data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'G. Erker' 'Roland Frohlich' 'Gerald Kehr' 'Juri Ugolotti' _publ_contact_author_name 'G. Erker' _publ_contact_author_email ERKER@UNI-MUENSTER.DE _publ_section_title ; Photochemical Isomerisation of Boryl-Substituted Silole Derivatives ; # Attachment 'erk5152.cif' data_erk5152 _database_code_depnum_ccdc_archive 'CCDC 765606' #TrackingRef 'erk5152.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 Si3' _chemical_formula_weight 252.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 18.3002(4) _cell_length_b 32.3093(7) _cell_length_c 5.8892(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3482.09(12) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1441 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 2.299 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4244 _exptl_absorpt_correction_T_max 0.7243 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6100 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 5.48 _diffrn_reflns_theta_max 67.48 _reflns_number_total 1473 _reflns_number_gt 1460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0462P)^2^+1.2055P] 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 SHELXL _refine_ls_extinction_coef 0.00321(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.42(4) _refine_ls_number_reflns 1473 _refine_ls_number_parameters 75 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.063 _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 Si1 Si 0.2500 0.2500 0.78314(10) 0.0443(2) Uani 1 2 d S . . Si2 Si 0.06963(2) 0.175938(12) 0.32514(7) 0.04208(17) Uani 1 1 d . . . C1 C 0.18461(9) 0.22269(6) 0.5976(3) 0.0512(4) Uani 1 1 d . . . C2 C 0.13966(8) 0.20451(5) 0.4866(3) 0.0507(4) Uani 1 1 d . . . C3 C 0.29907(11) 0.21208(6) 0.9610(5) 0.0679(6) Uani 1 1 d . . . H3A H 0.2641 0.1958 1.0462 0.102 Uiso 1 1 calc R . . H3B H 0.3311 0.2266 1.0654 0.102 Uiso 1 1 calc R . . H3C H 0.3279 0.1940 0.8648 0.102 Uiso 1 1 calc R . . C20 C 0.00060(9) 0.15644(6) 0.5273(4) 0.0571(4) Uani 1 1 d . . . H20A H 0.0245 0.1402 0.6441 0.086 Uiso 1 1 calc R . . H20B H -0.0344 0.1393 0.4472 0.086 Uiso 1 1 calc R . . H20C H -0.0245 0.1796 0.5969 0.086 Uiso 1 1 calc R . . C21 C 0.02697(11) 0.21187(6) 0.1170(3) 0.0606(5) Uani 1 1 d . . . H21A H 0.0137 0.2374 0.1929 0.091 Uiso 1 1 calc R . . H21B H -0.0165 0.1991 0.0536 0.091 Uiso 1 1 calc R . . H21C H 0.0614 0.2178 -0.0039 0.091 Uiso 1 1 calc R . . C22 C 0.11425(14) 0.13194(8) 0.1755(5) 0.0845(7) Uani 1 1 d . . . H22A H 0.1495 0.1425 0.0671 0.127 Uiso 1 1 calc R . . H22B H 0.0775 