Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Prof Seth Marder' _publ_contact_author_address ; School of Chemistry and Biochemistry Georgia Institute of Technology 770 State Street Atlanta GA 30332-0400 UNITED STATES OF AMERICA ; _publ_contact_author_email SETH.MARDER@CHEMISTRY.GATECH.EDU _publ_section_title ; Comparative studies of the geometric and electronic properties of 1,1-disubstituted-2,3,4,5-tetraphenylsiloles and 1,1,2,2-tetramethyl-3,4,5,6-tetraphenyl-1,2-disila-3,5-cyclohexadiene ; loop_ _publ_author_name 'Seth Marder' 'Mikhail Yu Antipin' 'Stephen Barlow' 'Jean-Luc Bredas' 'Alexander Korlyukov' 'Chad Risko' ; F.Sena ; 'Tatiana V. Timofeeva' 'Xiaowei Zhan' # Attachment 'zhan_jmc_CIFs.cif' # This file contains 3 structures. # # data_COMPOUND_II_CHLOROFORM_SOLVATE _database_code_depnum_ccdc_archive 'CCDC 604519' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H52 Si2, CHCl3' _chemical_formula_sum 'C63 H53 Cl3 Si2' _chemical_formula_weight 972.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.356(4) _cell_length_b 13.044(5) _cell_length_c 19.594(7) _cell_angle_alpha 97.790(8) _cell_angle_beta 104.678(8) _cell_angle_gamma 99.573(9) _cell_volume 2480.6(15) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 708 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 22.68 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 0.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9220 _exptl_absorpt_correction_T_max 0.9945 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Smart 1000 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 18367 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.2249 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 30.08 _reflns_number_total 13000 _reflns_number_gt 3945 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998b)' _computing_cell_refinement 'SAINTPlus (Bruker, 1998a)' _computing_data_reduction 'SAINTPlus (Bruker, 1998a)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0231P)^2^+1.66P] 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 13000 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2242 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1509 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _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 0.54212(12) 0.76740(9) 0.08474(6) 0.0349(3) Uani 1 1 d . . . Si1' Si 0.25957(12) 0.93375(9) 0.48572(7) 0.0397(3) Uani 1 1 d . . . Cl3S Cl 0.67189(13) 0.67943(10) 0.40040(8) 0.0761(4) Uani 1 1 d . . . Cl2S Cl 0.93470(15) 0.76515(12) 0.39355(10) 0.0975(6) Uani 1 1 d . . . Cl1S Cl 0.89766(18) 0.59951(12) 0.47170(10) 0.1156(7) Uani 1 1 d . . . C4 C 0.4189(4) 0.6884(3) -0.0498(2) 0.0308(9) Uani 1 1 d . . . C3 C 0.5233(4) 0.7833(3) -0.0476(2) 0.0305(9) Uani 1 1 d . . . C5' C 0.2050(4) 0.9455(3) 0.3906(2) 0.0339(10) Uani 1 1 d . . . C52 C 0.3140(4) 0.4747(3) -0.0053(2) 0.0322(10) Uani 1 1 d . . . H52A H 0.3666 0.4623 -0.0377 0.039 Uiso 1 1 calc R . . C3' C 0.2615(4) 0.7749(3) 0.3910(2) 0.0335(10) Uani 1 1 d . . . C21 C 0.7016(4) 0.9337(3) 0.0326(2) 0.0317(10) Uani 1 1 d . . . C41 C 0.3328(4) 0.6241(3) -0.1191(2) 0.0306(9) Uani 1 1 d . . . C26 C 0.6785(4) 1.0182(3) -0.0014(2) 0.0347(10) Uani 1 1 d . . . H26A H 0.5949 1.0116 -0.0374 0.042 Uiso 1 1 calc R . . C5 C 0.4097(4) 0.6683(3) 0.0144(2) 0.0297(9) Uani 1 1 d . . . C2 C 0.5998(4) 0.8360(3) 0.0175(2) 0.0310(9) Uani 1 1 d . . . C41' C 0.1656(4) 0.8324(3) 0.2712(2) 0.0320(10) Uani 1 1 d . . . C22' C 0.2750(4) 0.7204(3) 0.5693(2) 0.0411(11) Uani 1 1 d . . . H22A H 0.2022 0.7546 0.5728 0.049 Uiso 1 1 calc R . . C31' C 0.2787(4) 0.6771(3) 0.3512(2) 0.0372(10) Uani 1 1 d . . . C53 C 0.2326(4) 0.3912(3) 0.0079(2) 0.0375(10) Uani 1 1 d . . . H53A H 0.2291 0.3213 -0.0150 0.045 Uiso 1 1 calc R . . C4' C 0.2104(4) 0.8558(3) 0.3504(2) 0.0337(10) Uani 1 1 d . . . C42' C 0.0687(4) 0.7438(3) 0.2324(2) 0.0364(10) Uani 1 1 d . . . H42A H 0.0327 0.6941 0.2576 0.044 Uiso 1 1 calc R . . C42 C 0.3885(4) 0.5764(3) -0.1689(2) 0.0372(10) Uani 1 1 d . . . H42B H 0.4848 0.5849 -0.1585 0.045 Uiso 1 1 calc R . . C51' C 0.1441(4) 1.0308(3) 0.3628(2) 0.0348(10) Uani 1 1 d . . . C43' C 0.0233(4) 0.7251(3) 0.1598(2) 0.0389(11) Uani 1 1 d . . . H43A H -0.0449 0.6642 0.1349 0.047 Uiso 1 1 calc R . . C51 C 0.3221(4) 0.5768(3) 0.0272(2) 0.0322(10) Uani 1 1 d . . . C31 C 0.5341(4) 0.8113(3) -0.1169(2) 0.0332(10) Uani 1 1 d . . . C22 C 0.8236(4) 0.9471(3) 0.0853(2) 0.0406(11) Uani 1 1 d . . . H22B H 0.8408 0.8915 0.1107 0.049 Uiso 1 1 calc R . . C25 C 0.7739(4) 1.1107(3) 0.0157(2) 0.0371(10) Uani 1 1 d . . . H25A H 0.7561 1.1678 -0.0081 0.045 Uiso 1 1 calc R . . C35 C 0.4353(5) 0.8551(3) -0.2297(2) 0.0443(12) Uani 1 1 d . . . H35A H 0.3600 0.8723 -0.2618 0.053 Uiso 1 1 calc R . . C32 C 0.6516(4) 0.8097(3) -0.1367(2) 0.0412(11) Uani 1 1 d . . . H32A H 0.7283 0.7953 -0.1040 0.049 Uiso 1 1 calc R . . C46' C 0.2175(4) 0.9019(3) 0.2320(2) 0.0364(10) Uani 1 1 d . . . H46A H 0.2852 0.9634 0.2565 0.044 Uiso 1 1 calc R . . C54 C 0.1554(4) 0.4079(3) 0.0542(2) 0.0420(11) Uani 1 1 d . . . H54A H 0.0987 0.3496 0.0636 0.050 Uiso 1 1 calc R . . C46 C 0.1938(4) 0.6100(3) -0.1360(2) 0.0411(11) Uani 1 1 d . . . H46B H 0.1530 0.6419 -0.1027 0.049 Uiso 1 1 calc R . . C23 C 0.9206(4) 1.0391(3) 0.1015(2) 0.0467(12) Uani 1 1 d . . . H23A H 1.0054 1.0458 0.1365 0.056 Uiso 1 1 calc R . . C56 C 0.2441(4) 0.5905(3) 0.0736(2) 0.0415(11) Uani 1 1 d . . . H56A H 0.2490 0.6600 0.0976 0.050 Uiso 1 1 calc R . . C2' C 0.2844(4) 0.7983(3) 0.4626(2) 0.0365(10) Uani 1 1 d . . . C45' C 0.1726(4) 0.8828(3) 0.1588(2) 0.0415(11) Uani 1 1 d . . . H45A H 0.2087 0.9315 0.1330 0.050 Uiso 1 1 calc R . . C8 C 0.6625(4) 0.7246(3) 0.1576(2) 0.0392(11) Uani 1 1 d . . . H8A H 0.6286 0.6535 0.1665 0.047 Uiso 1 1 calc R . . H8B H 0.7565 0.7320 0.1530 0.047 Uiso 1 1 calc R . . C43 C 0.3071(5) 0.5172(3) -0.2329(2) 0.0440(12) Uani 1 1 d . . . H43B H 0.3472 0.4844 -0.2662 0.053 Uiso 1 1 calc R . . C21' C 0.3347(4) 0.7329(3) 0.5146(2) 0.0412(11) Uani 1 1 d . . . C25' C 0.4862(4) 0.6230(3) 0.5615(3) 0.0510(13) Uani 1 1 d . . . H25B H 0.5602 0.5898 0.5589 0.061 Uiso 1 1 calc R . . C55 C 0.1601(4) 0.5078(3) 0.0865(2) 0.0488(12) Uani 1 1 d . . . H55A H 0.1054 0.5200 0.1178 0.059 Uiso 1 1 calc R . . C52' C 0.0184(4) 1.0135(3) 0.3123(2) 0.0409(11) Uani 1 1 d . . . H52B H -0.0299 0.9429 0.2922 0.049 Uiso 1 1 calc R . . C6 C 0.5154(4) 0.8444(3) 0.1650(2) 0.0406(11) Uani 1 1 d . . . H6A H 0.5240 0.9210 0.1645 0.049 Uiso 1 1 calc R . . H6B H 0.4307 0.8146 0.1763 0.049 Uiso 1 1 calc R . . C8' C 0.1644(4) 0.9687(3) 0.5497(2) 0.0470(12) Uani 1 1 d . . . H8'A H 0.1122 1.0241 0.5380 0.056 Uiso 1 1 calc R . . H8'B H 0.1067 0.9071 0.5595 0.056 Uiso 1 1 calc R . . C6' C 0.3966(4) 1.0251(3) 0.5584(2) 0.0466(12) Uani 1 1 d . . . H6'A H 0.4811 0.9979 0.5735 0.056 Uiso 1 1 calc R . . H6'B H 0.4170 1.0981 0.5494 0.056 Uiso 1 1 calc R . . C34 C 0.5524(5) 0.8514(3) -0.2496(2) 0.0510(13) Uani 1 1 d . . . H34A H 0.5576 0.8644 -0.2955 0.061 Uiso 1 1 calc R . . C36 C 0.4253(4) 0.8345(3) -0.1650(2) 0.0420(11) Uani 1 1 d . . . H36A H 0.3426 0.8362 -0.1527 0.050 Uiso 1 1 calc R . . C44 C 0.1693(5) 0.5049(3) -0.2493(2) 0.0454(12) Uani 1 1 d . . . H44A H 0.1133 0.4650 -0.2944 0.054 Uiso 1 1 calc R . . C26' C 0.4411(4) 0.6840(3) 0.5118(2) 0.0449(11) Uani 1 1 d . . . H26B H 0.4845 0.6923 0.4751 0.054 Uiso 1 1 calc R . . C44' C 0.0766(4) 0.7951(3) 0.1222(2) 0.0418(11) Uani 1 1 d . . . H44B H 0.0466 0.7821 0.0713 0.050 Uiso 1 1 calc R . . C54' C 0.0302(6) 1.1968(4) 0.3197(3) 0.0608(14) Uani 1 1 d . . . H54B H -0.0101 1.2538 0.3057 0.073 Uiso 1 1 calc R . . C24' C 0.4241(5) 0.6106(3) 0.6144(3) 0.0529(13) Uani 1 1 d . . . H24A H 0.4543 0.5678 0.6483 0.063 Uiso 1 1 calc R . . C56' C 0.2089(5) 1.1349(3) 0.3906(2) 0.0508(13) Uani 1 1 d . . . H56B H 0.2942 1.1498 0.4265 0.061 Uiso 1 1 calc R . . C33 C 0.6616(5) 0.8286(3) -0.2027(2) 0.0489(12) Uani 1 1 d . . . H33A H 0.7435 0.8259 -0.2156 0.059 Uiso 1 1 calc R . . C53' C -0.0376(5) 1.0951(4) 0.2907(2) 0.0498(12) Uani 1 1 d . . . H53B H -0.1237 1.0812 0.2556 0.060 Uiso 1 1 calc R . . C24 C 0.8947(4) 1.1208(3) 0.0671(2) 0.0470(12) Uani 1 1 d . . . H24B H 0.9609 1.1851 0.0789 0.056 Uiso 1 1 calc