# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H28 S Si2' _chemical_formula_sum 'C30 H28 S Si2' _chemical_formula_weight 476.76 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' S S 0.1246 0.1234 '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 7.2587(15) _cell_length_b 13.877(3) _cell_length_c 13.896(3) _cell_angle_alpha 75.68(3) _cell_angle_beta 87.39(3) _cell_angle_gamma 78.99(3) _cell_volume 1331.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4962 _cell_measurement_theta_min 1.5124 _cell_measurement_theta_max 27.4816 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8088 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16033 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6063 _reflns_number_gt 5290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _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^)+(0.0468P)^2^+0.9135P] 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 6063 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1529 _refine_ls_wR_factor_gt 0.1460 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _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 S1 S 0.17446(10) 0.49941(5) 0.80607(5) 0.03416(18) Uani 1 1 d . . . Si1 Si 0.15821(11) 0.98786(6) 0.69366(5) 0.03275(19) Uani 1 1 d . . . Si2 Si 0.35537(13) 0.36996(6) 1.43972(6) 0.0405(2) Uani 1 1 d . . . C1 C 0.1782(3) 0.37852(19) 0.8850(2) 0.0305(6) Uani 1 1 d . . . C2 C 0.1448(4) 0.2941(2) 0.8563(2) 0.0367(6) Uani 1 1 d . . . H2 H 0.1178 0.2978 0.7891 0.044 Uiso 1 1 calc R . . C3 C 0.1522(4) 0.2047(2) 0.9285(2) 0.0379(6) Uani 1 1 d . . . H3 H 0.1308 0.1461 0.9104 0.045 Uiso 1 1 calc R . . C4 C 0.1905(4) 0.1990(2) 1.0275(2) 0.0381(6) Uani 1 1 d . . . H4 H 0.1941 0.1370 1.0759 0.046 Uiso 1 1 calc R . . C5 C 0.2231(4) 0.28309(19) 1.0554(2) 0.0339(6) Uani 1 1 d . . . H5 H 0.2494 0.2790 1.1228 0.041 Uiso 1 1 calc R . . C6 C 0.2170(3) 0.37397(19) 0.98412(19) 0.0286(5) Uani 1 1 d . . . C7 C 0.2436(3) 0.47141(18) 0.99712(19) 0.0276(5) Uani 1 1 d . . . C8 C 0.2793(3) 0.49662(18) 1.08224(19) 0.0279(5) Uani 1 1 d . . . H8 H 0.2920 0.4464 1.1432 0.033 Uiso 1 1 calc R . . C9 C 0.2978(3) 0.59700(18) 1.08100(18) 0.0260(5) Uani 1 1 d . . . C10 C 0.3299(3) 0.62437(18) 1.16962(18) 0.0268(5) Uani 1 1 d . . . C11 C 0.3531(3) 0.72361(18) 1.16732(19) 0.0268(5) Uani 1 1 d . . . C12 C 0.3919(4) 0.7514(2) 1.25490(19) 0.0316(6) Uani 1 1 d . . . H12 H 0.4009 0.7026 1.3168 0.038 Uiso 1 1 calc R . . C13 C 0.4164(4) 0.8471(2) 1.2515(2) 0.0347(6) Uani 1 1 d . . . H13 H 0.4435 0.8642 1.3108 0.042 Uiso 1 1 calc R . . C14 C 0.4018(4) 0.92077(19) 1.1605(2) 0.0346(6) Uani 1 1 d . . . H14 H 0.4200 0.9871 1.1589 0.041 Uiso 1 1 calc R . . C15 C 0.3620(4) 0.89792(19) 1.0754(2) 0.0326(6) Uani 1 1 d . . . H15 H 0.3502 0.9489 1.0150 0.039 Uiso 1 1 calc R . . C16 C 0.3374(3) 0.79852(18) 1.07504(19) 0.0269(5) Uani 1 1 d . . . C17 C 0.2983(3) 0.77240(18) 0.98729(18) 0.0270(5) Uani 1 1 d . . . C18 C 0.2812(3) 0.67221(18) 0.98796(18) 0.0265(5) Uani 1 1 d . . . C19 C 0.2444(3) 0.64416(19) 0.90018(18) 0.0280(5) Uani 1 1 d . . . H19 H 0.2329 0.6928 0.8382 0.034 Uiso 1 1 calc R . . C20 C 0.2256(3) 0.54686(19) 0.90512(19) 0.0288(5) Uani 1 1 d . . . C21 C 0.2673(4) 0.84833(19) 0.89553(19) 0.0304(6) Uani 1 1 d . . . C22 C 0.2316(4) 0.9087(2) 0.8173(2) 0.0360(6) Uani 1 1 d . . . C23 C -0.0472(5) 0.9427(3) 0.6562(3) 0.0568(9) Uani 1 1 d . . . H23B H -0.0987 0.9877 0.5935 0.085 Uiso 1 1 calc R . . H23C H -0.1437 0.9429 0.7079 0.085 Uiso 1 1 calc R . . H23A H -0.0072 0.8738 0.6476 0.085 Uiso 1 1 calc R . . C24 C 0.3581(5) 0.9713(3) 0.6075(2) 0.0529(8) Uani 1 1 d . . . H24A H 0.3826 0.9016 0.5999 0.079 Uiso 1 1 calc R . . H24C H 0.4700 0.9852 0.6344 0.079 Uiso 1 1 calc R . . H24B H 0.3272 1.0183 0.5426 0.079 Uiso 1 1 calc R . . C25 C 0.0928(4) 1.1222(2) 0.6979(2) 0.0444(7) Uani 1 1 d . . . H25A H 0.0477 1.1632 0.6323 0.067 Uiso 1 1 calc R . . H25C H 0.2027 1.1451 0.7164 0.067 Uiso 1 1 calc R . . H25B H -0.0068 1.1294 0.7470 0.067 Uiso 1 1 calc R . . C26 C 0.3360(4) 0.55007(19) 1.26236(19) 0.0298(5) Uani 1 1 d . . . C27 C 0.3397(4) 