0.1158 0.0962 0.127 Uiso 1 1 calc R . . H22C H 0.1390 0.1145 0.2853 0.127 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 Si1 0.0370(3) 0.0501(3) 0.0458(4) 0.000 0.000 -0.0100(2) Si2 0.0370(2) 0.0509(3) 0.0384(3) -0.00613(17) 0.00263(16) -0.00588(14) C1 0.0410(8) 0.0635(9) 0.0490(10) -0.0003(9) 0.0015(7) -0.0118(7) C2 0.0404(8) 0.0647(10) 0.0470(9) 0.0001(8) 0.0028(7) -0.0099(7) C3 0.0634(11) 0.0643(11) 0.0759(14) 0.0085(10) -0.0171(11) -0.0090(9) C20 0.0528(9) 0.0668(11) 0.0516(10) 0.0020(10) 0.0039(8) -0.0185(8) C21 0.0671(11) 0.0689(11) 0.0459(10) 0.0041(8) -0.0062(9) -0.0085(9) C22 0.0742(14) 0.0889(15) 0.0904(17) -0.0381(14) 0.0074(12) 0.0160(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C1 1.8451(18) . ? Si1 C1 1.8451(18) 14 ? Si1 C3 1.845(2) . ? Si1 C3 1.845(2) 14 ? Si2 C2 1.8435(17) . ? Si2 C20 1.8468(18) . ? Si2 C21 1.860(2) . ? Si2 C22 1.861(2) . ? C1 C2 1.204(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 C1 Si1 C1 107.38(12) . 14 ? C1 Si1 C3 109.52(9) . . ? C1 Si1 C3 109.76(9) 14 . ? C1 Si1 C3 109.76(9) . 14 ? C1 Si1 C3 109.52(9) 14 14 ? C3 Si1 C3 110.83(17) . 14 ? C2 Si2 C20 108.29(8) . . ? C2 Si2 C21 108.61(8) . . ? C20 Si2 C21 110.53(9) . . ? C2 Si2 C22 108.76(10) . . ? C20 Si2 C22 110.17(12) . . ? C21 Si2 C22 110.42(12) . . ? C2 C1 Si1 176.51(16) . . ? C1 C2 Si2 178.14(16) . . ? 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 C1 Si1 C1 C2 -168(3) 14 . . . ? C3 Si1 C1 C2 73(3) . . . . ? C3 Si1 C1 C2 -49(3) 14 . . . ? Si1 C1 C2 Si2 -18(7) . . . . ? C20 Si2 C2 C1 14(5) . . . . ? C21 Si2 C2 C1 134(5) . . . . ? C22 Si2 C2 C1 -106(5) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 67.48 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.132 _refine_diff_density_min -0.170 _refine_diff_density_rms 0.038 # Attachment 'erk5211.cif' data_erk5211 _database_code_depnum_ccdc_archive 'CCDC 765607' #TrackingRef 'erk5211.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H25 B F10 Si3' _chemical_formula_weight 598.52 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.7841(7) _cell_length_b 6.5724(2) _cell_length_c 33.4388(9) _cell_angle_alpha 90.00 _cell_angle_beta 107.519(1) _cell_angle_gamma 90.00 _cell_volume 5613.