R . . C36' C 0.3584(4) 0.6815(4) 0.3038(2) 0.0492(12) Uani 1 1 d . . . H36B H 0.4023 0.7483 0.2978 0.059 Uiso 1 1 calc R . . C7 C 0.6427(5) 0.8158(4) 0.2093(2) 0.0638(14) Uani 1 1 d . . . H7A H 0.7218 0.8761 0.2227 0.077 Uiso 1 1 calc R . . H7B H 0.6282 0.7926 0.2533 0.077 Uiso 1 1 calc R . . C45 C 0.1116(5) 0.5499(3) -0.2009(2) 0.0473(12) Uani 1 1 d . . . H45B H 0.0151 0.5401 -0.2117 0.057 Uiso 1 1 calc R . . C32' C 0.2168(4) 0.5793(3) 0.3585(2) 0.0519(13) Uani 1 1 d . . . H32B H 0.1619 0.5742 0.3906 0.062 Uiso 1 1 calc R . . C7' C 0.3020(5) 1.0100(4) 0.6069(2) 0.0618(14) Uani 1 1 d . . . H7'A H 0.3251 0.9576 0.6376 0.074 Uiso 1 1 calc R . . H7'B H 0.3039 1.0776 0.6373 0.074 Uiso 1 1 calc R . . C33' C 0.2335(5) 0.4882(4) 0.3196(3) 0.0630(16) Uani 1 1 d . . . H33B H 0.1908 0.4209 0.3254 0.076 Uiso 1 1 calc R . . C23' C 0.3190(5) 0.6593(3) 0.6187(2) 0.0534(13) Uani 1 1 d . . . H23B H 0.2764 0.6510 0.6558 0.064 Uiso 1 1 calc R . . C34' C 0.3103(6) 0.4945(5) 0.2733(3) 0.0757(18) Uani 1 1 d . . . H34B H 0.3193 0.4314 0.2461 0.091 Uiso 1 1 calc R . . C55' C 0.1549(6) 1.2171(4) 0.3684(3) 0.0665(15) Uani 1 1 d . . . H55B H 0.2040 1.2879 0.3868 0.080 Uiso 1 1 calc R . . C35' C 0.3748(5) 0.5897(5) 0.2651(3) 0.0653(15) Uani 1 1 d . . . H35B H 0.4304 0.5934 0.2332 0.078 Uiso 1 1 calc R . . C1S C 0.8444(5) 0.7102(4) 0.4477(3) 0.0638(14) Uani 1 1 d . . . H1SA H 0.8586 0.7635 0.4921 0.077 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 0.0360(7) 0.0353(7) 0.0352(7) 0.0093(6) 0.0132(6) 0.0055(5) Si1' 0.0377(7) 0.0448(7) 0.0379(8) 0.0104(6) 0.0135(6) 0.0053(6) Cl3S 0.0478(8) 0.0765(10) 0.1023(12) 0.0071(8) 0.0297(8) 0.0024(7) Cl2S 0.0705(10) 0.0862(11) 0.1407(15) 0.0041(10) 0.0600(11) -0.0031(8) Cl1S 0.1094(14) 0.0815(11) 0.1256(15) 0.0163(10) -0.0189(12) 0.0201(10) C4 0.030(2) 0.028(2) 0.038(3) 0.0069(19) 0.015(2) 0.0063(18) C3 0.026(2) 0.034(2) 0.036(3) 0.011(2) 0.013(2) 0.0107(18) C5' 0.031(2) 0.035(2) 0.038(3) 0.012(2) 0.012(2) 0.0044(19) C52 0.031(2) 0.035(2) 0.031(2) 0.0098(19) 0.009(2) 0.0058(19) C3' 0.027(2) 0.032(2) 0.040(3) 0.007(2) 0.010(2) -0.0013(18) C21 0.031(3) 0.035(2) 0.032(2) 0.0097(19) 0.012(2) 0.0062(19) C41 0.028(2) 0.036(2) 0.030(2) 0.0124(19) 0.010(2) 0.0049(18) C26 0.032(2) 0.036(2) 0.037(3) 0.007(2) 0.010(2) 0.010(2) C5 0.030(2) 0.025(2) 0.039(3) 0.0085(19) 0.015(2) 0.0094(18) C2 0.027(2) 0.033(2) 0.035(3) 0.010(2) 0.011(2) 0.0078(18) C41' 0.028(2) 0.039(2) 0.034(3) 0.010(2) 0.014(2) 0.0106(19) C22' 0.041(3) 0.044(3) 0.037(3) 0.015(2) 0.010(2) 0.003(2) C31' 0.033(3) 0.040(3) 0.035(3) 0.011(2) -0.001(2) 0.009(2) C53 0.033(2) 0.032(2) 0.047(3) 0.011(2) 0.010(2) 0.0054(19) C4' 0.025(2) 0.034(2) 0.035(3) 0.009(2) 0.002(2) -0.0058(18) C42' 0.032(3) 0.038(2) 0.040(3) 0.010(2) 0.014(2) 0.004(2) C42 0.037(3) 0.038(2) 0.042(3) 0.018(2) 0.017(2) 0.007(2) C51' 0.035(3) 0.040(3) 0.031(3) 0.007(2) 0.015(2) 0.004(2) C43' 0.027(2) 0.042(3) 0.039(3) 0.000(2) 0.003(2) -0.0003(19) C51 0.030(2) 0.039(2) 0.029(2) 0.0057(19) 0.011(2) 0.0054(19) C31 0.034(3) 0.029(2) 0.033(3) 0.0046(19) 0.008(2) -0.0017(18) C22 0.034(3) 0.036(2) 0.048(3) 0.015(2) 0.005(2) 0.003(2) C25 0.040(3) 0.034(2) 0.040(3) 0.008(2) 0.016(2) 0.005(2) C35 0.049(3) 0.044(3) 0.037(3) 0.016(2) 0.008(2) 0.002(2) C32 0.038(3) 0.046(3) 0.037(3) 0.006(2) 0.011(2) 0.000(2) C46' 0.030(2) 0.047(3) 0.035(3) 0.009(2) 0.012(2) 0.011(2) C54 0.044(3) 0.039(3) 0.048(3) 0.011(2) 0.023(2) 0.003(2) C46 0.040(3) 0.041(3) 0.041(3) 0.007(2) 0.010(2) 0.005(2) C23 0.032(3) 0.046(3) 0.053(3) 0.011(2) 0.002(2) 0.000(2) C56 0.049(3) 0.034(2) 0.045(3) 0.014(2) 0.020(2) 0.004(2) C2' 0.031(3) 0.041(2) 0.038(3) 0.014(2) 0.012(2) 0.0012(19) C45' 0.037(3) 0.051(3) 0.040(3) 0.010(2) 0.017(2) 0.009(2) C8 0.036(3) 0.038(2) 0.042(3) 0.010(2) 0.008(2) 0.005(2) C43 0.057(3) 0.039(3) 0.037(3) 0.004(2) 0.022(3) 0.003(2) C21' 0.042(3) 0.035(2) 0.040(3) 0.005(2) 0.005(2) -0.001(2) C25' 0.037(3) 0.051(3) 0.058(3) 0.015(3) -0.002(3) 0.009(2) C55 0.048(3) 0.055(3) 0.052(3) 0.012(2) 0.033(3) 0.003(2) C52' 0.040(3) 0.042(3) 0.042(3) 0.013(2) 0.014(2) 0.002(2) C6 0.037(3) 0.040(3) 0.050(3) 0.012(2) 0.020(2) 0.006(2) C8' 0.045(3) 0.053(3) 0.048(3) 0.019(2) 0.016(2) 0.015(2) C6' 0.054(3) 0.043(3) 0.044(3) 0.010(2) 0.013(2) 0.012(2) C34 0.059(3) 0.051(3) 0.034(3) 0.010(2) 0.012(3) -0.013(2) C36 0.040(3) 0.041(3) 0.045(3) 0.008(2) 0.016(2) 0.003(2) C44 0.051(3) 0.045(3) 0.031(3) 0.011(2) 0.005(2) -0.007(2) C26' 0.038(3) 0.053(3) 0.039(3) 0.012(2) 0.004(2) 0.005(2) C44' 0.035(3) 0.061(3) 0.033(3) 0.010(2) 0.012(2) 0.018(2) C54' 0.076(4) 0.045(3) 0.068(4) 0.022(3) 0.024(3) 0.018(3) C24' 0.051(3) 0.052(3) 0.048(3) 0.020(2) 0.001(3) -0.001(2) C56' 0.051(3) 0.044(3) 0.048(3) 0.015(2) 0.000(2) 0.001(2) C33 0.046(3) 0.049(3) 0.049(3) 0.003(2) 0.022(3) -0.005(2) C53' 0.045(3) 0.060(3) 0.055(3) 0.026(3) 0.018(3) 0.022(3) C24 0.040(3) 0.039(3) 0.057(3) 0.011(2) 0.012(3) -0.004(2) C36' 0.044(3) 0.054(3) 0.042(3) 0.002(2) -0.002(2) 0.020(2) C7 0.056(4) 0.082(4) 0.049(3) 0.002(3) 0.013(3) 0.014(3) C45 0.041(3) 0.053(3) 0.043(3) 0.018(2) 0.007(3) 0.000(2) C32' 0.050(3) 0.045(3) 0.053(3) 0.014(3) -0.001(3) 0.009(2) C7' 0.084(4) 0.061(3) 0.042(3) 0.003(3) 0.026(3) 0.013(3) C33' 0.060(4) 0.039(3) 0.065(4) 0.012(3) -0.024(3) 0.005(3) C23' 0.055(3) 0.055(3) 0.050(3) 0.017(3) 0.015(3) 0.002(3) C34' 0.081(5) 0.067(4) 0.065(4) 0.000(3) -0.013(3) 0.036(4) C55' 0.074(4) 0.041(3) 0.072(4) 0.020(3) 0.001(3) 0.004(3) C35' 0.056(4) 0.085(4) 0.052(3) 0.004(3) 0.000(3) 0.037(3) C1S 0.050(3) 0.057(3) 0.079(4) 0.014(3) 0.015(3) 0.002(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 Si1 C5 1.849(4) . ? Si1 C2 1.854(4) . ? Si1 C6 1.855(4) . ? Si1 C8 1.858(4) . ? Si1 C7 2.348(5) . ? Si1' C2' 1.840(4) . ? Si1' C5' 1.841(4) . ? Si1' C6' 1.848(4) . ? Si1' C8' 1.836(4) . ? Si1' C7' 2.346(5) . ? Cl3S C1S 1.742(5) . ? Cl2S C1S 1.732(5) . ? Cl1S C1S 1.710(5) . ? C4 C5 1.344(5) . ? C4 C41 1.474(5) . ? C4 C3 1.489(5) . ? C3 C2 1.340(5) . ? C3 C31 1.479(5) . ? C5' C4' 1.338(5) . ? C5' C51' 1.470(5) . ? C52 C53 1.358(5) . ? C52 C51 1.376(5) . ? C52 H52A 0.9500 . ? C3' C2' 1.346(5) . ? C3' C31' 1.464(5) . ? C3' C4' 1.492(5) . ? C21 C22 1.382(5) . ? C21 C26 1.387(5) . ? C21 C2 1.454(5) . ? C41 C46 1.368(5) . ? C41 C42 1.382(5) . ? C26 C25 1.368(5) . ? C26 H26A 0.9500 . ? C5 C51 1.464(5) . ? C41' C42' 1.382(5) . ? C41' C46' 1.392(5) . ? C41' C4' 1.474(5) . ? C22' C21' 1.382(5) . ? C22' C23' 1.373(5) . ? C22' H22A 0.9500 . ? C31' C36' 1.391(6) . ? C31' C32' 1.372(5) . ? C53 C54 1.372(5) . ? C53 H53A 0.9500 . ? C42' C43' 1.355(5) . ? C42' H42A 0.9500 . ? C42 C43 1.365(5) . ? C42 H42B 0.9500 . ? C51' C52' 1.382(5) . ? C51' C56' 1.379(5) . ? C43' C44' 1.378(5) . ? C43' H43A 0.9500 . ? C51 C56 1.375(5) . ? C31 C36 1.379(5) . ? C31 C32 1.371(5) . ? C22 C23 1.372(5) . ? C22 H22B 0.9500 . ? C25 C24 1.366(5) . ? C25 H25A 0.9500 . ? C35 C36 1.357(5) . ? C35 C34 1.370(6) . ? C35 H35A 0.9500 . ? C32 C33 1.374(5) . ? C32 H32A 0.9500 . ? C46' C45' 1.364(5) . ? C46' H46A 0.9500 . ? C54 C55 1.357(5) . ? C54 H54A 0.9500 . ? C46 C45 1.384(5) . ? C46 H46B 0.9500 . ? C23 C24 1.364(5) . ? C23 H23A 0.9500 . ? C56 C55 1.362(5) . ? C56 H56A 0.9500 . ? C2' C21' 1.466(5) . ? C45' C44' 1.360(5) . ? C45' H45A 0.9500 . ? C8 C7 1.530(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C43 C44 1.358(5) . ? C43 H43B 0.9500 . ? C21' C26' 1.370(5) . ? C25' C26' 1.379(5) . ? C25' C24' 1.365(6) . ? C25' H25B 0.9500 . ? C55 H55A 0.9500 . ? C52' C53' 1.361(5) . ? C52' H52B 0.9500 . ? C6 C7 1.517(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C8' C7' 1.532(6) . ? C8' H8'A 0.9900 . ? C8' H8'B 0.9900 . ? C6' C7' 1.536(6) . ? C6' H6'A 0.9900 . ? C6' H6'B 0.9900 . ? C34 C33 1.368(6) . ? C34 H34A 0.9500 . ? C36 H36A 0.9500 . ? C44 C45 1.361(6) . ? C44 H44A 0.9500 . ? C26' H26B 0.9500 . ? C44' H44B 0.9500 . ? C54' C55' 1.357(6) . ? C54' C53' 1.364(6) . ? C54' H54B 0.9500 . ? C24' C23' 1.363(6) . ? C24' H24A 0.9500 . ? C56' C55' 1.361(6) . ? C56' H56B 0.9500 . ? C33 H33A 0.9500 . ? C53' H53B 0.9500 . ? C24 H24B 0.9500 . ? C36' C35' 1.387(6) . ? C36' H36B 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C45 H45B 0.9500 . ? C32' C33' 1.384(6) . ? C32' H32B 0.9500 . ? C7' H7'A 0.9900 . ? C7' H7'B 0.9900 . ? C33' C34' 1.350(7) . ? C33' H33B 0.9500 . ? C23' H23B 0.9500 . ? C34' C35' 1.360(7) . ? C34' H34B 0.9500 . ? C55' H55B 0.9500 . ? C35' H35B 0.9500 . ? C1S H1SA 1.0000 . ? 