# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1574 #==================== data_general _publ_contact_author ; Dr. Honglae Sohn Department of Chemistry and Biochemistry University of California, San Diego La Jolla, CA 92093-0358 USA ; _publ_contact_author_email hsohn@chem.ucsd.edu _publ_contact_author_fax 1(858)534-5383 _publ_contact_author_phone 1(858)534-6176 _publ_requested_journal 'Journal name' loop_ _publ_author_name _publ_author_address 'Honglae Sohn' ; Department of Chemistry and Biochemistry University of California, San Diego 9500 Gilman Drive La Jolla, CA 92093-0358 USA ; 'Hee-Gweon Woo' ; Department of Chemistry Chonnam National University Kwangju 500-757 Korea ; 'Douglas R. Powell' ; Department of Chemistry University of Wisconsin 1101 University Ave. Madison, WI 53705 USA ; _publ_section_title ; Synthesis and Structural Characterization of a Silacycloheptadiene ; #==================== data_hs28 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H26 Cl4 Si2' _chemical_formula_weight 608.51 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.8402(3) _cell_length_b 20.6247(9) _cell_length_c 21.2353(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.484(2) _cell_angle_gamma 90.00 _cell_volume 2993.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 6027 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.5 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method ? _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.497 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.950 _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4/CCD' _diffrn_measurement_method 'phi scans' _diffrn_standards_number 190 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.06 _diffrn_reflns_number 11579 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.01 _reflns_number_total 4952 _reflns_number_observed 3967 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+6.1185P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4949 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_obs 0.0516 _refine_ls_wR_factor_all 0.1215 _refine_ls_wR_factor_obs 0.1031 _refine_ls_goodness_of_fit_all 1.204 _refine_ls_goodness_of_fit_obs 1.166 _refine_ls_restrained_S_all 1.220 _refine_ls_restrained_S_obs 1.166 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cl1 Cl -0.15610(14) 0.35117(5) 0.39042(5) 0.0342(3) Uani 1 d . . Cl2 Cl -0.16121(13) 0.34225(5) 0.23780(4) 0.0276(2) Uani 1 d . . Cl3 Cl 0.3334(2) 0.40532(7) 0.45686(5) 0.0569(4) Uani 1 d . . Cl4 Cl 0.4686(2) 0.52428(6) 0.36401(6) 0.0515(3) Uani 1 d . . Si1 Si 0.02676(14) 0.34164(5) 0.31687(5) 0.0214(2) Uani 1 d . . Si2 Si 0.2408(2) 0.46366(5) 0.38333(5) 0.0288(3) Uani 1 d . . C1 C 0.1630(5) 0.2631(2) 0.3236(2) 0.0219(8) Uani 1 d . . C2 C 0.2793(5) 0.2454(2) 0.2761(2) 0.0192(7) Uani 1 d . . C3 C 0.2983(5) 0.2871(2) 0.2184(2) 0.0185(7) Uani 1 d . . C4 C 0.3420(5) 0.3510(2) 0.2218(2) 0.0184(7) Uani 1 d . . C5 C 0.3878(5) 0.3850(2) 0.2842(2) 0.0206(8) Uani 1 d . . H5A H 0.4805(5) 0.4211(2) 0.2777(2) 0.025 Uiso 1 calc R . H5B H 0.4506(5) 0.3541(2) 0.3144(2) 0.025 Uiso 1 calc R . C6 C 0.1964(5) 0.4122(2) 0.3118(2) 0.0212(8) Uani 1 d . . H6 H 0.1368(5) 0.4415(2) 0.2787(2) 0.025 Uiso 1 calc R . C7 C 0.1561(6) 0.2255(2) 0.3840(2) 0.0254(8) Uani 1 d . . C8 C 0.3214(7) 0.2220(2) 0.4244(2) 0.0353(10) Uani 1 d . . H8 H 0.4373(7) 0.2443(2) 0.4141(2) 0.042 Uiso 1 calc R . C9 C 0.3180(9) 0.1859(2) 0.4800(2) 0.0484(13) Uani 1 d . . H9 H 0.4315(9) 0.1836(2) 