0.4844(2) 1.3381(2) 0.0363(6) Uani 1 1 d . . . C28 C 0.2279(7) 0.2837(3) 1.3981(3) 0.0799(14) Uani 1 1 d . . . H28B H 0.0955 0.3155 1.3870 0.120 Uiso 1 1 calc R . . H28C H 0.2378 0.2200 1.4491 0.120 Uiso 1 1 calc R . . H28A H 0.2832 0.2700 1.3360 0.120 Uiso 1 1 calc R . . C29 C 0.6087(5) 0.3123(3) 1.4592(3) 0.0591(9) Uani 1 1 d . . . H29B H 0.6214 0.2471 1.5082 0.089 Uiso 1 1 calc R . . H29C H 0.6732 0.3577 1.4835 0.089 Uiso 1 1 calc R . . H29A H 0.6647 0.3019 1.3962 0.089 Uiso 1 1 calc R . . C30 C 0.2483(5) 0.4006(3) 1.5549(2) 0.0561(9) Uani 1 1 d . . . H30A H 0.1168 0.4335 1.5421 0.084 Uiso 1 1 calc R . . H30C H 0.3168 0.4464 1.5759 0.084 Uiso 1 1 calc R . . H30B H 0.2549 0.3382 1.6074 0.084 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 S1 0.0381(4) 0.0358(4) 0.0302(3) -0.0091(3) 0.0018(3) -0.0097(3) Si1 0.0389(4) 0.0312(4) 0.0280(4) -0.0032(3) -0.0018(3) -0.0109(3) Si2 0.0556(5) 0.0300(4) 0.0334(4) 0.0032(3) -0.0070(4) -0.0141(4) C1 0.0233(12) 0.0329(13) 0.0358(14) -0.0107(11) 0.0043(11) -0.0039(11) C2 0.0294(14) 0.0420(15) 0.0441(16) -0.0203(13) 0.0043(12) -0.0081(12) C3 0.0314(14) 0.0317(14) 0.0555(18) -0.0186(13) 0.0048(13) -0.0089(12) C4 0.0306(14) 0.0298(13) 0.0515(18) -0.0070(13) 0.0030(13) -0.0046(11) C5 0.0305(14) 0.0300(13) 0.0396(15) -0.0065(12) 0.0012(12) -0.0045(11) C6 0.0215(12) 0.0285(12) 0.0373(14) -0.0107(11) 0.0018(10) -0.0053(10) C7 0.0226(12) 0.0247(12) 0.0340(13) -0.0055(10) 0.0013(10) -0.0034(10) C8 0.0249(12) 0.0250(12) 0.0297(13) -0.0002(10) 0.0003(10) -0.0035(10) C9 0.0211(12) 0.0251(12) 0.0293(13) -0.0017(10) -0.0006(10) -0.0049(10) C10 0.0237(12) 0.0261(12) 0.0279(12) -0.0011(10) -0.0017(10) -0.0049(10) C11 0.0215(12) 0.0257(12) 0.0319(13) -0.0037(10) -0.0006(10) -0.0054(10) C12 0.0285(13) 0.0337(13) 0.0301(13) -0.0041(11) -0.0018(11) -0.0039(11) C13 0.0332(14) 0.0348(14) 0.0380(15) -0.0118(12) -0.0038(12) -0.0058(12) C14 0.0321(14) 0.0251(12) 0.0474(16) -0.0089(12) 0.0000(12) -0.0074(11) C15 0.0327(14) 0.0256(12) 0.0368(14) -0.0018(11) -0.0014(11) -0.0062(11) C16 0.0197(11) 0.0248(12) 0.0337(13) -0.0032(10) 0.0009(10) -0.0036(10) C17 0.0222(12) 0.0242(11) 0.0308(13) 0.0014(10) -0.0010(10) -0.0053(10) C18 0.0202(12) 0.0266(12) 0.0298(13) -0.0021(10) -0.0003(10) -0.0035(10) C19 0.0262(13) 0.0283(12) 0.0266(12) -0.0017(10) 0.0004(10) -0.0045(10) C20 0.0256(12) 0.0303(13) 0.0300(13) -0.0058(11) 0.0016(10) -0.0064(10) C21 0.0310(13) 0.0264(12) 0.0333(14) -0.0035(11) 0.0004(11) -0.0095(11) C22 0.0408(16) 0.0305(13) 0.0356(15) -0.0024(12) -0.0017(12) -0.0111(12) C23 0.059(2) 0.066(2) 0.051(2) -0.0118(17) -0.0158(17) -0.0255(18) C24 0.062(2) 0.0536(19) 0.0432(18) -0.0131(15) 0.0095(16) -0.0103(17) C25 0.0421(17) 0.0327(14) 0.0539(19) -0.0018(14) -0.0029(14) -0.0067(13) C26 0.0285(13) 0.0293(13) 0.0322(13) -0.0065(11) -0.0025(11) -0.0072(11) C27 0.0461(17) 0.0294(13) 0.0329(14) -0.0017(11) -0.0069(12) -0.0116(12) C28 0.119(4) 0.052(2) 0.073(3) 0.0020(19) -0.027(3) -0.042(2) C29 0.072(2) 0.0483(19) 0.0458(19) 0.0011(15) -0.0028(17) 0.0005(18) C30 0.058(2) 0.057(2) 0.0406(18) 0.0054(16) -0.0032(16) 0.0009(17) _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 S1 C20 1.748(3) . ? S1 C1 1.759(3) . ? Si1 C22 1.836(3) . ? Si1 C25 1.848(3) . ? Si1 C24 1.856(3) . ? Si1 C23 1.864(3) . ? Si2 C27 1.835(3) . ? Si2 C28 1.854(4) . ? Si2 C30 1.855(3) . ? Si2 C29 1.863(4) . ? C1 C2 1.392(4) . ? C1 C6 1.402(4) . ? C2 C3 1.383(4) . ? C2 H2 0.9500 . ? C3 C4 1.396(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? C5 C6 1.392(4) . ? C5 H5 0.9500 . ? C6 C7 1.457(3) . ? C7 C8 1.362(3) . ? C7 C20 1.432(3) . ? C8 C9 1.421(3) . ? C8 H8 0.9500 . ? C9 C10 1.417(3) . ? C9 C18 1.440(3) . ? C10 C11 1.411(3) . ? C10 C26 1.434(3) . ? C11 C12 1.419(4) . ? C11 C16 1.431(3) . ? C12 C13 1.362(4) . ? C12 H12 0.9500 . ? C13 C14 1.410(4) . ? C13 H13 0.9500 . ? C14 C15 1.355(4) . ? C14 H14 0.9500 . ? C15 C16 1.425(3) . ? C15 H15 0.9500 . ? C16 C17 1.410(4) . ? C17 C18 1.417(3) . ? C17 C21 1.435(3) . ? C18 C19 1.419(3) . ? C19 C20 1.368(3) . ? C19 H19 0.9500 . ? C21 C22 1.201(4) . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23 H23A 0.9800 . ? C24 H24A 0.9800 . ? C24 H24C 0.9800 . ? C24 H24B 0.9800 . ? C25 H25A 0.9800 . ? C25 H25C 0.9800 . ? C25 H25B 0.9800 . ? C26 C27 1.207(4) . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C28 H28A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C29 H29A 0.9800 . ? C30 H30A 0.9800 . ? C30 H30C 0.9800 . ? C30 H30B 0.9800 . ? 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 C20 S1 C1 91.36(12) . . ? C22 Si1 C25 110.20(14) . . ? C22 Si1 C24 107.91(15) . . ? C25 Si1 C24 110.07(15) . . ? C22 Si1 C23 107.07(15) . . ? C25 Si1 C23 110.47(16) . . ? C24 Si1 C23 111.04(17) . . ? C27 Si2 C28 106.75(15) . . ? C27 Si2 C30 110.98(15) . . ? C28 Si2 C30 110.3(2) . . ? C27 Si2 C29 107.37(15) . . ? C28 Si2 C29 110.4(2) . . ? C30 Si2 C29 110.86(16) . . ? C2 C1 C6 121.4(2) . . ? C2 C1 S1 125.7(2) . . ? C6 C1 S1 112.93(19) . . ? C3 C2 C1 118.0(3) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? C2 C3 C4 121.3(3) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 119.6(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C1 119.4(2) . . ? C5 C6 C7 128.7(2) . . ? C1 C6 C7 111.9(2) . . ? C8 C7 C20 119.6(2) . . ? C8 C7 C6 128.7(2) . . ? C20 C7 C6 111.7(2) . . ? C7 C8 C9 120.9(2) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 121.1(2) . . ? C10 C9 C18 119.7(2) . . ? C8 C9 C18 119.2(2) . . ? C11 C10 C9 120.7(2) . . ? C11 C10 C26 120.2(2) . . ? C9 C10 C26 119.0(2) . . ? C10 C11 C12 121.5(2) . . ? C10 C11 C16 119.8(2) . . ? C12 C11 C16 118.7(2) . . ? C13 C12 C11 121.0(2) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 120.3(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 120.7(2) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 121.0(2) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 122.2(2) . . ? C17 C16 C11 119.6(2) . . ? C15 C16 C11 118.3(2) . . ? C16 C17 C18 121.3(2) . . ? C16 C17 C21 120.3(2) . . ? C18 C17 C21 118.4(2) . . ? C17 C18 C19 122.1(2) . . ? C17 C18 C9 118.9(2) . . ? C19 C18 C9 119.0(2) . . ? C20 C19 C18 119.8(2) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C7 121.6(2) . . ? C19 C20 S1 126.3(2) . . ? C7 C20 S1 112.13(18) . . ? C22 C21 C17 175.4(3) . . ? C21 C22 Si1 171.7(2) . . ? Si1 C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C23 H23A 109.5 . . ? H23B C23 H23A 109.5 . . ? H23C C23 H23A 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? H24C C24 H24B 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? C27 C26 C10 177.0(3) . . ? C26 C27 Si2 170.4(2) . . ? Si2 C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C28 H28A 109.5 . . ? H28B C28 H28A 109.5 . . ? H28C C28 H28A 109.5 . . ? Si2 C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? H30C C30 H30B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 S1 C1 C2 179.3(2) . . . . ? C20 S1 C1 C6 0.1(2) . . . . ? C6 C1 C2 C3 -0.4(4) . . . . ? S1 C1 C2 C3 -179.6(2) . . . . ? C1 C2 C3 C4 0.5(4) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? C4 C5 C6 C1 -0.1(4) . . . . ? C4 C5 C6 C7 178.8(3) . . . . ? C2 C1 C6 C5 0.2(4) . . . . ? S1 C1 C6 C5 179.50(19) . . . . ? C2 C1 C6 C7 -178.9(2) . . . . ? S1 C1 C6 C7 0.4(3) . . . . ? C5 C6 C7 C8 -0.5(4) . . . . ? C1 C6 C7 C8 178.5(2) . . . . ? C5 C6 C7 C20 -179.8(2) . . . . ? C1 C6 C7 C20 -0.7(3) . . . . ? C20 C7 C8 C9 0.4(4) . . . . ? C6 C7 C8 C9 -178.8(2) . . . . ? C7 C8 C9 C10 178.3(2) . . . . ? C7 C8 C9 C18 -0.9(4) . . . . ? C8 C9 C10 C11 178.3(2) . . . . ? C18 C9 C10 C11 -2.5(4) . . . . ? C8 C9 C10 C26 -2.6(4) . . . . ? C18 C9 C10 C26 176.7(2) . . . . ? C9 C10 C11 C12 -177.8(2) . . . . ? C26 C10 C11 C12 3.1(4) . . . . ? C9 C10 C11 C16 2.3(4) . . . . ? C26 C10 C11 C16 -176.9(2) . . . . ? C10 C11 C12 C13 179.1(2) . . . . ? C16 C11 C12 C13 -0.9(4) . . . . ? C11 C12 C13 C14 0.6(4) . . . . ? C12 C13 C14 C15 0.5(4) . . . . ? C13 C14 C15 C16 -1.2(4) . . . . ? C14 C15 C16 C17 -179.2(2) . . . . ? C14 C15 C16 C11 0.9(4) . . . . ? C10 C11 C16 C17 0.2(3) . . . . ? C12 C11 C16 C17 -179.8(2) . . . . ? C10 C11 C16 C15 -179.9(2) . . . . ? C12 C11 C16 C15 0.1(3) . . . . ? C15 C16 C17 C18 