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5787 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 27.88 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9292 _exptl_absorpt_correction_T_max 0.9975 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21439 _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 27.75 _reflns_number_total 6379 _reflns_number_gt 4407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0293P)^2^+23.8502P] 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 6379 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1332 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Si1 Si 0.41361(4) 0.13981(16) 0.17240(3) 0.0374(2) Uani 1 1 d . . . C11 C 0.43319(17) 0.3480(7) 0.21189(13) 0.0619(12) Uani 1 1 d . . . H11A H 0.4659 0.4075 0.2108 0.093 Uiso 1 1 calc R . . H11B H 0.4377 0.2931 0.2397 0.093 Uiso 1 1 calc R . . H11C H 0.4062 0.4517 0.2058 0.093 Uiso 1 1 calc R . . C12 C 0.46082(15) -0.0759(7) 0.18581(13) 0.0562(11) Uani 1 1 d . . . H12A H 0.4498 -0.1816 0.1647 0.084 Uiso 1 1 calc R . . H12B H 0.4619 -0.1305 0.2130 0.084 Uiso 1 1 calc R . . H12C H 0.4954 -0.0281 0.1867 0.084 Uiso 1 1 calc R . . C2 C 0.34229(13) 0.0692(5) 0.16168(10) 0.0343(7) Uani 1 1 d . . . Si21 Si 0.31717(4) -0.05397(17) 0.20244(3) 0.0413(2) Uani 1 1 d . . . C22 C 0.37310(18) -0.0952(8) 0.25111(12) 0.0676(13) Uani 1 1 d . . . H22A H 0.3604 -0.1595 0.2723 0.101 Uiso 1 1 calc R . . H22B H 0.3889 0.0348 0.2615 0.101 Uiso 1 1 calc R . . H22C H 0.3990 -0.1821 0.2448 0.101 Uiso 1 1 calc R . . C23 C 0.26903(19) 0.1107(7) 0.21773(14) 0.0670(13) Uani 1 1 d . . . H23A H 0.2469 0.1793 0.1931 0.100 Uiso 1 1 calc R . . H23B H 0.2877 0.2109 0.2380 0.100 Uiso 1 1 calc R . . H23C H 0.2476 0.0272 0.2300 0.100 Uiso 1 1 calc R . . C24 C 0.29135(18) -0.3115(7) 0.18463(14) 0.0613(11) Uani 1 1 d . . . H24A H 0.2576 -0.2991 0.1634 0.092 Uiso 1 1 calc R . . H24B H 0.2874 -0.3881 0.2083 0.092 Uiso 1 1 calc R . . H24C H 0.3156 -0.3817 0.1729 0.092 Uiso 1 1 calc R . . C3 C 0.31680(13) 0.1278(5) 0.12143(10) 0.0351(7) Uani 1 1 d . . . Si31 Si 0.24563(4) 0.12237(17) 0.08790(3) 0.0404(2) Uani 1 1 d . . . C32 C 0.24235(18) -0.0128(9) 0.03835(14) 0.0743(15) Uani 1 1 d . . . H32A H 0.2067 -0.0094 0.0198 0.111 Uiso 1 1 calc R . . H32B H 0.2532 -0.1531 0.0445 0.111 Uiso 1 1 calc R . . H32C H 0.2654 0.0534 0.0249 0.111 Uiso 1 1 calc R . . C33 C 0.19736(16) -0.0037(9) 0.11004(14) 0.0757(16) Uani 1 1 d . . . H33A H 0.1623 0.0140 0.0909 0.114 Uiso 1 1 calc R . . H33B H 0.1993 0.0572 0.1369 0.114 Uiso 1 1 calc R . . H33C H 0.2053 -0.1477 0.1138 0.114 Uiso 1 1 calc R . . C34 C 0.2263(2) 0.3915(8) 0.07582(17) 0.0819(16) Uani 1 1 d . . . H34A H 0.2511 0.4570 0.0639 0.123 Uiso 1 1 calc R . . H34B H 0.2263 0.4612 0.1014 0.123 Uiso 1 1 calc R . . H34C H 0.1916 0.3971 0.0559 0.123 Uiso 1 1 calc R . . C4 C 0.35155(13) 0.2197(5) 0.09874(10) 0.0372(8) Uani 1 1 d . . . H4 H 0.3373 0.2636 0.0709 0.045 Uiso 