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 C5 Si1 C2 92.37(18) . . ? C5 Si1 C6 125.72(18) . . ? C2 Si1 C6 120.36(18) . . ? C5 Si1 C8 120.38(17) . . ? C2 Si1 C8 122.29(18) . . ? C6 Si1 C8 79.41(18) . . ? C5 Si1 C7 143.28(18) . . ? C2 Si1 C7 124.29(18) . . ? C6 Si1 C7 40.20(15) . . ? C8 Si1 C7 40.61(15) . . ? C2' Si1' C5' 92.11(19) . . ? C2' Si1' C6' 116.83(19) . . ? C5' Si1' C6' 127.10(19) . . ? C2' Si1' C8' 122.21(19) . . ? C5' Si1' C8' 122.97(19) . . ? C6' Si1' C8' 79.27(19) . . ? C2' Si1' C7' 119.23(18) . . ? C5' Si1' C7' 148.66(18) . . ? C6' Si1' C7' 40.84(16) . . ? C8' Si1' C7' 40.73(16) . . ? C5 C4 C41 124.1(3) . . ? C5 C4 C3 115.4(3) . . ? C41 C4 C3 120.5(3) . . ? C2 C3 C31 125.6(4) . . ? C2 C3 C4 116.8(4) . . ? C31 C3 C4 117.6(3) . . ? C4' C5' C51' 125.0(4) . . ? C4' C5' Si1' 108.5(3) . . ? C51' C5' Si1' 125.7(3) . . ? C53 C52 C51 121.6(4) . . ? C53 C52 H52A 119.2 . . ? C51 C52 H52A 119.2 . . ? C2' C3' C31' 125.5(4) . . ? C2' C3' C4' 115.6(4) . . ? C31' C3' C4' 118.9(4) . . ? C22 C21 C26 117.5(4) . . ? C22 C21 C2 120.1(3) . . ? C26 C21 C2 122.3(4) . . ? C46 C41 C42 117.9(4) . . ? C46 C41 C4 120.3(4) . . ? C42 C41 C4 121.8(4) . . ? C25 C26 C21 121.2(4) . . ? C25 C26 H26A 119.4 . . ? C21 C26 H26A 119.4 . . ? C4 C5 C51 126.2(4) . . ? C4 C5 Si1 108.0(3) . . ? C51 C5 Si1 125.4(3) . . ? C3 C2 C21 126.3(4) . . ? C3 C2 Si1 107.3(3) . . ? C21 C2 Si1 126.3(3) . . ? C42' C41' C46' 116.8(4) . . ? C42' C41' C4' 122.6(3) . . ? C46' C41' C4' 120.6(4) . . ? C21' C22' C23' 121.2(4) . . ? C21' C22' H22A 119.4 . . ? C23' C22' H22A 119.4 . . ? C36' C31' C32' 118.1(4) . . ? C36' C31' C3' 120.1(4) . . ? C32' C31' C3' 121.8(4) . . ? C52 C53 C54 119.8(4) . . ? C52 C53 H53A 120.1 . . ? C54 C53 H53A 120.1 . . ? C5' C4' C41' 124.5(4) . . ? C5' C4' C3' 115.4(4) . . ? C41' C4' C3' 120.1(4) . . ? C43' C42' C41' 122.4(4) . . ? C43' C42' H42A 118.8 . . ? C41' C42' H42A 118.8 . . ? C43 C42 C41 121.0(4) . . ? C43 C42 H42B 119.5 . . ? C41 C42 H42B 119.5 . . ? C52' C51' C56' 116.6(4) . . ? C52' C51' C5' 123.4(4) . . ? C56' C51' C5' 119.8(4) . . ? C42' C43' C44' 119.6(4) . . ? C42' C43' H43A 120.2 . . ? C44' C43' H43A 120.2 . . ? C56 C51 C52 116.9(4) . . ? C56 C51 C5 120.3(4) . . ? C52 C51 C5 122.8(4) . . ? C36 C31 C32 117.8(4) . . ? C36 C31 C3 121.6(4) . . ? C32 C31 C3 120.5(4) . . ? C21 C22 C23 121.3(4) . . ? C21 C22 H22B 119.3 . . ? C23 C22 H22B 119.3 . . ? C24 C25 C26 119.9(4) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C36 C35 C34 121.1(4) . . ? C36 C35 H35A 119.5 . . ? C34 C35 H35A 119.5 . . ? C33 C32 C31 121.8(4) . . ? C33 C32 H32A 119.1 . . ? C31 C32 H32A 119.1 . . ? C45' C46' C41' 120.9(4) . . ? C45' C46' H46A 119.6 . . ? C41' C46' H46A 119.6 . . ? C55 C54 C53 120.0(4) . . ? C55 C54 H54A 120.0 . . ? C53 C54 H54A 120.0 . . ? C45 C46 C41 120.9(4) . . ? C45 C46 H46B 119.5 . . ? C41 C46 H46B 119.5 . . ? C24 C23 C22 119.7(4) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C55 C56 C51 122.3(4) . . ? C55 C56 H56A 118.8 . . ? C51 C56 H56A 118.8 . . ? C3' C2' C21' 126.4(4) . . ? C3' C2' Si1' 108.1(3) . . ? C21' C2' Si1' 125.2(3) . . ? C46' C45' C44' 120.9(4) . . ? C46' C45' H45A 119.6 . . ? C44' C45' H45A 119.6 . . ? C7 C8 Si1 87.2(3) . . ? C7 C8 H8A 114.1 . . ? Si1 C8 H8A 114.1 . . ? C7 C8 H8B 114.1 . . ? Si1 C8 H8B 114.1 . . ? H8A C8 H8B 111.3 . . ? C42 C43 C44 120.6(4) . . ? C42 C43 H43B 119.7 . . ? C44 C43 H43B 119.7 . . ? C26' C21' C22' 117.9(4) . . ? C26' C21' C2' 122.5(4) . . ? C22' C21' C2' 119.6(4) . . ? C26' C25' C24' 119.7(4) . . ? C26' C25' H25B 120.1 . . ? C24' C25' H25B 120.1 . . ? C54 C55 C56 119.3(4) . . ? C54 C55 H55A 120.3 . . ? C56 C55 H55A 120.3 . . ? C53' C52' C51' 121.6(4) . . ? C53' C52' H52B 119.2 . . ? C51' C52' H52B 119.2 . . ? C7 C6 Si1 87.7(3) . . ? C7 C6 H6A 114.0 . . ? Si1 C6 H6A 114.0 . . ? C7 C6 H6B 114.0 . . ? Si1 C6 H6B 114.0 . . ? H6A C6 H6B 111.2 . . ? C7' C8' Si1' 87.8(3) . . ? C7' C8' H8'A 114.0 . . ? Si1' C8' H8'A 114.0 . . ? C7' C8' H8'B 114.0 . . ? Si1' C8' H8'B 114.0 . . ? H8'A C8' H8'B 111.2 . . ? C7' C6' Si1' 87.2(3) . . ? C7' C6' H6'A 114.1 . . ? Si1' C6' H6'A 114.1 . . ? C7' C6' H6'B 114.1 . . ? Si1' C6' H6'B 114.1 . . ? H6'A C6' H6'B 111.3 . . ? C33 C34 C35 119.2(4) . . ? C33 C34 H34A 120.4 . . ? C35 C34 H34A 120.4 . . ? C35 C36 C31 120.7(4) . . ? C35 C36 H36A 119.7 . . ? C31 C36 H36A 119.7 . . ? C45 C44 C43 119.7(4) . . ? C45 C44 H44A 120.1 . . ? C43 C44 H44A 120.1 . . ? C25' C26' C21' 121.2(4) . . ? C25' C26' H26B 119.4 . . ? C21' C26' H26B 119.4 . . ? C45' C44' C43' 119.4(4) . . ? C45' C44' H44B 120.3 . . ? C43' C44' H44B 120.3 . . ? C55' C54' C53' 120.4(4) . . ? C55' C54' H54B 119.8 . . ? C53' C54' H54B 119.8 . . ? C23' C24' C25' 120.2(4) . . ? C23' C24' H24A 119.9 . . ? C25' C24' H24A 119.9 . . ? C55' C56' C51' 122.2(4) . . ? C55' C56' H56B 118.9 . . ? C51' C56' H56B 118.9 . . ? C34 C33 C32 119.4(4) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C52' C53' C54' 119.8(5) . . ? C52' C53' H53B 120.1 . . ? C54' C53' H53B 120.1 . . ? C23 C24 C25 120.3(4) . . ? C23 C24 H24B 119.8 . . ? C25 C24 H24B 119.8 . . ? C31' C36' C35' 121.0(5) . . ? C31' C36' H36B 119.5 . . ? C35' C36' H36B 119.5 . . ? C8 C7 C6 102.2(3) . . ? C8 C7 Si1 52.2(2) . . ? C6 C7 Si1 52.1(2) . . ? C8 C7 H7A 111.3 . . ? C6 C7 H7A 111.3 . . ? Si1 C7 H7A 113.1 . . ? C8 C7 H7B 111.3 . . ? C6 C7 H7B 111.3 . . ? Si1 C7 H7B 137.7 . . ? H7A C7 H7B 109.2 . . ? C44 C45 C46 119.9(4) . . ? C44 C45 H45B 120.0 . . ? C46 C45 H45B 120.0 . . ? C31' C32' C33' 120.6(5) . . ? C31' C32' H32B 119.7 . . ? C33' C32' H32B 119.7 . . ? C8' C7' C6' 100.0(3) . . ? C8' C7' Si1' 51.5(2) . . ? C6' C7' Si1' 51.9(2) . . ? C8' C7' H7'A 111.8 . . ? C6' C7' H7'A 111.8 . . ? Si1' C7' H7'A 110.0 . . ? C8' C7' H7'B 111.8 . . ? C6' C7' H7'B 111.8 . . ? Si1' C7' H7'B 140.5 . . ? H7'A C7' H7'B 109.5 . . ? C34' C33' C32' 120.3(5) . . ? C34' C33' H33B 119.9 . . ? C32' C33' H33B 119.9 . . ? C24' C23' C22' 119.7(5) . . ? C24' C23' H23B 120.1 . . ? C22' C23' H23B 120.1 . . ? C35' C34' C33' 121.0(6) . . ? C35' C34' H34B 119.5 . . ? C33' C34' H34B 119.5 . . ? C54' C55' C56' 119.4(5) . . ? C54' C55' H55B 120.3 . . ? C56' C55' H55B 120.3 . . ? C34' C35' C36' 119.0(6) . . ? C34' C35' H35B 120.5 . . ? C36' C35' H35B 120.5 . . ? Cl1S C1S Cl3S 110.6(3) . . ? Cl1S C1S Cl2S 111.3(3) . . ? Cl3S C1S Cl2S 107.9(3) . . ? Cl1S C1S H1SA 109.0 . . ? Cl3S C1S H1SA 109.0 . . ? Cl2S C1S H1SA 109.0 . . ? 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 C5 C4 C3 C2 2.3(5) . . . . ? C41 C4 C3 C2 -178.3(4) . . . . ? C5 C4 C3 C31 -177.8(3) . . . . ? C41 C4 C3 C31 1.5(5) . . . . ? C2' Si1' C5' C4' -1.1(3) . . . . ? C6' Si1' C5' C4' 125.4(3) . . . . ? C8' Si1' C5' C4' -132.3(3) . . . . ? C7' Si1' C5' C4' 179.8(3) . . . . ? C2' Si1' C5' C51' 169.5(3) . . . . ? C6' Si1' C5' C51' -64.0(4) . . . . ? C8' Si1' C5' C51' 38.3(4) . . . . ? C7' Si1' C5' C51' -9.6(6) . . . . ? C5 C4 C41 C46 58.1(5) . . . . ? C3 C4 C41 C46 -121.2(4) . . . . ? C5 C4 C41 C42 -121.9(4) . . . . ? C3 C4 C41 C42 58.8(5) . . . . ? C22 C21 C26 C25 0.9(6) . . . . ? C2 C21 C26 C25 177.5(4) . . . . ? C41 C4 C5 C51 4.8(6) . . . . ? C3 C4 C5 C51 -175.9(3) . . . . ? C41 C4 C5 Si1 178.0(3) . . . . ? C3 C4 C5 Si1 -2.7(4) . . . . ? C2 Si1 C5 C4 2.0(3) . . . . ? C6 Si1 C5 C4 132.7(3) . . . . ? C8 Si1 C5 C4 -128.1(3) . . . . ? C7 Si1 C5 C4 -174.8(3) . . . . ? C2 Si1 C5 C51 175.3(3) . . . . ? C6 Si1 C5 C51 -54.0(4) . . . . ? C8 Si1 C5 C51 45.2(4) . . . . ? C7 Si1 C5 C51 -1.5(5) . . . . ? C31 C3 C2 C21 4.0(7) . . . . ? C4 C3 C2 C21 -176.1(3) . . . . ? C31 C3 C2 Si1 179.5(3) . . . . ? C4 C3 C2 Si1 -0.6(4) . . . . ? C22 C21 C2 C3 -139.3(4) . . . . ? C26 C21 C2 C3 44.3(6) . . . . ? C22 C21 C2 Si1 46.1(5) . . . . ? C26 C21 C2 Si1 -130.4(4) . . . . ? C5 Si1 C2 C3 -0.7(3) . . . . ? C6 Si1 C2 C3 -135.3(3) . . . . ? C8 Si1 C2 C3 127.9(3) . . . . ? C7 Si1 C2 C3 176.9(3) . . . . ? C5 Si1 C2 C21 174.8(3) . . . . ? C6 Si1 C2 C21 40.2(4) . . . . ? C8 Si1 C2 C21 -56.6(4) . . . . ? C7 Si1 C2 