177.7(2) . . . . ? C11 C16 C17 C18 -2.4(4) . . . . ? C15 C16 C17 C21 -4.9(4) . . . . ? C11 C16 C17 C21 175.0(2) . . . . ? C16 C17 C18 C19 -179.1(2) . . . . ? C21 C17 C18 C19 3.4(4) . . . . ? C16 C17 C18 C9 2.2(4) . . . . ? C21 C17 C18 C9 -175.3(2) . . . . ? C10 C9 C18 C17 0.3(3) . . . . ? C8 C9 C18 C17 179.5(2) . . . . ? C10 C9 C18 C19 -178.5(2) . . . . ? C8 C9 C18 C19 0.8(3) . . . . ? C17 C18 C19 C20 -178.8(2) . . . . ? C9 C18 C19 C20 -0.1(4) . . . . ? C18 C19 C20 C7 -0.5(4) . . . . ? C18 C19 C20 S1 178.25(19) . . . . ? C8 C7 C20 C19 0.3(4) . . . . ? C6 C7 C20 C19 179.7(2) . . . . ? C8 C7 C20 S1 -178.56(19) . . . . ? C6 C7 C20 S1 0.8(3) . . . . ? C1 S1 C20 C19 -179.3(2) . . . . ? C1 S1 C20 C7 -0.48(19) . . . . ? C16 C17 C21 C22 -140(4) . . . . ? C18 C17 C21 C22 37(4) . . . . ? C17 C21 C22 Si1 -15(5) . . . . ? C25 Si1 C22 C21 139.4(18) . . . . ? C24 Si1 C22 C21 -100.4(18) . . . . ? C23 Si1 C22 C21 19.2(18) . . . . ? C11 C10 C26 C27 179(100) . . . . ? C9 C10 C26 C27 0(6) . . . . ? C10 C26 C27 Si2 23(7) . . . . ? C28 Si2 C27 C26 -45.3(16) . . . . ? C30 Si2 C27 C26 -165.6(15) . . . . ? C29 Si2 C27 C26 73.1(16) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.391 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.061 _database_code_depnum_ccdc_archive 'CCDC 942189' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a _audit_creation_date 2013-03-18 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H52 S Si2' _chemical_formula_sum 'C42 H52 S Si2' _chemical_formula_weight 645.08 _chemical_melting_point ? 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.241(2) _cell_length_b 15.168(3) _cell_length_c 20.461(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.260(3) _cell_angle_gamma 90.00 _cell_volume 3793.0(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12450 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.4841 _cell_measurement_theta_min 1.3425 _exptl_absorpt_coefficient_mu 0.176 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7511 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.130 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1392 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_unetI/netI 0.0460 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 33167 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 2.69 _diffrn_ambient_temperature 446(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 7969 _reflns_number_total 8672 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _refine_diff_density_max 0.697 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.052 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.231 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 418 _refine_ls_number_reflns 8672 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0812 _refine_ls_restrained_S_all 1.231 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+3.3127P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1584 _refine_ls_wR_factor_ref 0.1628 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 H2 H -0.3569 0.5510 0.0000 0.052 Uiso 1 1 calc R . . H3 H -0.3943 0.4248 0.0604 0.056 Uiso 1 1 calc R . . H4 H -0.2591 0.3586 0.1277 0.054 Uiso 1 1 calc R . . H5 H -0.0821 0.4164 0.1363 0.046 Uiso 1 1 calc R . . H9 H 0.0600 0.7437 -0.0096 0.039 Uiso 1 1 calc R . . H13 H 0.4604 0.7997 0.0234 0.044 Uiso 1 1 calc R . . H14 H 0.6279 0.7608 0.0704 0.049 Uiso 1 1 calc R . . H15 H 0.6449 0.6421 0.1448 0.047 Uiso 1 1 calc R . . H16 H 0.4944 0.5594 0.1672 0.040 Uiso 1 1 calc R . . H20 H 0.0969 0.4952 0.1287 0.034 Uiso 1 1 calc R . . H23 H 0.4812 0.3580 0.2962 0.040 Uiso 1 1 calc R . . H24A H 0.5711 0.2922 0.1806 0.072 Uiso 1 1 calc R . . H24B H 0.5441 0.3942 0.1917 0.072 Uiso 1 1 calc R . . H24C H 0.6352 0.3459 0.2382 0.072 Uiso 1 1 calc R . . H25A H 0.5076 0.1781 0.2606 0.068 Uiso 1 1 calc R . . H25B H 0.4511 0.2102 0.3251 0.068 Uiso 1 1 calc R . . H25C H 0.5782 0.2292 0.3169 0.068 Uiso 1 1 calc R . . H26 H 0.2207 0.2487 0.1410 0.042 Uiso 1 1 calc R . . H27A H 0.3377 0.1973 0.0663 0.071 Uiso 1 1 calc R . . H27B H 0.3779 0.2944 0.0866 0.071 Uiso 1 1 calc R . . H27C H 0.4420 0.2102 0.1162 0.071 Uiso 1 1 calc R . . H28A H 0.2563 0.0993 0.1518 0.071 Uiso 1 1 calc R . . H28B H 0.2354 0.1387 0.2225 0.071 Uiso 1 1 calc R . . H28C H 0.3574 0.1176 0.2030 0.071 Uiso 1 1 calc R . . H29 H 0.2435 0.2534 0.3138 0.043 Uiso 1 1 calc R . . H30A H 0.2550 0.4413 0.3219 0.079 Uiso 1 1 calc R . . H30B H 0.2020 0.3808 0.3758 0.079 Uiso 1 1 calc R . . H30C H 0.3299 0.3737 0.3645 0.079 Uiso 1 1 calc R . . H31A H 0.0997 0.2701 0.2331 0.088 Uiso 1 1 calc R . . H31B H 0.1032 0.3749 0.2422 0.088 Uiso 1 1 calc R . . H31C H 0.0657 0.3132 0.3004 0.088 Uiso 1 1 calc R . . H34 H 0.3976 0.8919 -0.1567 0.051 Uiso 1 1 calc R . . H35A H 0.3226 0.9840 -0.2400 0.109 Uiso 1 1 calc R . . H35B H 0.4505 1.0037 -0.2272 0.109 Uiso 1 1 calc R . . H35C H 0.3621 1.0695 -0.1993 0.109 Uiso 1 1 calc R . . H36A H 0.4730 0.9491 -0.0570 0.090 Uiso 1 1 calc R . . H36B H 0.5421 0.9794 -0.1171 0.090 Uiso 1 1 calc R . . H36C H 0.4599 1.0471 -0.0854 0.090 Uiso 1 1 calc R . . H37 H 0.2950 1.0743 -0.0430 0.071 Uiso 1 1 calc R . . H38A H 0.1080 1.1122 -0.1254 0.103 Uiso 1 1 calc R . . H38B H 0.2317 1.1379 -0.1383 0.103 Uiso 1 1 calc R . . H38C H 0.1716 1.1830 -0.0794 0.103 Uiso 1 1 calc R . . H39A H 0.1975 1.0047 0.0306 0.150 Uiso 1 1 calc R . . H39B H 0.0856 1.0263 -0.0105 0.150 Uiso 1 1 calc R . . H39C H 0.1572 1.1046 0.0222 0.150 Uiso 1 1 calc R . . H40 H 0.1328 0.9636 -0.2047 0.066 Uiso 1 1 calc R . . H41A H 0.1645 0.7832 -0.1669 0.107 Uiso 1 1 calc R . . H41B H 0.1031 0.8141 -0.2341 0.107 Uiso 1 1 calc R . . H41C H 0.2311 0.8331 -0.2208 0.107 Uiso 1 1 calc R . . H42A H 0.0194 0.8731 -0.1059 0.139 Uiso 1 1 calc R . . H42B H -0.0342 0.8973 -0.1768 0.139 Uiso 1 1 calc R . . H42C H 0.0009 0.9741 -0.1263 0.139 Uiso 1 1 calc R . . C1 C -0.1960(2) 0.55872(18) 0.03342(13) 0.0356(6) Uani 1 1 d . . . C2 C -0.3014(2) 0.5241(2) 0.02765(15) 0.0431(7) Uani 1 1 d . . . C3 C -0.3229(3) 0.4494(2) 0.06339(16) 0.0466(8) Uani 1 1 d . . . C4 C -0.2422(2) 0.4098(2) 0.10354(15) 0.0448(7) Uani 1 1 d . . . C5 C -0.1371(2) 0.44393(19) 0.10879(14) 0.0386(6) Uani 1 1 d . . . C6 C -0.1132(2) 0.51915(17) 0.07329(13) 0.0329(6) Uani 1 1 d . . . C7 C -0.0092(2) 0.56510(16) 0.07033(12) 0.0292(5) Uani 1 1 d . . . C8 C -0.0184(2) 0.64062(17) 0.02837(12) 0.0315(6) Uani 1 1 d . . . C9 C 0.0688(2) 0.69340(17) 0.01784(13) 0.0325(6) Uani 1 1 d . . . C10 C 0.1729(2) 0.67287(16) 0.04810(12) 0.0289(5) Uani 1 1 d . . . C11 C 0.2669(2) 0.72334(16) 0.03557(12) 0.0303(5) Uani 1 1 d . . . C12 C 0.3699(2) 0.70161(16) 0.06510(12) 0.0293(5) Uani 1 1 d . . . C13 C 0.4659(2) 0.75059(18) 0.05217(14) 0.0368(6) Uani 1 1 d . . . C14 C 0.5648(2) 0.72799(19) 0.08036(14) 0.0409(7) Uani 1 1 d . . . C15 C 0.5754(2) 0.65620(19) 0.12446(14) 0.0395(6) Uani 1 1 d . . . C16 C 0.4864(2) 0.60761(18) 0.13765(13) 0.0337(6) Uani 1 1 d . . . C17 C 0.3809(2) 0.62741(16) 0.10808(12) 0.0280(5) Uani 1 1 d . . . C18 C 0.2885(2) 0.57483(16) 0.11904(12) 0.0279(5) Uani 1 1 d . . . C19 C 0.1840(2) 0.59703(16) 0.09025(12) 0.0274(5) Uani 1 1 d . . . C20 C 0.0905(2) 0.54492(16) 0.10048(12) 0.0283(5) Uani 1 1 d . . . C21 C 0.3017(2) 0.49503(16) 0.15643(12) 0.0297(5) Uani 1 1 d . . . C22 C 0.3144(2) 0.42581(17) 0.18461(13) 0.0327(6) Uani 1 1 d . . . C23 C 0.4769(2) 0.31280(18) 0.26052(13) 0.0337(6) Uani 1 1 d . . . C24 C 0.5647(2) 0.3386(2) 0.21351(16) 0.0482(8) Uani 1 1 d . . . C25 C 0.5061(2) 0.2247(2) 0.29379(16) 0.0454(7) Uani 1 1 d . . . C26 C 0.2953(2) 0.23235(17) 0.15958(13) 0.0349(6) Uani 1 1 d . . . C27 C 0.3699(3) 0.2337(2) 0.10199(14) 0.0475(7) Uani 1 1 d . . . C28 C 0.2852(3) 0.13851(19) 0.18669(16) 0.0474(8) Uani 1 1 d . . . C29 C 0.2338(2) 0.31188(18) 0.29168(13) 0.0355(6) Uani 1 1 d . . . C30 C 0.2573(3) 0.3833(2) 0.34308(16) 0.0525(8) Uani 1 1 d . . . C31 C 0.1149(3) 0.3181(3) 0.26438(18) 0.0586(9) Uani 1 1 d . . . C32 C 0.2581(2) 0.79643(17) -0.00899(13) 0.0335(6) Uani 1 1 d . . . C33 C 0.2529(2) 0.85748(19) -0.04652(14) 0.0394(6) Uani 1 1 d . . . C34 C 0.3794(2) 0.9539(2) -0.14475(15) 0.0427(7) Uani 1 1 d . . . C35 C 0.3786(3) 1.0077(3) -0.20860(19) 0.0728(12) Uani 1 