C6 H11 109.5 . . ? Si2 C6 H12 109.5 . . ? H10 C6 H12 109.5 . . ? H11 C6 H12 109.5 . . ? Si2 C7 H13 109.5 . . ? Si2 C7 H14 109.5 . . ? H13 C7 H14 109.5 . . ? Si2 C7 H15 109.5 . . ? H13 C7 H15 109.5 . . ? H14 C7 H15 109.5 . . ? Si2 C8 H16 109.5 . . ? Si2 C8 H17 109.5 . . ? H16 C8 H17 109.5 . . ? Si2 C8 H18 109.5 . . ? H16 C8 H18 109.5 . . ? H17 C8 H18 109.5 . . ? O4 Si3 C11 108.95(10) . . ? O4 Si3 C10 107.82(10) . . ? C11 Si3 C10 113.48(14) . . ? O4 Si3 C9 100.25(11) . . ? C11 Si3 C9 112.29(14) . . ? C10 Si3 C9 113.04(13) . . ? Si3 C9 H19 109.5 . . ? Si3 C9 H20 109.5 . . ? H19 C9 H20 109.5 . . ? Si3 C9 H21 109.5 . . ? H19 C9 H21 109.5 . . ? H20 C9 H21 109.5 . . ? Si3 C10 H22 109.5 . . ? Si3 C10 H23 109.5 . . ? H22 C10 H23 109.5 . . ? Si3 C10 H24 109.5 . . ? H22 C10 H24 109.5 . . ? H23 C10 H24 109.5 . . ? Si3 C11 H25 109.5 . . ? Si3 C11 H26 109.5 . . ? H25 C11 H26 109.5 . . ? Si3 C11 H27 109.5 . . ? H25 C11 H27 109.5 . . ? H26 C11 H27 109.5 . . ? O1 B1 C12 106.48(14) . . ? O1 B1 C24 111.41(15) . . ? C12 B1 C24 116.49(15) . . ? O1 B1 C18 101.60(14) . . ? C12 B1 C18 115.34(16) . . ? C24 B1 C18 104.60(15) . . ? C13 C12 C17 113.44(17) . . ? C13 C12 B1 127.03(17) . . ? C17 C12 B1 119.26(16) . . ? F1 C13 C14 115.84(17) . . ? F1 C13 C12 120.80(16) . . ? C14 C13 C12 123.32(18) . . ? F2 C14 C15 119.48(18) . . ? F2 C14 C13 118.89(19) . . ? C15 C14 C13 121.62(19) . . ? C14 C15 C16 117.18(19) . . ? C14 C15 H28 121.4 . . ? C16 C15 H28 121.4 . . ? F3 C16 C17 119.42(19) . . ? F3 C16 C15 120.16(19) . . ? C17 C16 C15 120.4(2) . . ? F4 C17 C16 116.84(18) . . ? F4 C17 C12 119.13(17) . . ? C16 C17 C12 124.02(19) . . ? C19 C18 C23 113.82(17) . . ? C19 C18 B1 127.58(16) . . ? C23 C18 B1 118.50(16) . . ? F5 C19 C20 116.71(17) . . ? F5 C19 C18 120.62(17) . . ? C20 C19 C18 122.66(18) . . ? F6 C20 C21 118.79(18) . . ? F6 C20 C19 119.34(18) . . ? C21 C20 C19 121.85(18) . . ? C22 C21 C20 116.83(18) . . ? C22 C21 H29 121.6 . . ? C20 C21 H29 121.6 . . ? F7 C22 C21 119.94(18) . . ? F7 C22 C23 118.96(18) . . ? C21 C22 C23 121.09(19) . . ? F8 C23 C22 116.65(17) . . ? F8 C23 C18 119.61(17) . . ? C22 C23 C18 123.73(18) . . ? C29 C24 C25 113.66(17) . . ? C29 C24 B1 128.38(16) . . ? C25 C24 B1 117.19(16) . . ? F9 C25 C26 117.30(17) . . ? F9 C25 C24 118.77(17) . . ? C26 C25 C24 123.91(18) . . ? F10 C26 C25 118.92(19) . . ? F10 C26 C27 119.94(18) . . ? C25 C26 C27 121.14(19) . . ? C28 C27 C26 116.58(19) . . ? C28 C27 H30 121.7 . . ? C26 C27 H30 121.7 . . ? F11 C28 C27 119.42(19) . . ? F11 C28 C29 118.90(19) . . ? C27 C28 C29 121.67(19) . . ? F12 C29 C24 120.59(17) . . ? F12 C29 C28 116.37(17) . . ? C24 C29 C28 123.02(18) . . ? 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 C2 P1 C1 O1 -158.85(16) . . . . ? C2 P1 C1 O2 27.82(19) . . . . ? C1 P1 C2 O3 7.3(2) . . . . ? C1 P1 C2 O4 -176.74(15) . . . . ? O2 C1 O1 B1 -162.68(17) . . . . ? P1 C1 O1 B1 23.6(3) . . . . ? O1 C1 O2 Si1 -4.1(3) . . . . ? P1 C1 O2 Si1 169.54(10) . . . . ? O4 C2 O3 Si2 -6.1(2) . . . . ? P1 C2 O3 Si2 169.97(11) . . . . ? O3 C2 O4 Si3 178.30(14) . . . . ? P1 C2 O4 Si3 1.9(3) . . . . ? C1 O2 Si1 C3 58.47(19) . . . . ? C1 O2 Si1 C5 177.50(19) . . . . ? C1 