0.5073(2) 0.058 Uiso 1 calc R . C10 C 0.1503(9) 0.1535(2) 0.4953(2) 0.0535(15) Uani 1 d . . H10 H 0.1483(9) 0.1289(2) 0.5331(2) 0.064 Uiso 1 calc R . C11 C -0.0151(8) 0.1568(2) 0.4556(2) 0.0477(13) Uani 1 d . . H11 H -0.1301(8) 0.1341(2) 0.4661(2) 0.057 Uiso 1 calc R . C12 C -0.0145(6) 0.1932(2) 0.4002(2) 0.0336(10) Uani 1 d . . H12 H -0.1295(6) 0.1962(2) 0.3737(2) 0.040 Uiso 1 calc R . C13 C 0.3926(5) 0.1830(2) 0.2758(2) 0.0203(8) Uani 1 d . . C14 C 0.3117(6) 0.1242(2) 0.2947(2) 0.0265(8) Uani 1 d . . H14 H 0.1806(6) 0.1231(2) 0.3077(2) 0.032 Uiso 1 calc R . C15 C 0.4213(6) 0.0676(2) 0.2945(2) 0.0334(10) Uani 1 d . . H15 H 0.3653(6) 0.0280(2) 0.3076(2) 0.040 Uiso 1 calc R . C16 C 0.6117(6) 0.0687(2) 0.2752(2) 0.0374(10) Uani 1 d . . H16 H 0.6864(6) 0.0298(2) 0.2754(2) 0.045 Uiso 1 calc R . C17 C 0.6942(6) 0.1264(2) 0.2555(2) 0.0351(10) Uani 1 d . . H17 H 0.8249(6) 0.1272(2) 0.2420(2) 0.042 Uiso 1 calc R . C18 C 0.5837(5) 0.1828(2) 0.2556(2) 0.0278(9) Uani 1 d . . H18 H 0.6397(5) 0.2221(2) 0.2417(2) 0.033 Uiso 1 calc R . C19 C 0.2601(5) 0.2525(2) 0.1571(2) 0.0209(8) Uani 1 d . . C20 C 0.0845(5) 0.2192(2) 0.1461(2) 0.0257(8) Uani 1 d . . H20 H -0.0085(5) 0.2176(2) 0.1781(2) 0.031 Uiso 1 calc R . C21 C 0.0448(6) 0.1885(2) 0.0887(2) 0.0331(9) Uani 1 d . . H21 H -0.0769(6) 0.1671(2) 0.0810(2) 0.040 Uiso 1 calc R . C22 C 0.1828(7) 0.1889(2) 0.0428(2) 0.0359(10) Uani 1 d . . H22 H 0.1559(7) 0.1677(2) 0.0037(2) 0.043 Uiso 1 calc R . C23 C 0.3602(6) 0.2204(2) 0.0540(2) 0.0322(9) Uani 1 d . . H23 H 0.4556(6) 0.2200(2) 0.0228(2) 0.039 Uiso 1 calc R . C24 C 0.3986(6) 0.2525(2) 0.1106(2) 0.0262(8) Uani 1 d . . H24 H 0.5195(6) 0.2745(2) 0.1178(2) 0.031 Uiso 1 calc R . C25 C 0.3323(5) 0.3953(2) 0.1656(2) 0.0202(8) Uani 1 d . . C26 C 0.1708(6) 0.3948(2) 0.1222(2) 0.0258(8) Uani 1 d . . H26 H 0.0691(6) 0.3640(2) 0.1269(2) 0.031 Uiso 1 calc R . C27 C 0.1581(6) 0.4388(2) 0.0724(2) 0.0315(9) Uani 1 d . . H27 H 0.0473(6) 0.4381(2) 0.0438(2) 0.038 Uiso 1 calc R . C28 C 0.3055(6) 0.4834(2) 0.0643(2) 0.0342(10) Uani 1 d . . H28 H 0.2970(6) 0.5130(2) 0.0300(2) 0.041 Uiso 1 calc R . C29 C 0.4655(6) 0.4846(2) 0.1064(2) 0.0339(10) Uani 1 d . . H29 H 0.5666(6) 0.5155(2) 0.1011(2) 0.041 Uiso 1 calc R . C30 C 0.4796(6) 0.4412(2) 0.1563(2) 0.0274(9) Uani 1 d . . H30 H 0.5909(6) 0.4425(2) 0.1846(2) 0.033 Uiso 1 calc R . C31 C 0.0300(6) 0.5117(2) 0.4066(2) 0.0368(10) Uani 1 d . . H31 H -0.0648(6) 0.4913(2) 0.4314(2) 0.044 Uiso 1 calc R . C32 C 0.0032(7) 0.5728(2) 0.3907(2) 0.0463(12) Uani 1 d . . H32A H 0.0957(7) 0.5942(2) 0.3659(2) 0.056 Uiso 1 calc R . H32B H -0.1087(7) 0.5954(2) 0.4040(2) 0.056 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0355(5) 0.0352(6) 0.0331(5) 0.0037(4) 0.0161(4) 0.0048(4) Cl2 0.0211(4) 0.0298(5) 0.0317(5) 0.0013(4) -0.0011(4) -0.0001(4) Cl3 0.0709(9) 0.0673(9) 0.0315(6) 0.0017(6) -0.0099(6) 0.0300(7) Cl4 0.0396(6) 0.0428(7) 0.0725(9) -0.0288(6) 0.0075(6) -0.0104(5) Si1 0.0223(5) 0.0204(6) 0.0218(5) 0.0027(4) 0.0042(4) 0.0019(4) Si2 0.0313(6) 0.0269(6) 0.0279(6) -0.0066(5) -0.0018(4) 0.0056(5) C1 0.028(2) 0.018(2) 0.020(2) 0.0011(15) 0.0013(15) -0.0011(15) C2 0.020(2) 0.019(2) 0.018(2) -0.0002(14) -0.0019(14) -0.0030(14) C3 0.017(2) 0.019(2) 0.019(2) 0.0013(14) 0.0002(13) 0.0004(14) C4 0.017(2) 0.015(2) 0.023(2) 0.0009(14) 0.0026(13) 0.0005(13) C5 0.020(2) 0.017(2) 0.024(2) -0.0018(15) 0.0010(15) -0.0010(14) C6 0.023(2) 0.021(2) 0.020(2) 0.0011(15) 0.0017(14) 0.0015(14) C7 0.044(2) 0.012(2) 