1 d . . . C36 C 0.4719(3) 0.9852(2) -0.09674(19) 0.0601(9) Uani 1 1 d . . . C37 C 0.2201(3) 1.0549(2) -0.05885(18) 0.0593(9) Uani 1 1 d . . . C38 C 0.1792(3) 1.1286(2) -0.1046(2) 0.0689(11) Uani 1 1 d . . . C39 C 0.1601(5) 1.0470(3) 0.0008(2) 0.1003(17) Uani 1 1 d . . . C40 C 0.1340(3) 0.9179(2) -0.16943(18) 0.0552(9) Uani 1 1 d . . . C41 C 0.1606(3) 0.8290(3) -0.20063(19) 0.0710(11) Uani 1 1 d . . . C42 C 0.0197(3) 0.9153(3) -0.1421(3) 0.0924(15) Uani 1 1 d . . . Si1 Si 0.33234(6) 0.31707(5) 0.22457(3) 0.02871(17) Uani 1 1 d . . . Si2 Si 0.24430(7) 0.94912(5) -0.10599(4) 0.0379(2) Uani 1 1 d . . . S1 S -0.15109(6) 0.65283(5) -0.00752(4) 0.03991(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0372(14) 0.0358(14) 0.0346(14) -0.0097(12) 0.0091(11) 0.0017(12) C2 0.0367(15) 0.0503(18) 0.0425(16) -0.0157(14) 0.0051(12) 0.0021(13) C3 0.0388(16) 0.0524(18) 0.0498(18) -0.0178(15) 0.0131(14) -0.0082(14) C4 0.0467(17) 0.0450(17) 0.0444(17) -0.0080(14) 0.0177(14) -0.0098(14) C5 0.0414(15) 0.0404(15) 0.0349(14) -0.0042(12) 0.0095(12) -0.0039(13) C6 0.0372(14) 0.0325(13) 0.0299(13) -0.0074(11) 0.0092(11) -0.0005(11) C7 0.0369(14) 0.0264(12) 0.0250(12) -0.0039(10) 0.0060(10) 0.0024(11) C8 0.0368(14) 0.0297(13) 0.0280(13) -0.0026(10) 0.0015(11) 0.0062(11) C9 0.0425(15) 0.0253(12) 0.0295(13) 0.0041(10) 0.0014(11) 0.0026(11) C10 0.0383(14) 0.0243(12) 0.0248(12) 0.0010(10) 0.0072(10) 0.0020(10) C11 0.0421(15) 0.0222(12) 0.0270(12) 0.0013(10) 0.0062(11) 0.0010(11) C12 0.0385(14) 0.0238(12) 0.0259(12) -0.0027(10) 0.0055(10) -0.0006(10) C13 0.0448(16) 0.0286(13) 0.0377(15) 0.0024(11) 0.0083(12) -0.0053(12) C14 0.0395(16) 0.0388(15) 0.0454(16) -0.0020(13) 0.0117(13) -0.0100(13) C15 0.0387(15) 0.0395(15) 0.0404(15) -0.0065(13) 0.0038(12) -0.0014(12) C16 0.0402(15) 0.0306(13) 0.0305(13) -0.0009(11) 0.0034(11) 0.0015(12) C17 0.0341(13) 0.0237(12) 0.0269(12) -0.0023(10) 0.0068(10) 0.0020(10) C18 0.0365(13) 0.0243(12) 0.0234(12) -0.0002(10) 0.0063(10) 0.0024(10) C19 0.0362(13) 0.0218(11) 0.0244(12) -0.0027(9) 0.0040(10) 0.0003(10) C20 0.0375(14) 0.0220(11) 0.0260(12) 0.0006(10) 0.0062(10) 0.0011(10) C21 0.0333(13) 0.0266(12) 0.0294(13) 0.0008(10) 0.0041(10) 0.0016(10) C22 0.0340(14) 0.0292(13) 0.0354(14) 0.0036(11) 0.0063(11) 0.0011(11) C23 0.0324(14) 0.0333(14) 0.0353(14) 0.0050(11) 0.0012(11) -0.0018(11) C24 0.0360(16) 0.0523(19) 0.0566(19) 0.0135(16) 0.0059(14) -0.0037(14) C25 0.0418(16) 0.0391(16) 0.0544(19) 0.0139(14) -0.0055(14) 0.0023(13) C26 0.0376(14) 0.0310(13) 0.0360(14) 0.0029(11) -0.0005(11) 0.0039(11) C27 0.0527(19) 0.0519(18) 0.0376(16) -0.0023(14) 0.0018(14) 0.0071(15) C28 0.058(2) 0.0324(15) 0.0509(18) -0.0016(13) -0.0034(15) -0.0046(14) C29 0.0402(15) 0.0282(13) 0.0390(15) 0.0065(11) 0.0109(12) 0.0016(11) C30 0.077(2) 0.0384(16) 0.0442(18) -0.0026(14) 0.0247(17) -0.0036(16) C31 0.0393(17) 0.075(2) 0.063(2) 0.0122(19) 0.0176(16) 0.0053(17) C32 0.0393(15) 0.0299(13) 0.0313(13) 0.0032(11) 0.0035(11) -0.0024(11) C33 0.0470(17) 0.0347(15) 0.0367(15) 0.0052(12) 0.0052(12) -0.0025(13) C34 0.0481(17) 0.0362(15) 0.0440(16) 0.0073(13) 0.0055(13) -0.0043(13) C35 0.076(3) 0.079(3) 0.065(2) 0.034(2) 0.022(2) -0.006(2) C36 0.048(2) 0.054(2) 0.078(3) -0.0091(19) 0.0031(18) -0.0088(16) C37 0.075(2) 0.0453(19) 0.058(2) 0.0098(16) 0.0114(18) 0.0177(18) C38 0.084(3) 0.0418(19) 0.078(3) 0.0038(18) -0.023(2) 0.0131(19) C39 0.159(5) 0.065(3) 0.081(3) -0.012(2) 0.034(3) 0.005(3) C40 0.0455(18) 0.058(2) 0.061(2) 0.0256(17) -0.0092(15) -0.0045(16) C41 0.077(3) 0.076(3) 0.058(2) 0.003(2) -0.020(2) -0.016(2) C42 0.048(2) 0.094(3) 0.134(4) 0.019(3) -0.002(2) -0.011(2) Si1 0.0317(4) 0.0244(3) 0.0303(4) 0.0059(3) 0.0043(3) 0.0007(3) Si2 0.0449(5) 0.0316(4) 0.0374(4) 0.0125(3) 0.0043(3) 0.0024(3) S1 0.0382(4) 0.0379(4) 0.0430(4) 0.0004(3) -0.0029(3) 0.0041(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.392(4) . ? C1 C6 1.400(4) . ? C2 H2 0.9500 . ? C2 C3 1.381(4) . ? C3 H3 0.9500 . ? C3 C4 1.386(5) . ? C4 H4 0.9500 . ? C4 C5 1.384(4) . ? C5 H5 0.9500 . ? C5 C6 1.393(4) . ? C6 C7 1.456(4) . ? C7 C8 1.432(3) . ? C7 C20 