O2 Si1 C4 -65.09(19) . . . . ? C2 O3 Si2 C8 -58.3(2) . . . . ? C2 O3 Si2 C7 65.53(19) . . . . ? C2 O3 Si2 C6 -176.75(18) . . . . ? C2 O4 Si3 C11 56.1(2) . . . . ? C2 O4 Si3 C10 -67.5(2) . . . . ? C2 O4 Si3 C9 174.1(2) . . . . ? C1 O1 B1 C12 39.4(2) . . . . ? C1 O1 B1 C24 -88.6(2) . . . . ? C1 O1 B1 C18 160.52(18) . . . . ? O1 B1 C12 C13 -120.36(19) . . . . ? C24 B1 C12 C13 4.6(3) . . . . ? C18 B1 C12 C13 127.8(2) . . . . ? O1 B1 C12 C17 53.3(2) . . . . ? C24 B1 C12 C17 178.22(17) . . . . ? C18 B1 C12 C17 -58.6(2) . . . . ? C17 C12 C13 F1 -177.74(17) . . . . ? B1 C12 C13 F1 -3.8(3) . . . . ? C17 C12 C13 C14 -0.2(3) . . . . ? B1 C12 C13 C14 173.72(19) . . . . ? F1 C13 C14 F2 -2.0(3) . . . . ? C12 C13 C14 F2 -179.63(18) . . . . ? F1 C13 C14 C15 177.2(2) . . . . ? C12 C13 C14 C15 -0.5(3) . . . . ? F2 C14 C15 C16 179.7(2) . . . . ? C13 C14 C15 C16 0.5(3) . . . . ? C14 C15 C16 F3 -179.5(2) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? F3 C16 C17 F4 -0.2(3) . . . . ? C15 C16 C17 F4 -179.8(2) . . . . ? F3 C16 C17 C12 178.8(2) . . . . ? C15 C16 C17 C12 -0.9(4) . . . . ? C13 C12 C17 F4 179.83(17) . . . . ? B1 C12 C17 F4 5.4(3) . . . . ? C13 C12 C17 C16 0.9(3) . . . . ? B1 C12 C17 C16 -173.6(2) . . . . ? O1 B1 C18 C19 -128.71(19) . . . . ? C12 B1 C18 C19 -14.0(3) . . . . ? C24 B1 C18 C19 115.3(2) . . . . ? O1 B1 C18 C23 55.1(2) . . . . ? C12 B1 C18 C23 169.77(16) . . . . ? C24 B1 C18 C23 -60.9(2) . . . . ? C23 C18 C19 F5 177.56(16) . . . . ? B1 C18 C19 F5 1.2(3) . . . . ? C23 C18 C19 C20 -1.4(3) . . . . ? B1 C18 C19 C20 -177.75(18) . . . . ? F5 C19 C20 F6 0.2(3) . . . . ? C18 C19 C20 F6 179.15(17) . . . . ? F5 C19 C20 C21 -178.32(18) . . . . ? C18 C19 C20 C21 0.7(3) . . . . ? F6 C20 C21 C22 -178.26(18) . . . . ? C19 C20 C21 C22 0.2(3) . . . . ? C20 C21 C22 F7 178.70(18) . . . . ? C20 C21 C22 C23 -0.3(3) . . . . ? F7 C22 C23 F8 -1.0(3) . . . . ? C21 C22 C23 F8 177.95(18) . . . . ? F7 C22 C23 C18 -179.56(18) . . . . ? C21 C22 C23 C18 -0.6(3) . . . . ? C19 C18 C23 F8 -177.11(16) . . . . ? B1 C18 C23 F8 -0.4(3) . . . . ? C19 C18 C23 C22 1.4(3) . . . . ? B1 C18 C23 C22 178.07(18) . . . . ? O1 B1 C24 C29 -1.3(3) . . . . ? C12 B1 C24 C29 -123.7(2) . . . . ? C18 B1 C24 C29 107.6(2) . . . . ? O1 B1 C24 C25 -170.54(15) . . . . ? C12 B1 C24 C25 67.1(2) . . . . ? C18 B1 C24 C25 -61.5(2) . . . . ? C29 C24 C25 F9 180.00(16) . . . . ? B1 C24 C25 F9 -9.2(2) . . . . ? C29 C24 C25 C26 -1.6(3) . . . . ? B1 C24 C25 C26 169.13(18) . . . . ? F9 C25 C26 F10 0.7(3) . . . . ? C24 C25 C26 F10 -177.70(17) . . . . ? F9 C25 C26 C27 179.90(18) . . . . ? C24 C25 C26 C27 1.5(3) . . . . ? F10 C26 C27 C28 178.87(18) . . . . ? C25 C26 C27 C28 -0.3(3) . . . . ? C26 C27 C28 F11 -179.71(18) . . . . ? C26 C27 C28 C29 -0.5(3) . . . . ? C25 C24 C29 F12 178.78(16) . . . . ? B1 C24 C29 F12 9.3(3) . . . . ? C25 C24 C29 C28 0.7(3) . . . . ? B1 C24 C29 C28 -168.78(19) . . . . ? F11 C28 C29 F12 1.4(3) . . . . ? C27 C28 C29 F12 -177.81(19) . . . . ? F11 C28 C29 C24 179.49(18) . . . . ? C27 C28 C29 C24 0.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.396 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.054