0.021(2) 0.0022(15) 0.006(2) 0.005(2) C8 0.055(3) 0.023(2) 0.027(2) 0.001(2) -0.004(2) 0.005(2) C9 0.093(4) 0.029(3) 0.023(2) 0.001(2) -0.005(2) 0.019(3) C10 0.116(5) 0.024(3) 0.023(2) 0.007(2) 0.020(3) 0.019(3) C11 0.086(4) 0.020(2) 0.041(3) -0.001(2) 0.034(3) -0.006(2) C12 0.050(3) 0.023(2) 0.029(2) -0.002(2) 0.017(2) -0.001(2) C13 0.028(2) 0.016(2) 0.017(2) 0.0009(14) -0.0021(14) 0.0015(14) C14 0.038(2) 0.020(2) 0.022(2) -0.002(2) 0.003(2) -0.001(2) C15 0.055(3) 0.019(2) 0.027(2) 0.003(2) 0.003(2) 0.004(2) C16 0.044(3) 0.025(2) 0.042(3) -0.001(2) -0.006(2) 0.013(2) C17 0.026(2) 0.033(3) 0.046(3) 0.000(2) -0.003(2) 0.009(2) C18 0.028(2) 0.021(2) 0.034(2) 0.000(2) 0.000(2) -0.001(2) C19 0.029(2) 0.011(2) 0.023(2) 0.0033(14) -0.0012(15) 0.0002(14) C20 0.029(2) 0.024(2) 0.024(2) 0.002(2) 0.004(2) -0.005(2) C21 0.041(2) 0.029(2) 0.030(2) 0.000(2) -0.002(2) -0.011(2) C22 0.056(3) 0.029(2) 0.022(2) -0.004(2) 0.000(2) -0.010(2) C23 0.049(3) 0.025(2) 0.023(2) 0.002(2) 0.012(2) -0.006(2) C24 0.032(2) 0.020(2) 0.027(2) 0.002(2) 0.005(2) -0.003(2) C25 0.028(2) 0.013(2) 0.020(2) -0.0024(14) 0.0056(15) 0.0022(14) C26 0.034(2) 0.020(2) 0.023(2) 0.002(2) 0.002(2) -0.001(2) C27 0.046(3) 0.022(2) 0.026(2) 0.002(2) -0.004(2) 0.004(2) C28 0.057(3) 0.019(2) 0.027(2) 0.006(2) 0.006(2) 0.003(2) C29 0.044(3) 0.021(2) 0.038(2) 0.006(2) 0.015(2) -0.006(2) C30 0.033(2) 0.020(2) 0.030(2) 0.003(2) 0.004(2) -0.001(2) C31 0.039(2) 0.032(3) 0.039(2) -0.011(2) 0.004(2) 0.003(2) C32 0.038(3) 0.038(3) 0.062(3) -0.013(2) 0.000(2) 0.010(2) _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 Cl1 Si1 2.0523(13) . ? Cl2 Si1 2.0701(13) . ? Cl3 Si2 2.050(2) . ? Cl4 Si2 2.053(2) . ? Si1 C6 1.868(4) . ? Si1 C1 1.872(4) . ? Si2 C31 1.835(4) . ? Si2 C6 1.867(4) . ? C1 C2 1.361(5) . ? C1 C7 1.502(5) . ? C2 C13 1.501(5) . ? C2 C3 1.507(5) . ? C3 C4 1.353(5) . ? C3 C19 1.497(5) . ? C4 C25 1.501(5) . ? C4 C5 1.520(5) . ? C5 C6 1.562(5) . ? C7 C8 1.392(5) . ? C7 C12 1.399(5) . ? C8 C9 1.397(6) . ? C9 C10 1.378(7) . ? C10 C11 1.383(7) . ? C11 C12 1.395(6) . ? C13 C18 1.394(5) . ? C13 C14 1.398(5) . ? C14 C15 1.388(5) . ? C15 C16 1.382(6) . ? C16 C17 1.390(6) . ? C17 C18 1.386(5) . ? C19 C20 1.394(5) . ? C19 C24 1.398(5) . ? C20 C21 1.391(5) . ? C21 C22 1.386(6) . ? C22 C23 1.388(6) . ? C23 C24 1.387(5) . ? C25 C30 1.403(5) . ? C25 C26 1.407(5) . ? C26 C27 1.394(5) . ? C27 C28 1.381(6) . ? C28 C29 1.383(6) . ? C29 C30 1.387(5) . ? C31 C32 1.315(6) . ? 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 C6 Si1 C1 111.8(2) . . ? C6 Si1 Cl1 111.70(12) . . ? C1 Si1 Cl1 110.06(12) . . ? C6 Si1 Cl2 108.31(12) . . ? C1 Si1 Cl2 110.88(12) . . ? Cl1 Si1 Cl2 103.83(6) . . ? C31 Si2 C6 115.0(2) . . ? C31 Si2 Cl3 109.4(2) . . ? C6 Si2 Cl3 108.69(13) . . ? C31 Si2 Cl4 109.7(2) . . ? C6 Si2 Cl4 106.37(12) . . ? Cl3 Si2 Cl4 107.32(8) . . ? C2 C1 C7 122.4(3) . . ? C2 C1 Si1 118.8(3) . . ? C7 C1 Si1 118.6(3) . . ? C1 C2 C13 123.4(3) . . ? C1 C2 C3 121.5(3) . . ? C13 C2 C3 115.1(3) . . ? C4 C3 C19 122.7(3) . . ? C4 C3 C2 122.7(3) . . ? C19 C3 C2 114.6(3) . . ? C3 C4 C25 123.2(3) . . ? C3 C4 C5 122.2(3) . . ? C25 C4 C5 114.4(3) . . ? C4 C5 C6 110.4(3) . . ? C5 C6 Si2 113.6(2) . . ? C5 C6 Si1 105.9(2) . . ? Si2 C6 Si1 118.4(2) . . ? C8 C7 C12 119.2(4) . . ? C8 C7 C1 119.9(3) . . ? C12 C7 C1 120.9(4) . . ? C7 C8 C9 120.4(4) . . ? C10 C9 C8 120.1(5) . . ? C9 C10 C11 120.0(4) . . ? C10 C11 C12 120.5(5) . . ? C11 C12 C7 119.8(4) . . ? C18 C13 C14 118.2(3) . . ? C18 