1.370(4) . ? C8 C9 1.361(4) . ? C9 H9 0.9500 . ? C9 C10 1.420(4) . ? C10 C11 1.417(4) . ? C10 C19 1.439(3) . ? C11 C12 1.406(4) . ? C11 C32 1.436(3) . ? C12 C13 1.428(4) . ? C12 C17 1.430(3) . ? C13 H13 0.9500 . ? C13 C14 1.355(4) . ? C14 H14 0.9500 . ? C14 C15 1.415(4) . ? C15 H15 0.9500 . ? C15 C16 1.355(4) . ? C16 H16 0.9500 . ? C16 C17 1.427(4) . ? C17 C18 1.411(3) . ? C18 C19 1.419(4) . ? C18 C21 1.436(3) . ? C19 C20 1.417(3) . ? C20 H20 0.9500 . ? C21 C22 1.204(3) . ? C23 H23 1.0000 . ? C23 C24 1.534(4) . ? C23 C25 1.533(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26 1.0000 . ? C26 C27 1.532(4) . ? C26 C28 1.535(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29 1.0000 . ? C29 C30 1.526(4) . ? C29 C31 1.532(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.202(4) . ? C34 H34 1.0000 . ? C34 C35 1.540(4) . ? C34 C36 1.531(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37 1.0000 . ? C37 C38 1.524(5) . ? C37 C39 1.464(6) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40 1.0000 . ? C40 C41 1.534(5) . ? C40 C42 1.537(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? Si1 C22 1.848(3) . ? Si1 C23 1.878(3) . ? Si1 C26 1.886(3) . ? Si1 C29 1.880(3) . ? Si2 C33 1.846(3) . ? Si2 C34 1.876(3) . ? Si2 C37 1.903(4) . ? Si2 C40 1.880(3) . ? S1 C1 1.759(3) . ? S1 C8 1.754(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 C2 C1 C6 121.7(3) . . ? C2 C1 S1 125.4(2) . . ? C6 C1 S1 112.9(2) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C3 C2 C1 117.9(3) . . ? C2 C3 H3 119.4 . . ? C2 C3 C4 121.3(3) . . ? C4 C3 H3 119.4 . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C5 C4 C3 120.8(3) . . ? C4 C5 H5 120.4 . . ? C4 C5 C6 119.2(3) . . ? C6 C5 H5 120.4 . . ? C1 C6 C7 112.1(2) . . ? C5 C6 C1 119.3(3) . . ? C5 C6 C7 128.6(3) . . ? C8 C7 C6 111.6(2) . . ? C20 C7 C6 129.3(2) . . ? C20 C7 C8 119.1(2) . . ? C7 C8 S1 112.0(2) . . ? C9 C8 C7 122.0(2) . . ? C9 C8 S1 126.0(2) . . ? C8 C9 H9 120.2 . . ? C8 C9 C10 119.6(2) . . ? C10 C9 H9 120.2 . . ? C9 C10 C19 119.2(2) . . ? C11 C10 C9 121.4(2) . . ? C11 C10 C19 119.4(2) . . ? C10 C11 C32 120.0(2) . . ? C12 C11 C10 120.9(2) . . ? C12 C11 C32 119.1(2) . . ? C11 C12 C13 121.7(2) . . ? C11 C12 C17 119.9(2) . . ? C13 C12 C17 118.3(2) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C14 C13 C12 120.9(3) . . ? C13 C14 H14 119.6 . . ? C13 C14 C15 120.9(3) . . ? C15 C14 H14 119.6 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C16 C15 C14 120.0(3) . . ? C15 C16 H16 119.3 . . ? C15 C16 C17 121.3(3) . . ? C17 C16 H16 119.3 . . ? C16 C17 C12 118.5(2) . . ? C18 C17 C12 119.6(2) . . ? C18 C17 C16 121.8(2) . . ? C17 C18 C19 120.8(2) . . ? C17 C18 C21 119.6(2) . . ? C19 C18 C21 119.5(2) . . ? C18 C19 C10 119.4(2) . . ? C20 C19 C10 119.0(2) . . ? C20 C19 C18 121.6(2) . . ? C7 C20 H20 119.5 . . ? C7 C20 C19 121.0(2) . . ? C19 C20 H20 119.5 . . ? C22 C21 C18 176.3(3) . . ? C21 C22 Si1 177.5(2) . . ? C24 C23 H23 105.8 . . ? C24 C23 Si1 115.09(19) . . ? C25 C23 H23 105.8 . . ? C25 C23 C24 110.3(2) . . ? C25 C23 Si1 113.24(19) . . ? Si1 C23 H23 105.8 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24C C24 H24B 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H25B C25 H25A 109.5 . . ? H25B C25 H25C 109.5 . . ? H25C C25 H25A 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? C27 C26 H26 106.1 . . ? C27 C26 C28 110.7(2) . . ? C27 C26 Si1 113.8(2) . . ? C28 C26 H26 106.1 . . ? C28 C26 Si1 113.46(19) . . ? Si1 C26 H26 106.1 . . ? H27B C27 H27A 109.5 . . ? H27C C27 H27A 109.5 . . ? H27C C27 H27B 109.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? C30 C29 H29 107.7 . . ? C30 C29 C31 110.2(3) . . ? C30 C29 Si1 111.7(2) . . ? C31 C29 H29 107.7 . . ? C31 C29 Si1 111.5(2) . . ? Si1 C29 H29 107.7 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30C C30 H30B 109.