C21 -7.6(4) . . . . ? C2' C3' C31' C36' -127.4(4) . . . . ? C4' C3' C31' C36' 54.7(5) . . . . ? C2' C3' C31' C32' 53.3(6) . . . . ? C4' C3' C31' C32' -124.7(4) . . . . ? C51 C52 C53 C54 0.4(6) . . . . ? C51' C5' C4' C41' 5.0(6) . . . . ? Si1' C5' C4' C41' 175.7(3) . . . . ? C51' C5' C4' C3' -172.7(4) . . . . ? Si1' C5' C4' C3' -2.0(4) . . . . ? C42' C41' C4' C5' -123.8(4) . . . . ? C46' C41' C4' C5' 54.4(6) . . . . ? C42' C41' C4' C3' 53.8(5) . . . . ? C46' C41' C4' C3' -128.0(4) . . . . ? C2' C3' C4' C5' 5.6(5) . . . . ? C31' C3' C4' C5' -176.3(4) . . . . ? C2' C3' C4' C41' -172.3(3) . . . . ? C31' C3' C4' C41' 5.9(5) . . . . ? C46' C41' C42' C43' -1.3(6) . . . . ? C4' C41' C42' C43' 176.9(4) . . . . ? C46 C41 C42 C43 0.1(6) . . . . ? C4 C41 C42 C43 -179.9(4) . . . . ? C4' C5' C51' C52' 45.9(6) . . . . ? Si1' C5' C51' C52' -123.2(4) . . . . ? C4' C5' C51' C56' -138.3(4) . . . . ? Si1' C5' C51' C56' 52.6(5) . . . . ? C41' C42' C43' C44' 1.5(6) . . . . ? C53 C52 C51 C56 0.1(6) . . . . ? C53 C52 C51 C5 179.5(4) . . . . ? C4 C5 C51 C56 -132.9(4) . . . . ? Si1 C5 C51 C56 55.1(5) . . . . ? C4 C5 C51 C52 47.7(6) . . . . ? Si1 C5 C51 C52 -124.3(4) . . . . ? C2 C3 C31 C36 -120.2(4) . . . . ? C4 C3 C31 C36 59.9(5) . . . . ? C2 C3 C31 C32 62.9(6) . . . . ? C4 C3 C31 C32 -116.9(4) . . . . ? C26 C21 C22 C23 -2.3(6) . . . . ? C2 C21 C22 C23 -178.9(4) . . . . ? C21 C26 C25 C24 0.2(6) . . . . ? C36 C31 C32 C33 -1.2(6) . . . . ? C3 C31 C32 C33 175.7(4) . . . . ? C42' C41' C46' C45' 0.8(6) . . . . ? C4' C41' C46' C45' -177.5(4) . . . . ? C52 C53 C54 C55 0.2(6) . . . . ? C42 C41 C46 C45 -0.1(6) . . . . ? C4 C41 C46 C45 179.9(4) . . . . ? C21 C22 C23 C24 2.5(7) . . . . ? C52 C51 C56 C55 -1.2(6) . . . . ? C5 C51 C56 C55 179.3(4) . . . . ? C31' C3' C2' C21' 2.2(7) . . . . ? C4' C3' C2' C21' -179.8(4) . . . . ? C31' C3' C2' Si1' 176.1(3) . . . . ? C4' C3' C2' Si1' -6.0(4) . . . . ? C5' Si1' C2' C3' 4.1(3) . . . . ? C6' Si1' C2' C3' -130.0(3) . . . . ? C8' Si1' C2' C3' 135.9(3) . . . . ? C7' Si1' C2' C3' -176.5(3) . . . . ? C5' Si1' C2' C21' 178.0(4) . . . . ? C6' Si1' C2' C21' 44.0(4) . . . . ? C8' Si1' C2' C21' -50.2(4) . . . . ? C7' Si1' C2' C21' -2.5(4) . . . . ? C41' C46' C45' C44' -0.5(6) . . . . ? C5 Si1 C8 C7 -138.0(3) . . . . ? C2 Si1 C8 C7 106.7(3) . . . . ? C6 Si1 C8 C7 -12.7(3) . . . . ? C41 C42 C43 C44 0.7(6) . . . . ? C23' C22' C21' C26' -1.2(6) . . . . ? C23' C22' C21' C2' 179.7(4) . . . . ? C3' C2' C21' C26' 44.3(6) . . . . ? Si1' C2' C21' C26' -128.5(4) . . . . ? C3' C2' C21' C22' -136.5(4) . . . . ? Si1' C2' C21' C22' 50.6(5) . . . . ? C53 C54 C55 C56 -1.3(6) . . . . ? C51 C56 C55 C54 1.9(7) . . . . ? C56' C51' C52' C53' 0.6(6) . . . . ? C5' C51' C52' C53' 176.5(4) . . . . ? C5 Si1 C6 C7 132.7(3) . . . . ? C2 Si1 C6 C7 -108.6(3) . . . . ? C8 Si1 C6 C7 12.8(3) . . . . ? C2' Si1' C8' C7' 98.8(3) . . . . ? C5' Si1' C8' C7' -143.8(3) . . . . ? C6' Si1' C8' C7' -16.3(3) . . . . ? C2' Si1' C6' C7' -104.6(3) . . . . ? C5' Si1' C6' C7' 139.7(3) . . . . ? C8' Si1' C6' C7' 16.2(3) . . . . ? C36 C35 C34 C33 -1.3(6) . . . . ? C34 C35 C36 C31 1.2(6) . . . . ? C32 C31 C36 C35 0.1(6) . . . . ? C3 C31 C36 C35 -176.9(4) . . . . ? C42 C43 C44 C45 -1.5(6) . . . . ? C24' C25' C26' C21' 0.1(6) . . . . ? C22' C21' C26' C25' 0.8(6) . . . . ? C2' C21' C26' C25' 180.0(4) . . . . ? C46' C45' C44' C43' 0.7(6) . . . . ? C42' C43' C44' C45' -1.1(6) . . . . ? C26' C25' C24' C23' -0.8(7) . . . . ? C52' C51' C56' C55' -1.9(7) . . . . ? C5' C51' C56' C55' -177.9(4) . . . . ? C35 C34 C33 C32 0.1(6) . . . . ? C31 C32 C33 C34 1.1(6) . . . . ? C51' C52' C53' C54' -0.6(7) . . . . ? C55' C54' C53' C52' 1.9(7) . . . . ? C22 C23 C24 C25 -1.2(7) . . . . ? C26 C25 C24 C23 -0.1(6) . . . . ? C32' C31' C36' C35' 0.0(6) . . . . ? C3' C31' C36' C35' -179.4(4) . . . . ? Si1 C8 C7 C6 15.7(3) . . . . ? Si1 C6 C7 C8 -15.7(3) . . . . ? C5 Si1 C7 C8 74.7(4) . . . . ? C2 Si1 C7 C8 -101.4(3) . . . . ? C6 Si1 C7 C8 160.5(4) . . . . ? C5 Si1 C7 C6 -85.8(4) . . . . ? C2 Si1 C7 C6 98.1(3) . . . . ? C8 Si1 C7 C6 -160.5(4) . . . . ? C43 C44 C45 C46 1.5(6) . . . . ? C41 C46 C45 C44 -0.7(6) . . . . ? C36' C31' C32' C33' -0.1(6) . . . . ? C3' C31' C32' C33' 179.3(4) . . . . ? Si1' C8' C7' C6' 19.7(3) . . . . ? Si1' C6' C7' C8' -19.5(3) . . . . ? C2' Si1' C7' C8' -106.6(3) . . . . ? C5' Si1' C7' C8' 72.3(4) . . . . ? C6' Si1' C7' C8' 155.1(4) . . . . ? C2' Si1' C7' C6' 98.3(3) . . . . ? C5' Si1' C7' C6' -82.8(4) . . . . ? C8' Si1' C7' C6' -155.1(4) . . . . ? C31' C32' C33' C34' -0.6(7) . . . . ? C25' C24' C23' C22' 0.5(7) . . . . ? C21' C22' C23' C24' 0.5(7) . . . . ? C32' C33' C34' C35' 1.4(8) . . . . ? C53' C54' C55' C56' -3.1(8) . . . . ? C51' C56' C55' C54' 3.1(8) . . . . ? C33' C34' C35' C36' -1.5(7) . . . . ? C31' C36' C35' C34' 0.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 0.773 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.073 _publ_section_references ; Bruker (1998a). SAINTPlus. Data Reduction and Correction Program v. 6.01, Bruker AXS, Madison, Wisconsin, USA. Bruker (1998b). SMART. Bruker Molecular Analysis Research Tool, v. 5.059. Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998b). SHELXTL v. 5.10, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; data_COMPOUND_III _database_code_depnum_ccdc_archive 'CCDC 604520' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H26 O2 Si' _chemical_formula_sum 'C30 H26 O2 Si' _chemical_formula_weight 446.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 27.005(7) _cell_length_b 16.153(7) _cell_length_c 16.336(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.294(10) _cell_angle_gamma 90.00 _cell_volume 7114(4) _cell_formula_units_Z 12 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 972 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 25.87 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.934 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Smart 1000 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 22456 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.02 _reflns_number_total 7021 _reflns_number_gt 4211 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998b)' _computing_cell_refinement 'SAINTPlus (Bruker, 1998a)' _computing_data_reduction 'SAINTPlus (Bruker, 1998a)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0291P)^2^+10.966P] 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 7021 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.11080(3) 0.76057(6) 0.09373(5) 0.0349(2) Uani 1 1 d . . . O1 O 0.05948(7) 0.70880(15) 0.07687(12) 0.0485(6) Uani 1 1 d . . . O2 O 0.10261(7) 0.85070(14) 0.05177(12) 0.0464(6) Uani 1 1 d . . . C2 C 0.16284(9) 0.69701(18) 0.05886(15) 0.0280(6) Uani 1 1 d . . . C3 C 0.19033(9) 0.67425(17) 0.12692(15) 0.0268(6) Uani 1 1 d . . . C4 C 0.17523(9) 0.71179(17) 0.20760(15) 0.0269(6) Uani 1 1 d . . . C5 C 0.13514(9) 0.76131(18) 0.20359(15) 0.0287(6) Uani 1 1 d . . . C6 C 0.01123(11) 0.7302(3) 0.0968(2) 0.0622(11) Uani 1 1 d . . . H6A H -0.0116 0.6885 0.0765 0.093 Uiso 1 1 calc R . . H6B H 0.0023 0.7825 0.0722 0.093 Uiso 1 1 calc R . . H6C H 0.0100 0.7343 0.1553 0.093 Uiso 1 1 calc R . . C7 C 0.14208(12) 0.9099(2) 0.0498(2) 0.0653(11) Uani 1 1 d . . . H7A H 0.1313 0.9565 0.0168 0.098 Uiso 1 1 calc R . . H7B H 0.1703 0.8847 0.0267 0.098 Uiso 1 1 calc R . . H7C H 0.1511 0.9283 0.1045 0.098 Uiso 1 1 calc R . . C21 C 0.17095(9) 0.67344(17) -0.02686(15) 0.0269(6) Uani 1 1 d . . . C22 C 0.13058(10) 0.66840(18) -0.08387(16) 0.0332(7) Uani 1 1 d . . . H22B H 0.0991 0.6810 -0.0674 0.040 Uiso 1 1 calc R . . C23 C 0.13614(11) 0.64514(19) -0.16415(17) 0.0392(8) Uani 1 1 d . . . H23A H 0.1085 0.6412 -0.2006 0.047 Uiso 1 1 calc R . . C24 C 0.18267(11) 0.62777(19) -0.19026(17) 0.0387(7) Uani 1 1 d . . . H24A H 0.1865 0.6112 -0.2441 0.046 Uiso 1 1 calc R . . C25 C 0.22346(11) 0.63512(19) -0.13622(16) 0.0367(7) Uani 1 1 d . . . H25A H 0.2550 0.6251 -0.1541 0.044 Uiso 1 1 calc R . . C26 C 0.21788(10) 0.65721(18) -0.05566(16) 0.0320(7) Uani 1 1 d . . . H26A H 0.2458 0.6614 -0.0198 0.038 Uiso 1 1 calc R . . C31 C 0.23083(9) 0.61156(18) 0.12936(14) 0.0262(6) Uani 1 1 d . . . C32 C 0.21933(10) 0.53061(18) 0.10855(15) 0.0322(7) Uani 