C13 C2 119.7(3) . . ? C14 C13 C2 122.1(3) . . ? C15 C14 C13 120.5(4) . . ? C16 C15 C14 120.3(4) . . ? C15 C16 C17 120.2(4) . . ? C18 C17 C16 119.3(4) . . ? C17 C18 C13 121.5(4) . . ? C20 C19 C24 119.1(3) . . ? C20 C19 C3 119.8(3) . . ? C24 C19 C3 121.1(3) . . ? C21 C20 C19 120.3(4) . . ? C22 C21 C20 120.0(4) . . ? C21 C22 C23 120.0(4) . . ? C24 C23 C22 120.2(4) . . ? C23 C24 C19 120.2(4) . . ? C30 C25 C26 117.4(3) . . ? C30 C25 C4 121.0(3) . . ? C26 C25 C4 121.5(3) . . ? C27 C26 C25 120.9(4) . . ? C28 C27 C26 120.5(4) . . ? C27 C28 C29 119.5(4) . . ? C28 C29 C30 120.6(4) . . ? C29 C30 C25 121.1(4) . . ? C32 C31 Si2 123.4(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 C6 Si1 C1 C2 -60.9(3) . . . . ? Cl1 Si1 C1 C2 174.4(3) . . . . ? Cl2 Si1 C1 C2 60.1(3) . . . . ? C6 Si1 C1 C7 112.9(3) . . . . ? Cl1 Si1 C1 C7 -11.8(3) . . . . ? Cl2 Si1 C1 C7 -126.2(3) . . . . ? C7 C1 C2 C13 7.5(5) . . . . ? Si1 C1 C2 C13 -179.0(3) . . . . ? C7 C1 C2 C3 -174.2(3) . . . . ? Si1 C1 C2 C3 -0.7(5) . . . . ? C1 C2 C3 C4 51.3(5) . . . . ? C13 C2 C3 C4 -130.3(3) . . . . ? C1 C2 C3 C19 -127.2(4) . . . . ? C13 C2 C3 C19 51.2(4) . . . . ? C19 C3 C4 C25 7.8(5) . . . . ? C2 C3 C4 C25 -170.6(3) . . . . ? C19 C3 C4 C5 -177.7(3) . . . . ? C2 C3 C4 C5 3.9(5) . . . . ? C3 C4 C5 C6 -89.8(4) . . . . ? C25 C4 C5 C6 85.1(4) . . . . ? C4 C5 C6 Si2 -172.9(2) . . . . ? C4 C5 C6 Si1 55.5(3) . . . . ? C31 Si2 C6 C5 166.4(3) . . . . ? Cl3 Si2 C6 C5 -70.5(3) . . . . ? Cl4 Si2 C6 C5 44.7(3) . . . . ? C31 Si2 C6 Si1 -68.4(3) . . . . ? Cl3 Si2 C6 Si1 54.7(2) . . . . ? Cl4 Si2 C6 Si1 169.9(2) . . . . ? C1 Si1 C6 C5 25.3(3) . . . . ? Cl1 Si1 C6 C5 149.2(2) . . . . ? Cl2 Si1 C6 C5 -97.1(2) . . . . ? C1 Si1 C6 Si2 -103.5(2) . . . . ? Cl1 Si1 C6 Si2 20.3(2) . . . . ? Cl2 Si1 C6 Si2 134.1(2) . . . . ? C2 C1 C7 C8 65.0(5) . . . . ? Si1 C1 C7 C8 -108.5(4) . . . . ? C2 C1 C7 C12 -114.5(4) . . . . ? Si1 C1 C7 C12 72.0(4) . . . . ? C12 C7 C8 C9 1.1(6) . . . . ? C1 C7 C8 C9 -178.5(4) . . . . ? C7 C8 C9 C10 -0.2(6) . . . . ? C8 C9 C10 C11 -0.1(7) . . . . ? C9 C10 C11 C12 -0.6(7) . . . . ? C10 C11 C12 C7 1.5(6) . . . . ? C8 C7 C12 C11 -1.7(6) . . . . ? C1 C7 C12 C11 177.8(4) . . . . ? C1 C2 C13 C18 -138.4(4) . . . . ? C3 C2 C13 C18 43.2(4) . . . . ? C1 C2 C13 C14 42.4(5) . . . . ? C3 C2 C13 C14 -136.0(3) . . . . ? C18 C13 C14 C15 1.4(5) . . . . ? C2 C13 C14 C15 -179.4(3) . . . . ? C13 C14 C15 C16 -0.4(6) . . . . ? C14 C15 C16 C17 -0.4(6) . . . . ? C15 C16 C17 C18 0.3(6) . . . . ? C16 C17 C18 C13 0.8(6) . . . . ? C14 C13 C18 C17 -1.6(5) . . . . ? C2 C13 C18 C17 179.2(3) . . . . ? C4 C3 C19 C20 -123.9(4) . . . . ? C2 C3 C19 C20 54.7(4) . . . . ? C4 C3 C19 C24 56.7(5) . . . . ? C2 C3 C19 C24 -124.8(4) . . . . ? C24 C19 C20 C21 -2.4(6) . . . . ? C3 C19 C20 C21 178.1(3) . . . . ? C19 C20 C21 C22 2.2(6) . . . . ? C20 C21 C22 C23 -0.4(6) . . . . ? C21 C22 C23 C24 -1.2(6) . . . . ? C22 C23 C24 C19 0.9(6) . . . . ? C20 C19 C24 C23 0.9(5) . . . . ? C3 C19 C24 C23 -179.7(3) . . . . ? C3 C4 C25 C30 -137.2(4) . . . . ? C5 C4 C25 C30 47.9(4) . . . . ? C3 C4 C25 C26 46.2(5) . . . . ? C5 C4 C25 C26 -128.6(3) . . . . ? C30 C25 C26 C27 -0.6(5) . . . . ? C4 C25 C26 C27 176.0(3) . . . . ? C25 C26 C27 C28 0.8(6) . . . . ? C26 C27 C28 C29 -0.7(6) . . . . ? C27 C28 C29 C30 0.5(6) . . . . ? C28 C29 C30 C25 -0.4(6) . . . . ? C26 C25 C30 C29 0.4(5) . . . . ? C4 C25 C30 C29 -176.2(3) . . . . ? C6 Si2 C31 C32 -96.6(4) . . . . ? Cl3 Si2 C31 C32 140.8(4) . . . . ? Cl4 Si2 C31 C32 