1 1 calc R . . C5 C 0.40364(13) 0.2398(6) 0.11832(10) 0.0385(8) Uani 1 1 d . . . B1 B 0.44194(16) 0.3113(6) 0.09559(12) 0.0386(9) Uani 1 1 d . . . C51 C 0.50193(13) 0.2509(6) 0.11369(10) 0.0379(8) Uani 1 1 d . . . C52 C 0.52204(14) 0.0665(6) 0.10650(11) 0.0424(8) Uani 1 1 d . . . F52 F 0.49022(9) -0.0724(4) 0.08198(8) 0.0643(7) Uani 1 1 d . . . C53 C 0.57435(15) 0.0156(6) 0.12289(12) 0.0472(9) Uani 1 1 d . . . F53 F 0.59216(10) -0.1643(4) 0.11409(9) 0.0703(7) Uani 1 1 d . . . C54 C 0.60785(14) 0.1515(7) 0.14816(12) 0.0487(10) Uani 1 1 d . . . F54 F 0.65868(8) 0.1035(4) 0.16437(8) 0.0694(7) Uani 1 1 d . . . C55 C 0.58973(15) 0.3353(7) 0.15674(11) 0.0479(9) Uani 1 1 d . . . F55 F 0.62244(10) 0.4680(5) 0.18226(8) 0.0779(8) Uani 1 1 d . . . C56 C 0.53770(14) 0.3822(6) 0.13936(11) 0.0432(8) Uani 1 1 d . . . F56 F 0.52050(9) 0.5646(4) 0.14844(8) 0.0642(7) Uani 1 1 d . . . C61 C 0.42518(13) 0.4514(6) 0.05523(10) 0.0369(7) Uani 1 1 d . . . C62 C 0.39939(13) 0.6337(6) 0.05446(10) 0.0389(8) Uani 1 1 d . . . F62 F 0.38453(9) 0.6933(4) 0.08765(6) 0.0546(6) Uani 1 1 d . . . C63 C 0.38949(14) 0.7679(6) 0.02129(11) 0.0418(8) Uani 1 1 d . . . F63 F 0.36630(10) 0.9474(4) 0.02249(7) 0.0622(6) Uani 1 1 d . . . C64 C 0.40459(14) 0.7186(6) -0.01326(11) 0.0444(9) Uani 1 1 d . . . F64 F 0.39554(9) 0.8482(4) -0.04558(7) 0.0644(7) Uani 1 1 d . . . C65 C 0.42884(14) 0.5366(6) -0.01447(10) 0.0439(9) Uani 1 1 d . . . F65 F 0.44285(9) 0.4855(4) -0.04866(7) 0.0619(7) Uani 1 1 d . . . C66 C 0.43916(14) 0.4077(6) 0.01929(11) 0.0417(8) Uani 1 1 d . . . F66 F 0.46422(9) 0.2317(4) 0.01725(7) 0.0559(6) 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 Si1 0.0307(5) 0.0469(6) 0.0330(5) 0.0057(4) 0.0069(4) 0.0016(4) C11 0.054(3) 0.071(3) 0.052(2) -0.009(2) 0.0035(19) -0.012(2) C12 0.046(2) 0.072(3) 0.052(2) 0.015(2) 0.0164(18) 0.018(2) C2 0.0353(18) 0.0379(18) 0.0309(16) 0.0009(14) 0.0116(13) -0.0011(14) Si21 0.0448(6) 0.0477(6) 0.0348(5) 0.0041(4) 0.0171(4) -0.0022(5) C22 0.074(3) 0.091(4) 0.036(2) 0.013(2) 0.013(2) -0.005(3) C23 0.083(3) 0.067(3) 0.069(3) -0.002(2) 0.049(3) 0.006(3) C24 0.062(3) 0.053(2) 0.073(3) 0.008(2) 0.026(2) -0.005(2) C3 0.0315(17) 0.0401(18) 0.0337(17) 0.0009(14) 0.0098(13) 0.0011(14) Si31 0.0298(5) 0.0528(6) 0.0364(5) 0.0011(4) 0.0065(4) -0.0008(4) C32 0.060(3) 0.104(4) 0.057(3) -0.028(3) 0.016(2) -0.017(3) C33 0.038(2) 0.123(5) 0.065(3) 0.018(3) 0.013(2) -0.014(3) C34 0.065(3) 0.068(3) 0.090(4) 0.002(3) -0.011(3) 0.017(3) C4 0.0351(18) 0.0416(19) 0.0369(17) 0.0069(15) 0.0138(14) 0.0025(15) C5 0.0329(19) 0.045(2) 