1 1 d . . . H32A H 0.1868 0.5170 0.0919 0.039 Uiso 1 1 calc R . . C33 C 0.25518(11) 0.46972(19) 0.11209(16) 0.0412(8) Uani 1 1 d . . . H33A H 0.2468 0.4155 0.0979 0.049 Uiso 1 1 calc R . . C34 C 0.30348(12) 0.4893(2) 0.13672(18) 0.0465(8) Uani 1 1 d . . . H34B H 0.3277 0.4483 0.1398 0.056 Uiso 1 1 calc R . . C35 C 0.31561(11) 0.5696(2) 0.15662(17) 0.0429(8) Uani 1 1 d . . . H35B H 0.3483 0.5829 0.1725 0.051 Uiso 1 1 calc R . . C36 C 0.27981(9) 0.63113(19) 0.15337(15) 0.0325(7) Uani 1 1 d . . . H36B H 0.2884 0.6853 0.1672 0.039 Uiso 1 1 calc R . . C41 C 0.20731(9) 0.69068(18) 0.28268(15) 0.0262(6) Uani 1 1 d . . . C42 C 0.20931(9) 0.61147(18) 0.31505(16) 0.0303(7) Uani 1 1 d . . . H42A H 0.1897 0.5700 0.2905 0.036 Uiso 1 1 calc R . . C43 C 0.24003(10) 0.5932(2) 0.38336(17) 0.0376(7) Uani 1 1 d . . . H43A H 0.2406 0.5400 0.4052 0.045 Uiso 1 1 calc R . . C44 C 0.26974(11) 0.6539(2) 0.41884(17) 0.0438(8) Uani 1 1 d . . . H44A H 0.2909 0.6417 0.4642 0.053 Uiso 1 1 calc R . . C45 C 0.26816(11) 0.7328(2) 0.38715(18) 0.0442(8) Uani 1 1 d . . . H45A H 0.2882 0.7738 0.4114 0.053 Uiso 1 1 calc R . . C46 C 0.23709(10) 0.75170(19) 0.31966(16) 0.0347(7) Uani 1 1 d . . . H46A H 0.2361 0.8053 0.2990 0.042 Uiso 1 1 calc R . . C51 C 0.11300(9) 0.80755(18) 0.27101(15) 0.0280(6) Uani 1 1 d . . . C52 C 0.11865(9) 0.78459(18) 0.35380(16) 0.0312(7) Uani 1 1 d . . . H52A H 0.1364 0.7371 0.3686 0.037 Uiso 1 1 calc R . . C53 C 0.09797(10) 0.83201(19) 0.41370(16) 0.0340(7) Uani 1 1 d . . . H53A H 0.1022 0.8161 0.4684 0.041 Uiso 1 1 calc R . . C54 C 0.07127(10) 0.90231(19) 0.39335(17) 0.0358(7) Uani 1 1 d . . . H54A H 0.0582 0.9344 0.4342 0.043 Uiso 1 1 calc R . . C55 C 0.06386(10) 0.92504(19) 0.31195(17) 0.0387(7) Uani 1 1 d . . . H55A H 0.0453 0.9718 0.2975 0.046 Uiso 1 1 calc R . . C56 C 0.08443(10) 0.87722(19) 0.25216(17) 0.0367(7) Uani 1 1 d . . . H56A H 0.0789 0.8923 0.1975 0.044 Uiso 1 1 calc R . . Si1' Si 0.0000 0.45202(7) 0.2500 0.0272(3) Uani 1 2 d S . . O1' O -0.04083(6) 0.50916(12) 0.19976(11) 0.0344(5) Uani 1 1 d . . . C2' C 0.02629(9) 0.37332(17) 0.18122(15) 0.0266(6) Uani 1 1 d . . . C3' C 0.01498(9) 0.29836(18) 0.21145(14) 0.0267(6) Uani 1 1 d . . . C4' C -0.07072(12) 0.5706(2) 0.23530(19) 0.0514(9) Uani 1 1 d . . . H4'B H -0.0843 0.6068 0.1931 0.077 Uiso 1 1 calc R . . H4'C H -0.0508 0.6022 0.2746 0.077 Uiso 1 1 calc R . . H4'D H -0.0972 0.5444 0.2622 0.077 Uiso 1 1 calc R . . C21' C 0.05646(9) 0.39325(18) 0.11013(15) 0.0278(6) Uani 1 1 d . . . C22' C 0.04787(10) 0.4679(2) 0.07020(17) 0.0383(7) Uani 1 1 d . . . H22A H 0.0230 0.5026 0.0874 0.046 Uiso 1 1 calc R . . C23' C 0.07537(11) 0.4923(2) 0.00519(18) 0.0457(8) Uani 1 1 d . . . H23B H 0.0682 0.5421 -0.0215 0.055 Uiso 1 1 calc R . . C24' C 0.11317(10) 0.4431(2) -0.01998(17) 0.0373(7) Uani 1 1 d . . . H24B H 0.1317 0.4594 -0.0635 0.045 Uiso 1 1 calc R . . C25' C 0.12328(10) 0.3696(2) 0.02012(16) 0.0348(7) Uani 1 1 d . . . H25B H 0.1491 0.3365 0.0039 0.042 Uiso 1 1 calc R . . C26' C 0.09536(10) 0.34420(19) 0.08463(16) 0.0335(7) Uani 1 1 d . . . H26B H 0.1026 0.2942 0.1109 0.040 Uiso 1 1 calc R . . C31' C 0.02624(9) 0.21625(17) 0.17555(15) 0.0276(6) Uani 1 1 d . . . C32' C 0.06744(10) 0.17021(19) 0.20286(16) 0.0366(7) Uani 1 1 d . . . H32B H 0.0891 0.1913 0.2439 0.044 Uiso 1 1 calc R . . C33' C 0.07653(11) 0.0933(2) 0.16959(17) 0.0399(8) Uani 1 1 d . . . H33B H 0.1046 0.0636 0.1876 0.048 Uiso 1 1 calc R . . C34' C 0.04400(11) 0.06030(19) 0.10973(16) 0.0369(7) Uani 1 1 d . . . H34A H 0.0497 0.0080 0.0883 0.044 Uiso 1 1 calc R . . C35' C 0.00316(11) 0.10551(19) 0.08216(16) 0.0369(7) Uani 1 1 d . . . H35A H -0.0187 0.0840 0.0415 0.044 Uiso 1 1 calc R . . C36' C -0.00539(10) 0.18236(19) 0.11466(16) 0.0322(7) Uani 1 1 d . . . H36A H -0.0331 0.2123 0.0953 0.039 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 0.0314(4) 0.0451(6) 0.0280(4) 0.0014(4) 0.0001(3) 0.0133(4) O1 0.0305(11) 0.0678(17) 0.0466(12) -0.0088(12) -0.0027(9) 0.0106(11) O2 0.0492(13) 0.0527(15) 0.0375(11) 0.0046(11) 0.0050(9) 0.0191(12) C2 0.0246(14) 0.0312(17) 0.0282(14) 0.0010(13) 0.0004(11) 0.0034(12) C3 0.0274(14) 0.0239(16) 0.0291(14) -0.0041(12) 0.0018(11) -0.0029(12) C4 0.0295(14) 0.0239(16) 0.0273(13) -0.0002(12) 0.0015(11) -0.0025(13) C5 0.0299(14) 0.0290(17) 0.0275(14) 0.0016(13) 0.0024(11) 0.0027(13) C6 0.0394(19) 0.088(3) 0.060(2) 0.003(2) 0.0052(16) 0.008(2) C7 0.055(2) 0.062(3) 0.082(3) 0.023(2) 0.0231(19) 0.024(2) C21 0.0302(15) 0.0205(16) 0.0296(14) 0.0031(12) 0.0000(11) 0.0031(12) C22 0.0292(15) 0.0361(19) 0.0340(15) 0.0020(14) -0.0001(12) 0.0014(13) C23 0.0435(18) 0.041(2) 0.0314(15) 0.0009(14) -0.0105(13) -0.0084(15) C24 0.0519(19) 0.037(2) 0.0268(15) -0.0040(14) 0.0009(14) -0.0032(16) C25 0.0386(17) 0.039(2) 0.0329(16) 0.0010(14) 0.0072(13) 0.0037(14) C26 0.0307(15) 0.0351(19) 0.0297(14) 0.0006(13) -0.0008(12) 0.0042(13) C31 0.0298(14) 0.0292(17) 0.0193(13) -0.0015(12) -0.0010(11) 0.0054(13) C32 0.0365(16) 0.0314(18) 0.0283(14) 0.0005(13) -0.0023(12) 0.0021(14) C33 0.063(2) 0.0274(19) 0.0332(16) -0.0018(14) 0.0015(15) 0.0086(16) C34 0.053(2) 0.042(2) 0.0438(18) -0.0011(16) -0.0009(15) 0.0283(17) C35 0.0311(16) 0.055(2) 0.0420(17) -0.0041(17) -0.0044(13) 0.0115(16) C36 0.0337(16) 0.0334(18) 0.0301(14) -0.0053(13) -0.0019(12) 0.0063(14) C41 0.0248(13) 0.0287(17) 0.0251(13) -0.0019(13) 0.0033(11) 0.0016(12) C42 0.0304(15) 0.0267(17) 0.0336(15) -0.0014(13) -0.0004(12) -0.0006(13) C43 0.0414(17) 0.0349(19) 0.0363(16) 0.0075(14) 0.0005(13) 0.0077(15) C44 0.0432(18) 0.054(2) 0.0323(16) 0.0044(16) -0.0124(13) 0.0017(17) C45 0.0448(18) 0.047(2) 0.0392(16) -0.0027(16) -0.0094(14) -0.0117(16) C46 0.0417(16) 0.0300(18) 0.0322(15) 0.0024(14) 0.0011(13) -0.0029(14) C51 0.0274(14) 0.0269(17) 0.0296(14) -0.0013(13) 0.0022(11) -0.0002(13) C52 0.0315(15) 0.0286(17) 0.0339(15) 0.0039(14) 0.0054(12) 0.0025(13) C53 0.0389(16) 0.0345(19) 0.0292(15) 0.0032(14) 0.0081(12) -0.0027(14) C54 0.0393(16) 0.0331(19) 0.0363(16) -0.0043(14) 0.0134(13) 0.0000(14) C55 0.0424(17) 0.0336(19) 0.0408(17) 0.0032(15) 0.0083(13) 0.0131(15) C56 0.0410(17) 0.040(2) 0.0296(15) 0.0031(14) 0.0060(12) 0.0092(15) Si1' 0.0295(6) 0.0240(6) 0.0282(5) 0.000 0.0011(4) 0.000 O1' 0.0367(11) 0.0323(12) 0.0338(10) 0.0002(9) -0.0002(8) 0.0069(9) C2' 0.0245(14) 0.0269(17) 0.0276(14) 0.0021(12) -0.0037(11) 0.0002(12) C3' 0.0266(14) 0.0285(17) 0.0242(13) -0.0018(12) -0.0055(11) 0.0016(12) C4' 0.052(2) 0.053(2) 0.0486(19) -0.0060(17) -0.0023(15) 0.0241(18) C21' 0.0268(14) 0.0307(17) 0.0253(13) -0.0008(13) -0.0036(11) -0.0016(13) C22' 0.0349(16) 0.041(2) 0.0400(17) 0.0083(15) 0.0091(13) 0.0100(14) C23' 0.0462(18) 0.044(2) 0.0471(18) 0.0145(17) 0.0072(15) 0.0055(16) C24' 0.0353(16) 0.048(2) 0.0286(15) 0.0030(15) 0.0041(12) -0.0027(15) C25' 0.0282(15) 0.045(2) 0.0313(15) -0.0062(15) 0.0033(12) 0.0039(14) C26' 0.0383(16) 0.0309(18) 0.0312(15) 0.0014(13) 0.0005(12) 0.0047(14) C31' 0.0327(15) 0.0265(17) 0.0238(13) 0.0036(12) 0.0037(11) -0.0012(13) C32' 0.0451(18) 0.0319(19) 0.0316(15) -0.0034(14) -0.0071(13) 0.0048(15) C33' 0.0464(18) 0.036(2) 0.0367(16) 0.0017(15) -0.0026(14) 0.0123(15) C34' 0.0544(19) 0.0278(18) 0.0289(15) -0.0018(13) 0.0070(14) 0.0048(15) C35' 0.0445(18) 0.0362(19) 0.0298(15) -0.0055(14) -0.0002(13) -0.0066(15) C36' 0.0323(15) 0.0333(18) 0.0306(14) 0.0003(14) -0.0016(12) 0.0056(13) _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 O2 1.619(2) . ? Si1 O1 1.628(2) . ? Si1 C2 1.856(3) . ? Si1 C5 1.875(3) . ? O1 C6 1.405(3) . ? O2 C7 1.434(4) . ? C2 C3 1.352(3) . ? C2 C21 1.480(3) . ? C3 C31 1.489(4) . ? C3 C4 1.527(3) . ? C4 C5 1.345(4) . ? C4 C41 1.500(3) . ? C5 C51 1.485(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C21 C22 1.395(4) . ? C21 C26 1.402(3) . ? C22 C23 1.381(4) . ? C22 H22B 0.9300 . ? C23 C24 1.379(4) . ? C23 H23A 0.9300 . ? C24 C25 1.377(4) . ? C24 H24A 0.9300 . ? C25 C26 1.380(4) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C31 C32 1.382(4) . ? C31 C36 1.394(4) . ? C32 C33 1.379(4) . ? C32 H32A 0.9300 . ? C33 C34 1.380(4) . ? C33 H33A 0.9300 . ? C34 C35 1.371(4) . ? C34 H34B 0.9300 . ? C35 C36 1.386(4) . ? C35 H35B 0.9300 . ? C36 H36B 0.9300 . ? C41 C42 1.384(4) . ? C41 C46 1.388(4) . ? C42 C43 1.383(4) . ? C42 H42A 0.9300 . ? C43 C44 1.374(4) . ? C43 H43A 0.9300 . ? C44 C45 1.375(4) . ? C44 H44A 0.9300 . ? C45 C46 1.381(4) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C51 C56 1.389(4) . ? C51 C52 1.402(4) . ? C52 C53 1.385(4) . ? C52 H52A 0.9300 . ? C53 C54 1.376(4) . ? C53 H53A 0.9300 . ? C54 C55 1.383(4) . ? C54 H54A 0.9300 . ? C55 C56 1.386(4) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? Si1' O1' 1.6240(19) 2 ? Si1' O1' 1.6240(19) . ? Si1' C2' 1.864(3) . ? Si1' C2' 1.864(3) 2 ? O1' C4' 1.424(3) . ? C2' C3' 1.349(4) . ? C2' C21' 1.492(3) . ? C3' C31' 1.489(4) . ? C3' C3' 1.536(5) 2 ? C4' H4'B 0.9600 . ? C4' H4'C 0.9600 . ? C4' H4'D 0.9600 . ? C21' C22' 1.385(4) . ? C21' C26' 1.398(4) . ? C22' C23' 1.387(4) . ? C22' H22A 0.9300 . ? C23' C24' 1.374(4) . ? C23' H23B 0.9300 . ? C24' C25' 1.376(4) . ? C24' H24B 0.9300 . ? C25' C26' 1.393(4) . ? C25' H25B 0.9300 . ? C26' H26B 0.9300 . ? C31' C36' 1.386(4) . ? C31' C32' 1.390(4) . ? C32' C33' 1.384(4) . ? C32' H32B 0.9300 . ? C33' C34' 1.383(4) . ? C33' H33B 0.9300 . ? C34' C35' 1.377(4) . ? C34' H34A 0.9300 . ? C35' C36' 1.375(4) . ? C35' H35A 0.9300 . ? C36' H36A 0.9300 . ? 