23.3(4) . . . . ? _refine_diff_density_max 0.316 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.066 data_97223 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C36 H25 Cl Si' _chemical_formula_structural 'C36 H25 Cl Si' _chemical_formula_analytical ? _chemical_formula_sum 'C36 H25 Cl Si' _chemical_formula_weight 521.10 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1677(3) _cell_length_b 16.5631(4) _cell_length_c 18.6634(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.333(2) _cell_angle_gamma 90.00 _cell_volume 2778.70(14) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour 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 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.204 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 0.978 _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4/CCD' _diffrn_measurement_method 'phi scan frames' _diffrn_standards_number 403 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.06 _diffrn_reflns_number 13288 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 29.17 _reflns_number_total 6555 _reflns_number_observed 5178 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXTL+ (Sheldrick, 1994)' _computing_structure_refinement 'SHELXTL+ (Sheldrick, 1994)' _computing_molecular_graphics 'SHELXTL+ (Sheldrick, 1994)' _computing_publication_material 'SHELXTL+ (Sheldrick, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.9732P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6555 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_obs 0.0394 _refine_ls_wR_factor_all 0.1059 _refine_ls_wR_factor_obs 0.0970 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.059 _refine_ls_restrained_S_all 1.022 _refine_ls_restrained_S_obs 1.059 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Si1 Si 0.58608(5) 0.24823(2) 0.21475(2) 0.02043(10) Uani 1 d . . Cl1 Cl 0.67874(4) 0.35155(2) 0.18161(2) 0.02710(10) Uani 1 d . . C1 C 0.4539(2) 0.27091(9) 0.27617(8) 0.0209(3) Uani 1 d . . C2 C 0.5092(2) 0.23124(9) 0.33960(8) 0.0202(3) Uani 1 d . . C3 C 0.6500(2) 0.18267(8) 0.34195(8) 0.0196(3) Uani 1 d . . C4 C 0.7159(2) 0.18819(9) 0.28296(8) 0.0208(3) Uani 1 d . . C5 C 0.3220(2) 0.32427(9) 0.25926(8) 0.0221(3) Uani 1 d . . C6 C 0.2524(2) 0.33497(10) 0.18611(9) 0.0277(3) Uani 1 d . . H6 H 0.2933(2) 0.30988(10) 0.14875(9) 0.033 Uiso 1 calc R . C7 C 0.1247(2) 0.38159(11) 0.16710(10) 0.0334(4) Uani 1 d . . H7 H 0.0789(2) 0.38779(11) 0.11713(10) 0.040 Uiso 1 calc R . C8 C 0.0641(2) 0.41891(11) 0.22056(11) 0.0350(4) Uani 1 d . . H8 H -0.0248(2) 0.44962(11) 0.20767(11) 0.042 Uiso 1 calc R . C9 C 0.1337(2) 0.41127(10) 0.29317(10) 0.0326(4) Uani 1 d . . H9 H 0.0934(2) 0.43783(10) 0.33003(10) 0.039 Uiso 1 calc R . C10 C 0.2620(2) 0.36501(10) 0.31249(9) 0.0275(3) Uani 1 d . . H10 H 0.3095(2) 0.36101(10) 0.36240(9) 0.033 Uiso 1 calc R . C11 C 0.4487(2) 0.23561(9) 0.40813(8) 0.0214(3) Uani 1 d . . C12 C 0.3138(2) 0.20106(10) 0.41391(10) 0.0308(4) Uani 1 d . . H12 H 0.2581(2) 0.17148(10) 0.37414(10) 0.037 Uiso 1 calc R . C13 C 0.2601(2) 0.20999(12) 0.47853(11) 0.0412(5) Uani 1 d . . H13 H 0.1681(2) 0.18600(12) 0.48274(11) 0.049 Uiso 1 calc R . C14 C 0.3398(2) 0.25336(12) 0.53625(10) 0.0411(5) Uani 1 d . . H14 H 0.3018(2) 0.25990(12) 0.57970(10) 0.049 Uiso 1 calc R . C15 C 0.4745(2) 0.28721(12) 0.53102(9) 0.0355(4) Uani 1 d . . H15 H 0.5296(2) 0.31689(12) 0.57087(9) 0.043 Uiso 1 calc R . C16 C 0.5294(2) 0.27786(10) 0.46744(8) 0.0271(3) Uani 1 d . . H16 