0.0368(18) 0.0079(15) 0.0097(14) 0.0010(15) B1 0.034(2) 0.042(2) 0.038(2) -0.0007(17) 0.0092(16) 0.0002(17) C51 0.0310(18) 0.045(2) 0.0385(18) 0.0068(15) 0.0111(14) -0.0030(15) C52 0.0326(19) 0.049(2) 0.045(2) -0.0004(17) 0.0120(15) -0.0036(16) F52 0.0516(14) 0.0530(14) 0.0810(17) -0.0124(13) 0.0091(12) -0.0073(12) C53 0.043(2) 0.047(2) 0.056(2) 0.0079(18) 0.0218(18) 0.0062(17) F53 0.0567(15) 0.0607(16) 0.097(2) -0.0011(14) 0.0279(14) 0.0154(13) C54 0.0274(19) 0.071(3) 0.050(2) 0.013(2) 0.0143(16) 0.0011(18) F54 0.0298(12) 0.100(2) 0.0764(16) 0.0187(15) 0.0137(11) 0.0086(13) C55 0.038(2) 0.063(3) 0.040(2) -0.0034(18) 0.0086(16) -0.0090(19) F55 0.0495(15) 0.099(2) 0.0769(17) -0.0251(16) 0.0063(13) -0.0188(15) C56 0.0336(19) 0.054(2) 0.046(2) 0.0003(17) 0.0177(15) -0.0003(17) F56 0.0563(15) 0.0586(15) 0.0790(17) -0.0179(13) 0.0223(13) 0.0010(12) C61 0.0298(17) 0.049(2) 0.0320(16) 0.0025(15) 0.0095(13) -0.0063(15) C62 0.0360(19) 0.050(2) 0.0313(17) -0.0010(15) 0.0111(14) -0.0010(16) F62 0.0646(15) 0.0613(14) 0.0432(12) 0.0034(11) 0.0242(11) 0.0115(12) C63 0.0348(19) 0.046(2) 0.0420(19) 0.0045(16) 0.0078(15) 0.0012(16) F63 0.0723(17) 0.0573(14) 0.0568(14) 0.0119(12) 0.0192(12) 0.0194(13) C64 0.036(2) 0.061(2) 0.0337(18) 0.0089(17) 0.0073(15) -0.0050(18) F64 0.0653(16) 0.0821(18) 0.0455(13) 0.0261(12) 0.0162(11) 0.0086(14) C65 0.036(2) 0.065(2) 0.0320(17) 0.0004(17) 0.0125(14) -0.0018(18) F65 0.0583(15) 0.0930(19) 0.0411(12) 0.0002(12) 0.0252(11) 0.0025(14) C66 0.0349(19) 0.049(2) 0.0434(19) -0.0003(16) 0.0148(15) -0.0008(16) F66 0.0626(15) 0.0565(14) 0.0547(13) 0.0000(11) 0.0269(11) 0.0099(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 Si1 C12 1.862(4) . ? Si1 C11 1.864(4) . ? Si1 C5 1.866(3) . ? Si1 C2 1.892(3) . ? C2 C3 1.368(4) . ? C2 Si21 1.876(3) . ? Si21 C24 1.857(4) . ? Si21 C23 1.869(4) . ? Si21 C22 1.870(4) . ? C3 C4 1.494(4) . ? C3 Si31 1.899(3) . ? Si31 C34 1.853(5) . ? Si31 C32 1.859(4) . ? Si31 C33 1.866(4) . ? C4 C5 1.357(5) . ? C5 B1 1.523(5) . ? B1 C61 1.583(5) . ? B1 C51 1.588(5) . ? C51 C52 1.377(5) . ? C51 C56 1.380(5) . ? C52 F52 1.346(4) . ? C52 C53 1.383(5) . ? C53 F53 1.340(4) . ? C53 C54 1.364(6) . ? C54 F54 1.343(4) . ? C54 C55 1.364(6) . ? C55 F55 1.344(4) . ? C55 C56 1.374(5) . ? C56 F56 1.351(4) . ? C61 C62 1.379(5) . ? C61 C66 1.392(5) . ? C62 F62 1.345(4) . ? C62 C63 1.379(5) . ? C63 F63 1.340(4) . ? C63 C64 1.373(5) . ? C64 F64 1.340(4) . ? C64 C65 1.367(6) . ? C65 F65 1.348(4) . ? C65 C66 1.371(5) . ? C66 F66 1.350(4) . ? 