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 O2 Si1 O1 107.22(12) . . ? O2 Si1 C2 117.06(12) . . ? O1 Si1 C2 108.42(12) . . ? O2 Si1 C5 115.55(12) . . ? O1 Si1 C5 114.41(11) . . ? C2 Si1 C5 93.85(12) . . ? C6 O1 Si1 128.8(2) . . ? C7 O2 Si1 121.74(19) . . ? C3 C2 C21 127.2(2) . . ? C3 C2 Si1 106.72(19) . . ? C21 C2 Si1 126.05(18) . . ? C2 C3 C31 125.1(2) . . ? C2 C3 C4 116.1(2) . . ? C31 C3 C4 118.6(2) . . ? C5 C4 C41 126.9(2) . . ? C5 C4 C3 116.6(2) . . ? C41 C4 C3 116.4(2) . . ? C4 C5 C51 128.4(2) . . ? C4 C5 Si1 106.25(18) . . ? C51 C5 Si1 125.39(19) . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C22 C21 C26 116.9(2) . . ? C22 C21 C2 119.6(2) . . ? C26 C21 C2 123.5(2) . . ? C23 C22 C21 121.8(3) . . ? C23 C22 H22B 119.1 . . ? C21 C22 H22B 119.1 . . ? C24 C23 C22 120.0(3) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C25 C24 C23 119.6(3) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C26 120.4(3) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C25 C26 C21 121.2(2) . . ? C25 C26 H26A 119.4 . . ? C21 C26 H26A 119.4 . . ? C32 C31 C36 118.7(3) . . ? C32 C31 C3 118.8(2) . . ? C36 C31 C3 122.5(3) . . ? C33 C32 C31 121.1(3) . . ? C33 C32 H32A 119.4 . . ? C31 C32 H32A 119.4 . . ? C32 C33 C34 119.9(3) . . ? C32 C33 H33A 120.1 . . ? C34 C33 H33A 120.1 . . ? C35 C34 C33 119.7(3) . . ? C35 C34 H34B 120.2 . . ? C33 C34 H34B 120.2 . . ? C34 C35 C36 120.8(3) . . ? C34 C35 H35B 119.6 . . ? C36 C35 H35B 119.6 . . ? C35 C36 C31 119.8(3) . . ? C35 C36 H36B 120.1 . . ? C31 C36 H36B 120.1 . . ? C42 C41 C46 118.8(2) . . ? C42 C41 C4 122.0(2) . . ? C46 C41 C4 119.2(2) . . ? C43 C42 C41 120.9(3) . . ? C43 C42 H42A 119.5 . . ? C41 C42 H42A 119.5 . . ? C44 C43 C42 119.8(3) . . ? C44 C43 H43A 120.1 . . ? C42 C43 H43A 120.1 . . ? C43 C44 C45 119.9(3) . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? C44 C45 C46 120.6(3) . . ? C44 C45 H45A 119.7 . . ? C46 C45 H45A 119.7 . . ? C45 C46 C41 120.0(3) . . ? C45 C46 H46A 120.0 . . ? C41 C46 H46A 120.0 . . ? C56 C51 C52 117.1(2) . . ? C56 C51 C5 119.0(2) . . ? C52 C51 C5 123.8(2) . . ? C53 C52 C51 120.6(3) . . ? C53 C52 H52A 119.7 . . ? C51 C52 H52A 119.7 . . ? C54 C53 C52 120.8(3) . . ? C54 C53 H53A 119.6 . . ? C52 C53 H53A 119.6 . . ? C53 C54 C55 119.8(3) . . ? C53 C54 H54A 120.1 . . ? C55 C54 H54A 120.1 . . ? C54 C55 C56 119.2(3) . . ? C54 C55 H55A 120.4 . . ? C56 C55 H55A 120.4 . . ? C55 C56 C51 122.4(3) . . ? C55 C56 H56A 118.8 . . ? C51 C56 H56A 118.8 . . ? O1' Si1' O1' 110.72(15) 2 . ? O1' Si1' C2' 114.91(10) 2 . ? O1' Si1' C2' 110.74(10) . . ? O1' Si1' C2' 110.74(10) 2 2 ? O1' Si1' C2' 114.91(10) . 2 ? C2' Si1' C2' 94.00(17) . 2 ? C4' O1' Si1' 125.07(17) . . ? C3' C2' C21' 128.6(3) . . ? C3' C2' Si1' 106.82(19) . . ? C21' C2' Si1' 124.5(2) . . ? C2' C3' C31' 126.9(2) . . ? C2' C3' C3' 116.18(15) . 2 ? C31' C3' C3' 116.89(14) . 2 ? O1' C4' H4'B 109.5 . . ? O1' C4' H4'C 109.5 . . ? H4'B C4' H4'C 109.5 . . ? O1' C4' H4'D 109.5 . . ? H4'B C4' H4'D 109.5 . . ? H4'C C4' H4'D 109.5 . . ? C22' C21' C26' 117.5(2) . . ? C22' C21' C2' 118.1(2) . . ? C26' C21' C2' 124.3(3) . . ? C21' C22' C23' 121.7(3) . . ? C21' C22' H22A 119.2 . . ? C23' C22' H22A 119.2 . . ? C24' C23' C22' 120.3(3) . . ? C24' C23' H23B 119.8 . . ? C22' C23' H23B 119.8 . . ? C23' C24' C25' 119.1(3) . . ? C23' C24' H24B 120.5 . . ? C25' C24' H24B 120.5 . . ? C24' C25' C26' 120.9(3) . . ? C24' C25' H25B 119.6 . . ? C26' C25' H25B 119.6 . . ? C25' C26' C21' 120.5(3) . . ? C25' C26' H26B 119.8 . . ? C21' C26' H26B 119.8 . . ? C36' C31' C32' 117.9(3) . . ? C36' C31' C3' 120.2(2) . . ? C32' C31' C3' 121.9(2) . . ? C33' C32' C31' 120.7(3) . . ? C33' C32' H32B 119.6 . . ? C31' C32' H32B 119.6 . . ? C34' C33' C32' 120.3(3) . . ? C34' C33' H33B 119.9 . . ? C32' C33' H33B 119.9 . . ? C35' C34' C33' 119.4(3) . . ? C35' C34' H34A 120.3 . . ? C33' C34' H34A 120.3 . . ? C36' C35' C34' 120.1(3) . . ? C36' C35' H35A 119.9 . . ? C34' C35' H35A 119.9 . . ? C35' C36' C31' 121.6(3) . . ? C35' C36' H36A 119.2 . . ? C31' C36' H36A 119.2 . . ? 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 O2 Si1 O1 C6 -56.2(3) . . . . ? C2 Si1 O1 C6 176.6(2) . . . . ? C5 Si1 O1 C6 73.4(3) . . . . ? O1 Si1 O2 C7 -175.2(2) . . . . ? C2 Si1 O2 C7 -53.2(3) . . . . ? C5 Si1 O2 C7 56.0(3) . . . . ? O2 Si1 C2 C3 127.3(2) . . . . ? O1 Si1 C2 C3 -111.3(2) . . . . ? C5 Si1 C2 C3 6.0(2) . . . . ? O2 Si1 C2 C21 -55.0(3) . . . . ? O1 Si1 C2 C21 66.4(3) . . . . ? C5 Si1 C2 C21 -176.3(2) . . . . ? C21 C2 C3 C31 -8.3(5) . . . . ? Si1 C2 C3 C31 169.3(2) . . . . ? C21 C2 C3 C4 176.6(3) . . . . ? Si1 C2 C3 C4 -5.7(3) . . . . ? C2 C3 C4 C5 2.3(4) . . . . ? C31 C3 C4 C5 -173.1(2) . . . . ? C2 C3 C4 C41 -176.6(2) . . . . ? C31 C3 C4 C41 8.0(3) . . . . ? C41 C4 C5 C51 0.6(5) . . . . ? C3 C4 C5 C51 -178.2(3) . . . . ? C41 C4 C5 Si1 -178.7(2) . . . . ? C3 C4 C5 Si1 2.5(3) . . . . ? O2 Si1 C5 C4 -127.3(2) . . . . ? O1 Si1 C5 C4 107.4(2) . . . . ? C2 Si1 C5 C4 -4.8(2) . . . . ? O2 Si1 C5 C51 53.3(3) . . . . ? O1 Si1 C5 C51 -71.9(3) . . . . ? C2 Si1 C5 C51 175.9(2) . . . . ? C3 C2 C21 C22 151.0(3) . . . . ? Si1 C2 C21 C22 -26.2(4) . . . . ? C3 C2 C21 C26 -30.5(5) . . . . ? Si1 C2 C21 C26 152.3(2) . . . . ? C26 C21 C22 C23 2.7(4) . . . . ? C2 C21 C22 C23 -178.7(3) . . . . ? C21 C22 C23 C24 -1.3(5) . . . . ? C22 C23 C24 C25 -1.1(5) . . . . ? C23 C24 C25 C26 2.0(5) . . . . ? C24 C25 C26 C21 -0.6(5) . . . . ? C22 C21 C26 C25 -1.7(4) . . . . ? C2 C21 C26 C25 179.8(3) . . . . ? C2 C3 C31 C32 -62.8(4) . . . . ? C4 C3 C31 C32 112.1(3) . . . . ? C2 C3 C31 C36 118.4(3) . . . . ? C4 C3 C31 C36 -66.6(3) . . . . ? C36 C31 C32 C33 0.7(4) . . . . ? C3 C31 C32 C33 -178.1(2) . . . . ? C31 C32 C33 C34 0.0(4) . . . . ? C32 C33 C34 C35 -0.8(4) . . . . ? C33 C34 C35 C36 0.9(5) . . . . ? C34 C35 C36 C31 -0.2(4) . . . . ? C32 C31 C36 C35 -0.6(4) . . . . ? C3 C31 C36 C35 178.2(2) . . . . ? C5 C4 C41 C42 112.9(3) . . . . ? C3 C4 C41 C42 -68.4(3) . . . . ? C5 C4 C41 C46 -69.1(4) . . . . ? C3 C4 C41 C46 109.7(3) . . . . ? C46 C41 C42 C43 0.5(4) . . . . ? C4 C41 C42 C43 178.6(2) . . . . ? C41 C42 C43 C44 -1.3(4) . . . . ? C42 C43 C44 C45 1.1(4) . . . . ? C43 C44 C45 C46 -0.3(5) . . . . ? C44 C45 C46 C41 -0.5(4) . . . . ? C42 C41 C46 C45 0.4(4) . . . . ? C4 C41 C46 C45 -177.8(2) . . . . ? C4 C5 C51 C56 156.1(3) . . . . ? Si1 C5 C51 C56 -24.7(4) . . . . ? C4 C5 C51 C52 -24.6(4) . . . . ? Si1 C5 C51 C52 154.6(2) . . . . ? C56 C51 C52 C53 -2.5(4) . . . . ? C5 C51 C52 C53 178.3(3) . . . . ? C51 C52 C53 C54 0.3(4) . . . . ? C52 C53 C54 C55 1.6(4) . . . . ? C53 C54 C55 C56 -1.3(4) . . . . ? C54 C55 C56 C51 -1.0(5) . . . . ? C52 C51 C56 C55 2.8(4) . . . . ? C5 C51 C56 C55 -177.9(3) . . . . ? O1' Si1' O1' C4' -56.6(2) 2 . . . ? C2' Si1' O1' C4' 174.7(2) . . . . ? C2' Si1' O1' C4' 69.8(3) 2 . . . ? O1' Si1' C2' C3' 114.83(18) 2 . . . ? O1' Si1' C2' C3' -118.80(18) . . . . ? C2' Si1' C2' C3' -0.25(12) 2 . . . ? O1' Si1' C2' C21' -61.8(2) 2 . . . ? O1' Si1' C2' C21' 64.6(2) . . . . ? C2' Si1' C2' C21' -176.9(3) 2 . . . ? C21' C2' C3' C31' -6.3(4) . . . . ? Si1' C2' C3' C31' 177.3(2) . . . . ? C21' C2' C3' C3' 177.1(2) . . . 