H 0.6232(2) 0.30050(10) 0.46426(8) 0.032 Uiso 1 calc R . C17 C 0.7056(2) 0.13113(9) 0.40716(8) 0.0201(3) Uani 1 d . . C18 C 0.6234(2) 0.06452(10) 0.42178(9) 0.0260(3) Uani 1 d . . H18 H 0.5285(2) 0.05423(10) 0.39210(9) 0.031 Uiso 1 calc R . C19 C 0.6792(2) 0.01290(10) 0.47964(9) 0.0324(4) Uani 1 d . . H19 H 0.6242(2) -0.03345(10) 0.48832(9) 0.039 Uiso 1 calc R . C20 C 0.8146(2) 0.02925(11) 0.52428(9) 0.0349(4) Uani 1 d . . H20 H 0.8530(2) -0.00584(11) 0.56377(9) 0.042 Uiso 1 calc R . C21 C 0.8943(2) 0.09651(12) 0.51159(9) 0.0353(4) Uani 1 d . . H21 H 0.9863(2) 0.10838(12) 0.54321(9) 0.042 Uiso 1 calc R . C22 C 0.8411(2) 0.14707(10) 0.45289(9) 0.0282(3) Uani 1 d . . H22 H 0.8977(2) 0.19274(10) 0.44404(9) 0.034 Uiso 1 calc R . C23 C 0.8523(2) 0.14634(9) 0.27124(8) 0.0212(3) Uani 1 d . . C24 C 0.8817(2) 0.06520(10) 0.29035(9) 0.0292(4) Uani 1 d . . H24 H 0.8132(2) 0.03541(10) 0.31211(9) 0.035 Uiso 1 calc R . C25 C 1.0101(2) 0.02808(10) 0.27771(10) 0.0320(4) Uani 1 d . . H25 H 1.0287(2) -0.02688(10) 0.29098(10) 0.038 Uiso 1 calc R . C26 C 1.1113(2) 0.07027(10) 0.24602(9) 0.0295(4) Uani 1 d . . H26 H 1.1992(2) 0.04456(10) 0.23780(9) 0.035 Uiso 1 calc R . C27 C 1.0837(2) 0.14983(10) 0.22646(9) 0.0281(3) Uani 1 d . . H27 H 1.1527(2) 0.17902(10) 0.20457(9) 0.034 Uiso 1 calc R . C28 C 0.9551(2) 0.18766(9) 0.23865(8) 0.0250(3) Uani 1 d . . H28 H 0.9370(2) 0.24244(9) 0.22457(8) 0.030 Uiso 1 calc R . C29 C 0.5085(2) 0.19026(10) 0.13360(8) 0.0273(3) Uani 1 d . . C30 C 0.4490(2) 0.14865(10) 0.08334(9) 0.0287(4) Uani 1 d . . C31 C 0.3722(2) 0.09868(10) 0.02469(9) 0.0300(4) Uani 1 d . . C32 C 0.3988(2) 0.10625(13) -0.04612(10) 0.0407(5) Uani 1 d . . H32 H 0.4703(2) 0.14374(13) -0.05649(10) 0.049 Uiso 1 calc R . C33 C 0.3187(2) 0.0579(2) -0.10150(12) 0.0555(6) Uani 1 d . . H33 H 0.3339(2) 0.0637(2) -0.15014(12) 0.067 Uiso 1 calc R . C34 C 0.2174(2) 0.0016(2) -0.08619(13) 0.0585(7) Uani 1 d . . H34 H 0.1652(2) -0.0319(2) -0.12407(13) 0.070 Uiso 1 calc R . C35 C 0.1922(3) -0.00598(14) -0.01635(13) 0.0522(6) Uani 1 d . . H35 H 0.1229(3) -0.04478(14) -0.00592(13) 0.063 Uiso 1 calc R . C36 C 0.2676(2) 0.04289(11) 0.03885(11) 0.0402(4) Uani 1 d . . H36 H 0.2480(2) 0.03838(11) 0.08681(11) 0.048 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0242(2) 0.0195(2) 0.0177(2) 0.00093(15) 0.0045(2) 0.0015(2) Cl1 0.0302(2) 0.0220(2) 0.0298(2) 0.00469(14) 0.0079(2) 0.00095(14) C1 0.0215(8) 0.0203(7) 0.0207(7) -0.0007(5) 0.0036(6) -0.0010(5) C2 0.0210(8) 0.0191(7) 0.0207(7) -0.0010(5) 0.0046(6) -0.0022(5) C3 0.0209(8) 0.0172(7) 0.0199(7) 0.0000(5) 0.0025(6) -0.0009(5) C4 0.0243(8) 0.0183(7) 0.0197(7) 0.0006(5) 0.0044(6) 0.0016(5) C5 0.0198(8) 0.0204(7) 0.0259(7) 0.0047(6) 0.0040(6) -0.0029(5) C6 0.0273(9) 0.0273(8) 0.0273(8) 0.0051(6) 0.0028(7) -0.0007(6) C7 0.0269(9) 0.0337(9) 0.0361(9) 0.0106(7) -0.0026(7) -0.0017(7) C8 0.0205(9) 0.0316(9) 0.0521(11) 0.0125(8) 0.0052(8) 0.0021(6) C9 0.0278(9) 0.0293(9) 0.0433(10) 0.0052(7) 0.0133(8) 0.0040(7) C10 0.0262(8) 0.0263(8) 0.0305(8) 0.0041(6) 0.0069(7) 0.0025(6) C11 0.0218(8) 0.0224(7) 0.0208(7) 0.0040(5) 0.0056(6) 0.0029(6) C12 0.0264(9) 0.0328(9) 0.0335(9) 0.0058(7) 0.0067(7) -0.0034(7) C13 0.0311(10) 0.0471(11) 0.0513(12) 0.0181(9) 0.0229(9) 0.0014(8) C14 0.0480(12) 0.0502(12) 0.0310(9) 0.0099(8) 0.0220(9) 0.0114(9) C15 0.0435(11) 0.0417(10) 0.0223(8) -0.0011(7) 0.0091(8) 0.0071(8) C16 0.0270(9) 0.0315(8) 0.0237(8) -0.0003(6) 0.0074(7) 0.0005(6) C17 0.0222(8) 0.0206(7) 0.0178(7) 