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 C12 Si1 C11 111.3(2) . . ? C12 Si1 C5 112.96(17) . . ? C11 Si1 C5 110.85(19) . . ? C12 Si1 C2 115.62(18) . . ? C11 Si1 C2 111.51(18) . . ? C5 Si1 C2 93.49(15) . . ? C3 C2 Si21 130.9(3) . . ? C3 C2 Si1 107.1(2) . . ? Si21 C2 Si1 122.05(17) . . ? C24 Si21 C23 113.2(2) . . ? C24 Si21 C22 105.7(2) . . ? C23 Si21 C22 106.5(2) . . ? C24 Si21 C2 109.92(18) . . ? C23 Si21 C2 112.13(18) . . ? C22 Si21 C2 109.04(18) . . ? C2 C3 C4 114.2(3) . . ? C2 C3 Si31 133.7(3) . . ? C4 C3 Si31 112.1(2) . . ? C34 Si31 C32 109.1(3) . . ? C34 Si31 C33 109.2(3) . . ? C32 Si31 C33 106.8(2) . . ? C34 Si31 C3 105.97(19) . . ? C32 Si31 C3 107.77(18) . . ? C33 Si31 C3 117.80(18) . . ? C5 C4 C3 120.1(3) . . ? C4 C5 B1 122.6(3) . . ? C4 C5 Si1 105.1(2) . . ? B1 C5 Si1 132.1(3) . . ? C5 B1 C61 123.0(3) . . ? C5 B1 C51 119.3(3) . . ? C61 B1 C51 117.7(3) . . ? C52 C51 C56 115.1(3) . . ? C52 C51 B1 123.9(3) . . ? C56 C51 B1 120.9(3) . . ? F52 C52 C51 119.6(3) . . ? F52 C52 C53 117.2(3) . . ? C51 C52 C53 123.1(4) . . ? F53 C53 C54 120.2(3) . . ? F53 C53 C52 120.7(4) . . ? C54 C53 C52 119.1(4) . . ? F54 C54 C53 119.6(4) . . ? F54 C54 C55 120.3(4) . . ? C53 C54 C55 120.1(3) . . ? F55 C55 C54 120.2(4) . . ? F55 C55 C56 120.5(4) . . ? C54 C55 C56 119.3(4) . . ? F56 C56 C55 118.4(3) . . ? F56 C56 C51 118.3(3) . . ? C55 C56 C51 123.3(4) . . ? C62 C61 C66 115.2(3) . . ? C62 C61 B1 122.2(3) . . ? C66 C61 B1 122.4(3) . . ? F62 C62 C63 116.4(3) . . ? F62 C62 C61 120.6(3) . . ? C63 C62 C61 123.0(3) . . ? F63 C63 C64 119.3(3) . . ? F63 C63 C62 121.2(3) . . ? C64 C63 C62 119.5(3) . . ? F64 C64 C65 120.3(3) . . ? F64 C64 C63 120.1(4) . . ? C65 C64 C63 119.6(3) . . ? F65 C65 C64 119.9(3) . . ? F65 C65 C66 120.4(4) . . ? C64 C65 C66 119.7(3) . . ? F66 C66 C65 117.9(3) . . ? F66 C66 C61 119.2(3) . . ? C65 C66 C61 122.9(4) . . ? 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 C12 Si1 C2 C3 -119.6(3) . . . . ? C11 Si1 C2 C3 112.0(3) . . . . ? C5 Si1 C2 C3 -2.0(3) . . . . ? C12 Si1 C2 Si21 61.3(3) . . . . ? C11 Si1 C2 Si21 -67.1(3) . . . . ? C5 Si1 C2 Si21 178.9(2) . . . . ? C3 C2 Si21 C24 64.2(4) . . . . ? Si1 C2 Si21 C24 -116.9(2) . . . . ? C3 C2 Si21 C23 -62.7(4) . . . . ? Si1 C2 Si21 C23 116.2(2) . . . . ? C3 C2 Si21 C22 179.7(4) . . . . ? Si1 C2 Si21 C22 -1.5(3) . . . . ? Si21 C2 C3 C4 -179.3(3) . . . . ? Si1 C2 C3 C4 1.7(4) . . . . ? Si21 C2 C3 Si31 2.1(6) . . . . ? Si1 C2 C3 Si31 -177.0(2) . . . . ? C2 C3 Si31 C34 117.1(4) . . . . ? C4 C3 Si31 C34 -61.6(3) . . . . ? C2 C3 Si31 C32 -126.2(4) . . . . ? C4 C3 Si31 C32 55.1(3) . . . . ? C2 C3 Si31 C33 -5.4(5) . . . . ? C4 