2 ? Si1' C2' C3' C3' 0.6(3) . . . 2 ? C3' C2' C21' C22' 155.1(3) . . . . ? Si1' C2' C21' C22' -29.0(3) . . . . ? C3' C2' C21' C26' -29.7(4) . . . . ? Si1' C2' C21' C26' 146.2(2) . . . . ? C26' C21' C22' C23' 2.4(4) . . . . ? C2' C21' C22' C23' 178.0(3) . . . . ? C21' C22' C23' C24' -1.8(5) . . . . ? C22' C23' C24' C25' 0.0(5) . . . . ? C23' C24' C25' C26' 0.9(4) . . . . ? C24' C25' C26' C21' -0.2(4) . . . . ? C22' C21' C26' C25' -1.4(4) . . . . ? C2' C21' C26' C25' -176.7(2) . . . . ? C2' C3' C31' C36' -84.4(3) . . . . ? C3' C3' C31' C36' 92.2(3) 2 . . . ? C2' C3' C31' C32' 97.4(3) . . . . ? C3' C3' C31' C32' -86.0(3) 2 . . . ? C36' C31' C32' C33' 0.4(4) . . . . ? C3' C31' C32' C33' 178.7(3) . . . . ? C31' C32' C33' C34' -1.4(4) . . . . ? C32' C33' C34' C35' 1.5(4) . . . . ? C33' C34' C35' C36' -0.7(4) . . . . ? C34' C35' C36' C31' -0.2(4) . . . . ? C32' C31' C36' C35' 0.4(4) . . . . ? C3' C31' C36' C35' -177.9(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.528 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.056 _publ_section_references ; Bruker (1998a). SAINTPlus. Data Reduction and Correction Program v. 6.01, Bruker AXS, Madison, Wisconsin, USA. Bruker (1998b). SMART. Bruker Molecular Analysis Research Tool, v. 5.059. Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998b). SHELXTL v. 5.10, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; data_COMPOUND_IV _database_code_depnum_ccdc_archive 'CCDC 604521' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H32 Si2' _chemical_formula_sum 'C32 H32 Si2' _chemical_formula_weight 472.76 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 9.782(2) _cell_length_b 22.465(6) _cell_length_c 12.753(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.581(19) _cell_angle_gamma 90.00 _cell_volume 2763.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 15.0 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details I>2\s(I) _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Rebuild Syntex P2~1~/Siemens P3 four-circle diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6412 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.06 _reflns_number_total 6066 _reflns_number_gt 4454 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Siemens P3/PC (Siemens, 1989)' _computing_cell_refinement 'Siemens P3/PC (Siemens, 1989)' _computing_data_reduction 'Siemens P3/PC (Siemens, 1989)' _computing_structure_solution 'SHELXTL PLUS 5 (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL PLUS 5 (Sheldrick, 1998)' _computing_molecular_graphics 'SHELXTL PLUS 5 (Sheldrick, 1998)' _computing_publication_material 'SHELXTL PLUS 5 (Sheldrick, 1998)' _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^)+(0.03P)^2^+2.16P] 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 6066 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 Si1 Si 0.86683(5) 0.14155(2) 0.70626(4) 0.02791(12) Uani 1 1 d . . . Si2 Si 1.00857(5) 0.20092(2) 0.62148(4) 0.02983(12) Uani 1 1 d . . . C1 C 1.00940(16) 0.12132(7) 0.81999(13) 0.0255(3) Uani 1 1 d . . . C2 C 1.13611(17) 0.10484(7) 0.80186(13) 0.0248(3) Uani 1 1 d . . . C3 C 1.17601(16) 0.09905(7) 0.69314(13) 0.0255(3) Uani 1 1 d . . . C4 C 1.14319(17) 0.14020(7) 0.61591(13) 0.0269(3) Uani 1 1 d . . . C5 C 0.71255(19) 0.17217(10) 0.75699(17) 0.0428(5) Uani 1 1 d . . . H5A H 0.6675 0.1408 0.7893 0.064 Uiso 1 1 calc R . . H5B H 0.6490 0.1889 0.6990 0.064 Uiso 1 1 calc R . . H5C H 0.7419 0.2026 0.8087 0.064 Uiso 1 1 calc R . . C6 C 0.8091(2) 0.07448(9) 0.62482(16) 0.0432(5) Uani 1 1 d . . . H6A H 0.7506 0.0505 0.6613 0.065 Uiso 1 1 calc R . . H6B H 0.8886 0.0517 0.6140 0.065 Uiso 1 1 calc R . . H6C H 0.7583 0.0867 0.5573 0.065 Uiso 1 1 calc R . . C7 C 1.0866(2) 0.26687(8) 0.69811(17) 0.0427(5) Uani 1 1 d . . . H7A H 1.1432 0.2884 0.6564 0.064 Uiso 1 1 calc R . . H7B H 1.1427 0.2538 0.7630 0.064 Uiso 1 1 calc R . . H7C H 1.0141 0.2923 0.7143 0.064 Uiso 1 1 calc R . . C8 C 0.9353(2) 0.22285(10) 0.48183(16) 0.0462(5) Uani 1 1 d . . . H8A H 1.0011 0.2472 0.4536 0.069 Uiso 1 1 calc R . . H8B H 0.8510 0.2448 0.4814 0.069 Uiso 1 1 calc R . . H8C H 0.9163 0.1878 0.4389 0.069 Uiso 1 1 calc R . . C11 C 0.98414(16) 0.13357(7) 0.93002(13) 0.0260(3) Uani 1 1 d . . . C12 C 0.88710(17) 0.10136(9) 0.97455(14) 0.0341(4) Uani 1 1 d . . . H12A H 0.8361 0.0717 0.9349 0.041 Uiso 1 1 calc R . . C13 C 0.8651(2) 0.11274(11) 1.07723(15) 0.0444(5) Uani 1 1 d . . . H13A H 0.8011 0.0901 1.1062 0.053 Uiso 1 1 calc R . . C14 C 0.9368(2) 0.15711(11) 1.13638(16) 0.0479(5) Uani 1 1 d . . . H14A H 0.9218 0.1647 1.2052 0.058 Uiso 1 1 calc R . . C15 C 1.0318(2) 0.19043(9) 1.09248(16) 0.0452(5) Uani 1 1 d . . . H15A H 1.0804 0.2208 1.1319 0.054 Uiso 1 1 calc R . . C16 C 1.05522(19) 0.17898(8) 0.99043(15) 0.0351(4) Uani 1 1 d . . . H16A H 1.1191 0.2019 0.9618 0.042 Uiso 1 1 calc R . . C21 C 1.25351(16) 0.09194(7) 0.89090(13) 0.0252(3) Uani 1 1 d . . . C22 C 1.38096(18) 0.11958(8) 0.89317(14) 0.0319(4) Uani 1 1 d . . . H22A H 1.3944 0.1446 0.8377 0.038 Uiso 1 1 calc R . . C23 C 1.48808(19) 0.11023(9) 0.97694(15) 0.0376(4) Uani 1 1 d . . . H23A H 1.5724 0.1296 0.9781 0.045 Uiso 1 1 calc R . . C24 C 1.47054(19) 0.07235(9) 1.05874(15) 0.0393(4) Uani 1 1 d . . . H24A H 1.5427 0.0662 1.1151 0.047 Uiso 1 1 calc R . . C25 C 1.3453(2) 0.04365(9) 1.05660(14) 0.0369(4) Uani 1 1 d . . . H25A H 1.3335 0.0178 1.1114 0.044 Uiso 1 1 calc R . . C26 C 1.23709(18) 0.05310(8) 0.97321(14) 0.0308(4) Uani 1 1 d . . . H26A H 1.1532 0.0335 0.9722 0.037 Uiso 1 1 calc R . . C31 C 1.25558(16) 0.04353(8) 0.67784(12) 0.0258(3) Uani 1 1 d . . . C32 C 1.38559(18) 0.04358(9) 0.64776(14) 0.0332(4) Uani 1 1 d . . . H32A H 1.4286 0.0795 0.6374 0.040 Uiso 1 1 calc R . . C33 C 1.45161(19) -0.00959(9) 0.63312(15) 0.0388(4) Uani 1 1 d . . . H33A H 1.5389 -0.0091 0.6133 0.047 Uiso 1 1 calc R . . C34 C 1.3892(2) -0.06320(9) 0.64771(14) 0.0379(4) Uani 1 1 d . . . H34A H 1.4339 -0.0988 0.6375 0.045 Uiso 1 1 calc R . . C35 C 1.2602(2) -0.06386(8) 0.67746(14) 0.0349(4) Uani 1 1 d . . . H35A H 1.2169 -0.0999 0.6864 0.042 Uiso 1 1 calc R . . C36 C 1.19478(18) -0.01083(8) 0.69414(13) 0.0298(4) Uani 1 1 d . . . H36A H 1.1090 -0.0116 0.7165 0.036 Uiso 1 1 calc R . . C41 C 1.19327(17) 0.13565(7) 0.51160(13) 0.0286(4) Uani 1 1 d . . . C42 C 1.2858(2) 0.17808(9) 0.48590(15) 0.0373(4) Uani 1 1 d . . . H42A H 1.3189 0.2075 0.5350 0.045 Uiso 1 1 calc R . . C43 C 1.3293(2) 0.17703(9) 0.38786(17) 0.0432(5) Uani 1 1 d . . . H43A H 1.3930 0.2051 0.3723 0.052 Uiso 1 1 calc R . . C44 C 1.2787(2) 0.13462(10) 0.31318(16) 0.0421(5) Uani 1 1 d . . . H44A H 1.3071 0.1342 0.2471 0.051 Uiso 1 1 calc R . . C45 C 1.1860(2) 0.09290(9) 0.33740(15) 0.0401(4) Uani 1 1 d . . . H45A H 1.1512 0.0643 0.2872 0.048 Uiso 1 1 calc R . . C46 C 1.14366(19) 0.09304(8) 0.43612(14) 0.0337(4) Uani 1 1 d . . . H46A H 1.0816 0.0643 0.4517 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0236(2) 0.0290(2) 0.0298(2) 0.00414(19) 0.00039(18) -0.00109(18) Si2 0.0323(3) 0.0251(2) 0.0330(3) 0.0048(2) 0.0082(2) 0.00195(19) C1 0.0248(8) 0.0243(8) 0.0267(8) 0.0004(6) 0.0022(6) -0.0037(6) C2 0.0262(8) 0.0219(8) 0.0253(8) 0.0004(6) 0.0013(6) -0.0025(6) C3 0.0229(8) 0.0273(8) 0.0261(8) -0.0010(7) 0.0031(6) -0.0023(6) C4 0.0271(8) 0.0254(8) 0.0288(8) 0.0004(7) 0.0064(6) -0.0037(7) C5 0.0283(9) 0.0487(12) 0.0513(12) 0.0129(10) 0.0065(8) 0.0070(8) C6 0.0422(11) 0.0425(11) 0.0398(11) -0.0028(9) -0.0076(9) -0.0084(9) C7 0.0475(11) 0.0308(10) 0.0544(12) -0.0040(9) 0.0222(10) -0.0049(9) C8 0.0529(12) 0.0443(12) 0.0413(11) 0.0149(9) 0.0075(9) 0.0136(10) C11 0.0210(7) 0.0283(8) 0.0277(8) 0.0012(7) 0.0008(6) 0.0027(6) C12 0.0239(8) 0.0438(10) 0.0339(9) 0.0035(8) 0.0025(7) -0.0036(7) C13 0.0296(9) 0.0707(15) 0.0338(10) 0.0123(10) 0.0084(8) 0.0042(9) C14 0.0439(12) 0.0704(15) 0.0297(10) -0.0022(10) 0.0066(9) 0.0181(11) C15 0.0505(12) 0.0429(11) 0.0393(11) -0.0145(9) -0.0016(9) 0.0065(9) C16 0.0350(9) 0.0319(9) 0.0381(10) -0.0037(8) 0.0052(8) -0.0026(8) C21 0.0235(8) 0.0267(8) 0.0252(8) -0.0037(6) 0.0038(6) 0.0032(6) C22 0.0280(9) 0.0371(10) 