0.0006(5) 0.0048(6) 0.0025(5) C18 0.0252(8) 0.0265(8) 0.0252(8) 0.0029(6) 0.0027(6) -0.0009(6) C19 0.0352(10) 0.0298(9) 0.0341(9) 0.0105(7) 0.0115(8) 0.0025(7) C20 0.0369(10) 0.0422(10) 0.0257(8) 0.0126(7) 0.0068(8) 0.0112(8) C21 0.0287(9) 0.0478(11) 0.0255(8) 0.0020(7) -0.0039(7) 0.0030(8) C22 0.0256(9) 0.0302(8) 0.0272(8) 0.0011(6) 0.0015(7) -0.0025(6) C23 0.0250(8) 0.0217(7) 0.0167(6) -0.0006(5) 0.0036(6) 0.0019(6) C24 0.0358(10) 0.0218(8) 0.0329(9) 0.0018(6) 0.0134(7) 0.0023(6) C25 0.0400(10) 0.0219(8) 0.0357(9) 0.0037(6) 0.0115(8) 0.0092(7) C26 0.0275(9) 0.0321(9) 0.0292(8) -0.0040(7) 0.0067(7) 0.0066(7) C27 0.0270(9) 0.0304(8) 0.0281(8) -0.0015(6) 0.0086(7) -0.0014(6) C28 0.0296(9) 0.0209(7) 0.0252(8) 0.0022(6) 0.0067(7) 0.0016(6) C29 0.0322(9) 0.0273(8) 0.0222(7) -0.0021(6) 0.0052(7) 0.0025(6) C30 0.0319(9) 0.0272(8) 0.0265(8) -0.0007(6) 0.0044(7) 0.0049(7) C31 0.0295(9) 0.0295(8) 0.0286(8) -0.0065(6) -0.0006(7) 0.0066(7) C32 0.0304(10) 0.0573(12) 0.0348(10) -0.0138(9) 0.0073(8) 0.0008(8) C33 0.0399(12) 0.092(2) 0.0346(11) -0.0289(11) 0.0081(9) -0.0014(11) C34 0.0393(12) 0.075(2) 0.0572(14) -0.0372(12) 0.0004(11) -0.0048(11) C35 0.0429(12) 0.0463(12) 0.0649(15) -0.0159(10) 0.0049(11) -0.0103(9) C36 0.0448(11) 0.0350(10) 0.0385(10) -0.0026(8) 0.0023(9) -0.0013(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C29 1.816(2) . ? Si1 C4 1.8523(15) . ? Si1 C1 1.862(2) . ? Si1 Cl1 2.0589(5) . ? C1 C2 1.361(2) . ? C1 C5 1.481(2) . ? C2 C11 1.493(2) . ? C2 C3 1.514(2) . ? C3 C4 1.359(2) . ? C3 C17 1.492(2) . ? C4 C23 1.483(2) . ? C5 C10 1.400(2) . ? C5 C6 1.400(2) . ? C6 C7 1.389(2) . ? C7 C8 1.380(3) . ? C8 C9 1.386(3) . ? C9 C10 1.391(2) . ? C11 C12 1.386(2) . ? C11 C16 1.393(2) . ? C12 C13 1.397(3) . ? C13 C14 1.379(3) . ? C14 C15 1.377(3) . ? C15 C16 1.386(2) . ? C17 C22 1.387(2) . ? C17 C18 1.393(2) . ? C18 C19 1.394(2) . ? C19 C20 1.379(3) . ? C20 C21 1.378(3) . ? C21 C22 1.389(2) . ? C23 C28 1.397(2) . ? C23 C24 1.403(2) . ? C24 C25 1.389(2) . ? C25 C26 1.384(2) . ? C26 C27 1.377(2) . ? C27 C28 1.393(2) . ? C29 C30 1.205(2) . ? C30 C31 1.441(2) . ? C31 C36 1.394(3) . ? C31 C32 1.396(3) . ? C32 C33 1.396(3) . ? C33 C34 1.386(3) . ? C34 C35 1.373(3) . ? C35 C36 1.384(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 C29 Si1 C4 112.51(7) . . ? C29 Si1 C1 115.11(7) . . ? C4 Si1 C1 95.35(7) . . ? C29 Si1 Cl1 107.82(6) . . ? C4 Si1 Cl1 113.91(5) . . ? C1 Si1 Cl1 111.96(5) . . ? C2 C1 C5 128.45(14) . . ? C2 C1 Si1 105.19(11) . . ? C5 C1 Si1 126.30(11) . . ? C1 C2 C11 125.76(14) . . ? C1 C2 C3 116.80(13) . . ? C11 C2 C3 117.33(12) . . ? C4 C3 C17 124.32(13) . . ? C4 C3 C2 116.95(13) . . ? C17 C3 C2 118.72(12) . . ? C3 C4 C23 127.61(13) . . ? C3 C4 Si1 105.34(11) . . ? C23 C4 Si1 126.60(11) . . ? C10 C5 C6 117.62(15) . . ? C10 C5 C1 123.70(14) . . ? C6 C5 C1 118.68(14) . . ? C7 C6 C5 121.3(2) . . ? C8 C7 C6 120.2(2) . . ? C7 C8 C9 119.5(2) . . ? C8 C9 C10 120.5(2) . . ? C9 C10 C5 120.8(2) . . ? C12 C11 C16 119.24(15) . . ? C12 C11 C2 122.29(14) . . ? C16 C11 C2 118.44(14) . . ? C11 C12 C13 119.6(2) . . ? C14 C13 C12 120.5(2) . . ? C15 C14 C13 120.1(2) . . ? C14 C15 C16 119.8(2) . . ? C15 C16 C11 120.7(2) . . ? C22 C17 C18 118.94(14) . . ? C22 C17 C3 120.95(14) . . ? C18 C17 C3 120.08(13) . . ? C17 C18 C19 120.5(2) . . ? C20 C19 C18 119.8(2) . . ? C21 C20 C19 120.0(2) . . ? C20 C21 C22 120.5(2) . . ? C17 C22 C21 120.2(2) . . ? C28 C23 C24 117.89(14) . . ? C28 C23 C4 119.72(13) . . ? C24 C23 