C3 Si31 C33 175.9(3) . . . . ? C2 C3 C4 C5 -0.3(5) . . . . ? Si31 C3 C4 C5 178.6(3) . . . . ? C3 C4 C5 B1 173.4(3) . . . . ? C3 C4 C5 Si1 -1.2(4) . . . . ? C12 Si1 C5 C4 121.6(3) . . . . ? C11 Si1 C5 C4 -112.8(3) . . . . ? C2 Si1 C5 C4 1.8(3) . . . . ? C12 Si1 C5 B1 -52.4(4) . . . . ? C11 Si1 C5 B1 73.2(4) . . . . ? C2 Si1 C5 B1 -172.2(4) . . . . ? C4 C5 B1 C61 26.3(6) . . . . ? Si1 C5 B1 C61 -160.6(3) . . . . ? C4 C5 B1 C51 -156.0(4) . . . . ? Si1 C5 B1 C51 17.1(6) . . . . ? C5 B1 C51 C52 82.1(5) . . . . ? C61 B1 C51 C52 -100.1(4) . . . . ? C5 B1 C51 C56 -95.9(4) . . . . ? C61 B1 C51 C56 81.9(4) . . . . ? C56 C51 C52 F52 179.7(3) . . . . ? B1 C51 C52 F52 1.7(5) . . . . ? C56 C51 C52 C53 -1.2(5) . . . . ? B1 C51 C52 C53 -179.3(3) . . . . ? F52 C52 C53 F53 0.7(5) . . . . ? C51 C52 C53 F53 -178.4(3) . . . . ? F52 C52 C53 C54 -179.5(3) . . . . ? C51 C52 C53 C54 1.4(6) . . . . ? F53 C53 C54 F54 -0.4(6) . . . . ? C52 C53 C54 F54 179.8(3) . . . . ? F53 C53 C54 C55 179.4(3) . . . . ? C52 C53 C54 C55 -0.5(6) . . . . ? F54 C54 C55 F55 -1.5(6) . . . . ? C53 C54 C55 F55 178.7(4) . . . . ? F54 C54 C55 C56 179.2(3) . . . . ? C53 C54 C55 C56 -0.6(6) . . . . ? F55 C55 C56 F56 0.3(5) . . . . ? C54 C55 C56 F56 179.6(3) . . . . ? F55 C55 C56 C51 -178.5(3) . . . . ? C54 C55 C56 C51 0.8(6) . . . . ? C52 C51 C56 F56 -178.7(3) . . . . ? B1 C51 C56 F56 -0.6(5) . . . . ? C52 C51 C56 C55 0.1(5) . . . . ? B1 C51 C56 C55 178.2(3) . . . . ? C5 B1 C61 C62 53.6(5) . . . . ? C51 B1 C61 C62 -124.1(4) . . . . ? C5 B1 C61 C66 -131.8(4) . . . . ? C51 B1 C61 C66 50.5(5) . . . . ? C66 C61 C62 F62 -179.2(3) . . . . ? B1 C61 C62 F62 -4.2(5) . . . . ? C66 C61 C62 C63 -2.2(5) . . . . ? B1 C61 C62 C63 172.8(3) . . . . ? F62 C62 C63 F63 0.0(5) . . . . ? C61 C62 C63 F63 -177.1(3) . . . . ? F62 C62 C63 C64 178.7(3) . . . . ? C61 C62 C63 C64 1.6(6) . . . . ? F63 C63 C64 F64 -0.8(5) . . . . ? C62 C63 C64 F64 -179.5(3) . . . . ? F63 C63 C64 C65 179.2(3) . . . . ? C62 C63 C64 C65 0.5(5) . . . . ? F64 C64 C65 F65 -1.2(5) . . . . ? C63 C64 C65 F65 178.7(3) . . . . ? F64 C64 C65 C66 178.2(3) . . . . ? C63 C64 C65 C66 -1.8(5) . . . . ? F65 C65 C66 F66 1.0(5) . . . . ? C64 C65 C66 F66 -178.5(3) . . . . ? F65 C65 C66 C61 -179.4(3) . . . . ? C64 C65 C66 C61 1.2(6) . . . . ? C62 C61 C66 F66 -179.5(3) . . . . ? B1 C61 C66 F66 5.5(5) . . . . ? C62 C61 C66 C65 0.8(5) . . . . ? B1 C61 C66 C65 -174.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.75 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.343 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.066