0.0306(9) -0.0022(7) 0.0046(7) -0.0027(7) C23 0.0239(8) 0.0492(11) 0.0382(10) -0.0076(9) 0.0007(7) -0.0019(8) C24 0.0316(9) 0.0521(12) 0.0308(9) -0.0056(9) -0.0048(7) 0.0087(9) C25 0.0415(10) 0.0396(10) 0.0280(9) 0.0048(8) 0.0012(8) 0.0065(8) C26 0.0288(9) 0.0313(9) 0.0318(9) 0.0014(7) 0.0036(7) 0.0012(7) C31 0.0248(8) 0.0314(9) 0.0204(7) 0.0001(6) 0.0010(6) 0.0025(7) C32 0.0277(9) 0.0385(10) 0.0333(9) 0.0026(8) 0.0052(7) -0.0001(7) C33 0.0284(9) 0.0543(12) 0.0342(10) 0.0003(9) 0.0068(7) 0.0111(8) C34 0.0432(11) 0.0388(10) 0.0297(9) -0.0016(8) 0.0007(8) 0.0148(8) C35 0.0444(11) 0.0306(9) 0.0290(9) -0.0017(7) 0.0043(8) 0.0015(8) C36 0.0305(9) 0.0327(9) 0.0266(8) -0.0001(7) 0.0055(7) -0.0002(7) C41 0.0298(8) 0.0278(8) 0.0285(9) 0.0058(7) 0.0053(7) 0.0044(7) C42 0.0415(10) 0.0331(9) 0.0394(10) 0.0015(8) 0.0125(8) -0.0017(8) C43 0.0441(11) 0.0414(11) 0.0483(12) 0.0125(9) 0.0202(9) 0.0024(9) C44 0.0439(11) 0.0528(12) 0.0329(10) 0.0100(9) 0.0159(8) 0.0157(9) C45 0.0439(11) 0.0449(11) 0.0306(10) -0.0029(8) 0.0037(8) 0.0070(9) C46 0.0328(9) 0.0344(10) 0.0337(9) 0.0022(8) 0.0049(7) -0.0004(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 Si1 C6 1.863(2) . ? Si1 C5 1.869(2) . ? Si1 C1 1.8926(17) . ? Si1 Si2 2.3172(8) . ? Si2 C7 1.867(2) . ? Si2 C8 1.872(2) . ? Si2 C4 1.9056(18) . ? C1 C2 1.350(2) . ? C1 C11 1.490(2) . ? C2 C3 1.507(2) . ? C2 C21 1.503(2) . ? C3 C4 1.350(2) . ? C3 C31 1.500(2) . ? C4 C41 1.496(2) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C11 C12 1.388(2) . ? C11 C16 1.393(2) . ? C12 C13 1.386(3) . ? C12 H12A 0.9300 . ? C13 C14 1.371(3) . ? C13 H13A 0.9300 . ? C14 C15 1.382(3) . ? C14 H14A 0.9300 . ? C15 C16 1.383(3) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C21 C22 1.389(2) . ? C21 C26 1.395(2) . ? C22 C23 1.382(2) . ? C22 H22A 0.9300 . ? C23 C24 1.379(3) . ? C23 H23A 0.9300 . ? C24 C25 1.380(3) . ? C24 H24A 0.9300 . ? C25 C26 1.387(2) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C31 C32 1.388(2) . ? C31 C36 1.389(2) . ? C32 C33 1.385(3) . ? C32 H32A 0.9300 . ? C33 C34 1.377(3) . ? C33 H33A 0.9300 . ? C34 C35 1.377(3) . ? C34 H34A 0.9300 . ? C35 C36 1.385(2) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C41 C46 1.387(3) . ? C41 C42 1.391(2) . ? C42 C43 1.386(3) . ? C42 H42A 0.9300 . ? C43 C44 1.379(3) . ? C43 H43A 0.9300 . ? C44 C45 1.375(3) . ? C44 H44A 0.9300 . ? C45 C46 1.389(3) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? 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 C5 107.66(10) . . ? C6 Si1 C1 110.44(8) . . ? C5 Si1 C1 110.94(9) . . ? C6 Si1 Si2 110.77(7) . . ? C5 Si1 Si2 122.00(7) . . ? C1 Si1 Si2 94.25(6) . . ? C7 Si2 C8 110.35(10) . . ? C7 Si2 C4 111.27(9) . . ? C8 Si2 C4 108.08(9) . . ? C7 Si2 Si1 115.91(7) . . ? C8 Si2 Si1 115.57(8) . . ? C4 Si2 Si1 94.37(6) . . ? C2 C1 C11 120.84(15) . . ? C2 C1 Si1 121.00(13) . . ? C11 C1 Si1 117.44(12) . . ? C1 C2 C3 124.53(15) . . ? C1 C2 C21 122.11(15) . . ? C3 C2 C21 113.34(14) . . ? C4 C3 C31 122.69(15) . . ? C4 C3 C2 123.07(15) . . ? C31 C3 C2 114.24(14) . . ? C3 C4 C41 121.93(15) . . ? C3 C4 Si2 123.02(13) . . ? C41 C4 Si2 114.38(12) . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C11 C16 117.90(16) . . ? C12 C11 C1 121.39(15) . . ? C16 C11 C1 120.69(15) . . ? C13 C12 C11 120.99(18) . . ? C13 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? C14 C13 C12 120.56(19) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C13 C14 C15 119.21(19) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? C16 C15 C14 120.55(19) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C11 120.77(18) . . ? C15 C16 H16A 119.6 . . ? C11 C16 H16A 119.6 . . ? C22 C21 C26 118.65(15) . . ? C22 C21 C2 120.00(15) . . ? C26 C21 C2 121.34(15) . . ? C23 C22 C21 120.70(17) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 120.32(18) . . ? C22 C23 H23A 119.8 . . ? C24 C23 H23A 119.8 . . ? C23 C24 C25 119.68(17) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C24 C25 C26 120.35(18) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C25 C26 C21 120.28(17) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? C32 C31 C36 118.47(16) . . ? C32 C31 C3 123.66(16) . . ? C36 C31 C3 117.86(14) . . ? C33 C32 C31 120.38(18) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C34 C33 C32 120.58(17) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C35 C34 C33 119.61(17) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C34 C35 C36 120.05(18) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C31 120.87(16) . . ? C35 C36 H36A 119.6 . . ? C31 C36 H36A 119.6 . . ? C46 C41 C42 118.41(16) . . ? C46 C41 C4 122.41(16) . . ? C42 C41 C4 119.02(16) . . ? C43 C42 C41 120.69(19) . . ? C43 C42 H42A 119.7 . . ? C41 C42 H42A 119.7 . . ? C44 C43 C42 120.39(19) . . ? C44 C43 H43A 119.8 . . ? C42 C43 H43A 119.8 . . ? C45 C44 C43 119.34(18) . . ? C45 C44 H44A 120.3 . . ? C43 C44 H44A 120.3 . . ? C44 C45 C46 120.62(19) . . ? C44 C45 H45A 119.7 . . ? C46 C45 H45A 119.7 . . ? C41 C46 C45 120.54(18) . . ? C41 C46 H46A 119.7 . . ? C45 C46 H46A 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Si1 Si2 C7 -175.25(10) . . . . ? C5 Si1 Si2 C7 56.47(12) . . . . ? C1 Si1 Si2 C7 -61.50(10) . . . . ? C6 Si1 Si2 C8 53.38(11) . . . . ? C5 Si1 Si2 C8 -74.90(11) . . . . ? C1 Si1 Si2 C8 167.13(9) . . . . ? C6 Si1 Si2 C4 -59.05(9) . . . . ? C5 Si1 Si2 C4 172.67(9) . . . . ? C1 Si1 Si2 C4 54.70(8) . . . . ? C6 Si1 C1 C2 68.41(16) . . . . ? C5 Si1 C1 C2 -172.29(14) . . . . ? Si2 Si1 C1 C2 -45.61(14) . . . . ? C6 Si1 C1 C11 -121.20(13) . . . . ? C5 Si1 C1 C11 -1.91(15) . . . . ? Si2 Si1 C1 C11 124.77(12) . . . . ? C11 C1 C2 C3 -171.92(15) . . . . ? Si1 C1 C2 C3 -1.9(2) . . . . ? C11 C1 C2 C21 6.4(2) . . . . ? Si1 C1 C2 C21 176.42(12) . . . . ? C1 C2 C3 C4 45.3(2) . . . . ? C21 C2 C3 C4 -133.15(16) . . . . ? C1 C2 C3 C31 -134.73(17) . . . . ? C21 C2 C3 C31 46.85(19) . . . . ? C31 C3 C4 C41 -4.7(2) . . . . ? C2 C3 C4 C41 175.26(15) . . . . ? C31 C3 C4 Si2 165.29(12) . . . . ? C2 C3 C4 Si2 -14.7(2) . . . . ? C7 Si2 C4 C3 85.37(16) . . . . ? C8 Si2 C4 C3 -153.33(15) . . . . ? Si1 Si2 C4 C3 -34.63(14) . . . . ? C7 Si2 C4 C41 -103.92(14) . . . . ? C8 Si2 C4 C41 17.39(15) . . . . ? Si1 Si2 C4 C41 136.09(12) . . . . ? C2 C1 C11 C12 -120.33(18) . . . . ? Si1 C1 C11 C12 69.28(19) . . . . ? C2 C1 C11 C16 61.3(2) . . . . ? Si1 C1 C11 C16 -109.06(16) . . . . ? C16 C11 C12 C13 -2.1(3) . . . . ? C1 C11 C12 C13 179.48(17) . . . . ? C11 C12 C13 C14 1.4(3) . . . . ? C12 C13 C14 C15 -0.1(3) . . . . ? C13 C14 C15 C16 -0.5(3) . . . . ? C14 C15 C16 C11 -0.3(3) . . . . ? C12 C11 C16 C15 1.6(3) . . . . ? C1 C11 C16 C15 179.96(17) . . . . ? C1 C2 C21 C22 -128.30(18) . . . . ? C3 C2 C21 C22 50.2(2) . . . . ? C1 C2 C21 C26 50.7(2) . . . . ? C3 C2 C21 C26 -130.80(16) . . . . ? C26 C21 C22 C23 -1.9(3) . . . . ? C2 C21 C22 C23 177.11(16) . . . . ? C21 C22 C23 C24 1.2(3) . . . . ? C22 C23 C24 C25 0.1(3) . . . . ? C23 C24 C25 C26 -0.5(3) . . . . ? C24 C25 C26 C21 -0.3(3) . . . . ? C22 C21 C26 C25 1.5(3) . . . . ? C2 C21 C26 C25 -177.54(16) . . . . ? C4 C3 C31 C32 56.8(2) . . . . ? C2 C3 C31 C32 -123.24(17) . . . . ? C4 C3 C31 C36 -122.79(18) . . . . ? C2 C3 C31 C36 57.21(19) . . . . ? C36 C31 C32 C33 0.8(3) . . . . ? C3 C31 C32 C33 -178.70(16) . . . . ? C31 C32 C33 C34 0.3(3) . . . . ? C32 C33 C34 C35 -0.2(3) . . . . ? C33 C34 C35 C36 -1.0(3) . . . . ? C34 C35 C36 C31 2.1(3) . . . . ? C32 C31 C36 C35 -2.1(2) . . . . ? C3 C31 C36 C35 177.52(15) . . . . ? C3 C4 C41 C46 70.7(2) . . . . ? Si2 C4 C41 C46 -100.08(17) . . . . ? C3 C4 C41 C42 -113.81(19) . . . . ? Si2 C4 C41 C42 75.37(18) . . . . ? C46 C41 C42 C43 -1.2(3) . . . . ? C4 C41 C42 C43 -176.84(17) . . . . ? C41 C42 C43 C44 1.6(3) . . . . ? C42 C43 C44 C45 -0.8(3) . . . . ? C43 C44 C45 C46 -0.3(3) . . . . ? C42 C41 C46 C45 0.1(3) . . . . ? C4 C41 C46 C45 175.59(16) . . . . ? C44 C45 C46 C41 0.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.298 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.051 _publ_section_references ; Sheldrick G.M. (1998). SHELXTL v. 5.10, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. Siemens (1989). P3 and XDISK. Release 4.1. Siemens AXS, Madison, Wisconsin, USA. ; #===END