C4 122.38(14) . . ? C25 C24 C23 120.5(2) . . ? C26 C25 C24 120.7(2) . . ? C27 C26 C25 119.5(2) . . ? C26 C27 C28 120.3(2) . . ? C27 C28 C23 121.05(14) . . ? C30 C29 Si1 174.3(2) . . ? C29 C30 C31 177.5(2) . . ? C36 C31 C32 119.6(2) . . ? C36 C31 C30 119.2(2) . . ? C32 C31 C30 121.2(2) . . ? C31 C32 C33 119.0(2) . . ? C34 C33 C32 120.6(2) . . ? C35 C34 C33 120.1(2) . . ? C34 C35 C36 120.0(2) . . ? C35 C36 C31 120.6(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 C29 Si1 C1 C2 115.53(11) . . . . ? C4 Si1 C1 C2 -2.41(11) . . . . ? Cl1 Si1 C1 C2 -120.88(9) . . . . ? C29 Si1 C1 C5 -67.17(15) . . . . ? C4 Si1 C1 C5 174.90(13) . . . . ? Cl1 Si1 C1 C5 56.43(14) . . . . ? C5 C1 C2 C11 -2.1(3) . . . . ? Si1 C1 C2 C11 175.14(12) . . . . ? C5 C1 C2 C3 -178.05(14) . . . . ? Si1 C1 C2 C3 -0.8(2) . . . . ? C1 C2 C3 C4 5.3(2) . . . . ? C11 C2 C3 C4 -170.99(13) . . . . ? C1 C2 C3 C17 -173.51(13) . . . . ? C11 C2 C3 C17 10.2(2) . . . . ? C17 C3 C4 C23 -0.4(2) . . . . ? C2 C3 C4 C23 -179.13(14) . . . . ? C17 C3 C4 Si1 172.24(12) . . . . ? C2 C3 C4 Si1 -6.5(2) . . . . ? C29 Si1 C4 C3 -114.88(11) . . . . ? C1 Si1 C4 C3 5.12(11) . . . . ? Cl1 Si1 C4 C3 122.02(9) . . . . ? C29 Si1 C4 C23 57.8(2) . . . . ? C1 Si1 C4 C23 177.83(13) . . . . ? Cl1 Si1 C4 C23 -65.27(14) . . . . ? C2 C1 C5 C10 23.3(2) . . . . ? Si1 C1 C5 C10 -153.38(13) . . . . ? C2 C1 C5 C6 -156.7(2) . . . . ? Si1 C1 C5 C6 26.7(2) . . . . ? C10 C5 C6 C7 -2.7(2) . . . . ? C1 C5 C6 C7 177.31(15) . . . . ? C5 C6 C7 C8 0.4(3) . . . . ? C6 C7 C8 C9 1.7(3) . . . . ? C7 C8 C9 C10 -1.3(3) . . . . ? C8 C9 C10 C5 -1.0(3) . . . . ? C6 C5 C10 C9 3.0(2) . . . . ? C1 C5 C10 C9 -177.00(15) . . . . ? C1 C2 C11 C12 70.4(2) . . . . ? C3 C2 C11 C12 -113.7(2) . . . . ? C1 C2 C11 C16 -107.9(2) . . . . ? C3 C2 C11 C16 68.1(2) . . . . ? C16 C11 C12 C13 0.8(2) . . . . ? C2 C11 C12 C13 -177.4(2) . . . . ? C11 C12 C13 C14 0.5(3) . . . . ? C12 C13 C14 C15 -1.1(3) . . . . ? C13 C14 C15 C16 0.3(3) . . . . ? C14 C15 C16 C11 1.0(3) . . . . ? C12 C11 C16 C15 -1.6(2) . . . . ? C2 C11 C16 C15 176.69(15) . . . . ? C4 C3 C17 C22 65.7(2) . . . . ? C2 C3 C17 C22 -115.6(2) . . . . ? C4 C3 C17 C18 -112.5(2) . . . . ? C2 C3 C17 C18 66.2(2) . . . . ? C22 C17 C18 C19 -2.6(2) . . . . ? C3 C17 C18 C19 175.60(15) . . . . ? C17 C18 C19 C20 2.2(3) . . . . ? C18 C19 C20 C21 0.0(3) . . . . ? C19 C20 C21 C22 -1.7(3) . . . . ? C18 C17 C22 C21 1.0(2) . . . . ? C3 C17 C22 C21 -177.25(15) . . . . ? C20 C21 C22 C17 1.2(3) . . . . ? C3 C4 C23 C28 -140.2(2) . . . . ? Si1 C4 C23 C28 48.7(2) . . . . ? C3 C4 C23 C24 41.2(2) . . . . ? Si1 C4 C23 C24 -129.93(14) . . . . ? C28 C23 C24 C25 0.7(2) . . . . ? C4 C23 C24 C25 179.33(15) . . . . ? C23 C24 C25 C26 -0.1(3) . . . . ? C24 C25 C26 C27 -0.4(3) . . . . ? C25 C26 C27 C28 0.2(3) . . . . ? C26 C27 C28 C23 0.5(2) . . . . ? C24 C23 C28 C27 -0.9(2) . . . . ? C4 C23 C28 C27 -179.56(14) . . . . ? C4 Si1 C29 C30 76.5(15) . . . . ? C1 Si1 C29 C30 -31.3(15) . . . . ? Cl1 Si1 C29 C30 -157.0(15) . . . . ? Si1 C29 C30 C31 25.1(51) . . . . ? C29 C30 C31 C36 -29.5(40) . . . . ? C29 C30 C31 C32 149.3(39) . . . . ? C36 C31 C32 C33 0.5(3) . . . . ? C30 C31 C32 C33 -178.3(2) . . . . ? C31 C32 C33 C34 -1.8(3) . . . . ? C32 C33 C34 C35 1.5(4) . . . . ? C33 C34 C35 C36 0.2(4) . . . . ? C34 C35 C36 C31 -1.6(3) . . . . ? C32 C31 C36 C35 1.2(3) . . . . ? C30 C31 C36 C35 -179.9(2) . . . . ? _refine_diff_density_max 0.347 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.049 #===END