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H31B C31 H31A 109.5 . . ? H31B C31 H31C 109.5 . . ? H31C C31 H31A 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? C33 C32 C11 178.7(3) . . ? C32 C33 Si2 178.5(3) . . ? C35 C34 H34 106.3 . . ? C35 C34 Si2 114.6(2) . . ? C36 C34 H34 106.3 . . ? C36 C34 C35 110.5(3) . . ? C36 C34 Si2 112.2(2) . . ? Si2 C34 H34 106.3 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H36B C36 H36A 109.5 . . ? H36C C36 H36A 109.5 . . ? H36C C36 H36B 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? C38 C37 H37 104.3 . . ? C38 C37 Si2 111.3(3) . . ? C39 C37 H37 104.3 . . ? C39 C37 C38 114.1(4) . . ? C39 C37 Si2 117.0(3) . . ? Si2 C37 H37 104.3 . . ? H38B C38 H38A 109.5 . . ? H38B C38 H38C 109.5 . . ? H38C C38 H38A 109.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H39B C39 H39A 109.5 . . ? H39B C39 H39C 109.5 . . ? H39C C39 H39A 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? C41 C40 H40 107.7 . . ? C41 C40 C42 110.4(3) . . ? C41 C40 Si2 110.4(2) . . ? C42 C40 H40 107.7 . . ? C42 C40 Si2 112.9(3) . . ? Si2 C40 H40 107.7 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41C C41 H41B 109.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H42B C42 H42A 109.5 . . ? H42B C42 H42C 109.5 . . ? H42C C42 H42A 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? C22 Si1 C23 106.82(12) . . ? C22 Si1 C26 106.17(12) . . ? C22 Si1 C29 107.20(12) . . ? C23 Si1 C26 115.87(13) . . ? C23 Si1 C29 109.97(13) . . ? C29 Si1 C26 110.35(13) . . ? C33 Si2 C34 106.82(14) . . ? C33 Si2 C37 107.77(14) . . ? C33 Si2 C40 106.08(14) . . ? C34 Si2 C37 110.35(16) . . ? C34 Si2 C40 109.50(15) . . ? C40 Si2 C37 115.85(17) . . ? C8 S1 C1 91.28(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 -0.3(4) . . . . ? C1 C6 C7 C8 1.3(3) . . . . ? C1 C6 C7 C20 -177.7(2) . . . . ? C1 S1 C8 C7 0.61(19) . . . . ? C1 S1 C8 C9 179.0(2) . . . . ? C2 C1 C6 C5 -0.9(4) . . . . ? C2 C1 C6 C7 178.3(2) . . . . ? C2 C3 C4 C5 -0.2(4) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? C4 C5 C6 C1 0.3(4) . . . . ? C4 C5 C6 C7 -178.8(3) . . . . ? C5 C6 C7 C8 -179.6(3) . . . . ? C5 C6 C7 C20 1.4(4) . . . . ? C6 C1 C2 C3 0.8(4) . . . . ? C6 C7 C8 C9 -179.6(2) . . . . ? C6 C7 C8 S1 -1.2(3) . . . . ? C6 C7 C20 C19 178.4(2) . . . . ? C7 C8 C9 C10 1.2(4) . . . . ? C8 C7 C20 C19 -0.6(4) . . . . ? C8 C9 C10 C11 176.5(2) . . . . ? C8 C9 C10 C19 -0.9(4) . . . . ? C8 S1 C1 C2 -179.0(2) . . . . ? C8 S1 C1 C6 0.1(2) . . . . ? C9 C10 C11 C12 -179.1(2) . . . . ? C9 C10 C11 C32 -0.6(4) . . . . ? C9 C10 C19 C18 178.2(2) . . . . ? C9 C10 C19 C20 -0.1(3) . . . . ? C10 C11 C12 C13 178.8(2) . . . . ? C10 C11 C12 C17 0.4(4) . . . . ? C10 C11 C32 C33 -156(14) . . . . ? C10 C19 C20 C7 0.8(3) . . . . ? C11 C10 C19 C18 0.7(3) . . . . ? C11 C10 C19 C20 -177.5(2) . . . . ? C11 C12 C13 C14 -179.1(3) . . . . ? C11 C12 C17 C16 -179.5(2) . . . . ? C11 C12 C17 C18 1.9(3) . . . . ? C11 C32 C33 Si2 84(18) . . . . ? C12 C11 C32 C33 23(14) . . . . ? C12 C13 C14 C15 -1.3(4) . . . . ? C12 C17 C18 C19 -2.9(3) . . . . ? C12 C17 C18 C21 173.3(2) . . . . ? C13 C12 C17 C16 2.0(3) . . . . ? C13 C12 C17 C18 -176.6(2) . . . . ? C13 C14 C15 C16 1.8(4) . . . . ? C14 C15 C16 C17 -0.3(4) . . . . ? C15 C16 C17 C12 -1.6(4) . . . . ? C15 C16 C17 C18 177.0(2) . . . . ? C16 C17 C18 C19 178.6(2) . . . . ? C16 C17 C18 C21 -5.3(4) . . . . ? C17 C12 C13 C14 -0.6(4) . . . . ? C17 C18 C19 C10 1.6(3) . . . . ? C17 C18 C19 C20 179.8(2) . . . . ? C17 C18 C21 C22 -82(4) . . . . ? C18 C19 C20 C7 -177.4(2) . . . . ? C18 C21 C22 Si1 -32(9) . . . . ? C19 C10 C11 C12 -1.7(4) . . . . ? C19 C10 C11 C32 176.8(2) . . . . ? C19 C18 C21 C22 94(4) . . . . ? C20 C7 C8 C9 -0.5(4) . . . . ? C20 C7 C8 S1 177.97(19) . . . . ? C21 C18 C19 C10 -174.6(2) . . . . ? C21 C18 C19 C20 3.6(4) . . . . ? C22 Si1 C23 C24 -49.9(2) . . . . ? C22 Si1 C23 C25 -178.1(2) . . . . ? C22 Si1 C26 C27 62.7(2) . . . . ? C22 Si1 C26 C28 -169.5(2) . . . . ? C22 Si1 C29 C30 -61.4(2) . . . . ? C22 Si1 C29 C31 62.5(2) . . . . ? C23 Si1 C22 C21 123(6) . . . . ? C23 Si1 C26 C27 -55.7(2) . . . . ? C23 Si1 C26 C28 72.1(2) . . . . ? C23 Si1 C29 C30 54.4(2) . . . . ? C23 Si1 C29 C31 178.3(2) . . . . ? C26 Si1 C22 C21 -1(6) . . . . ? C26 Si1 C23 C24 68.1(2) . . . . ? C26 Si1 C23 C25 -60.1(2) . . . . ? C26 Si1 C29 C30 -176.6(2) . . . . ? C26 Si1 C29 C31 -52.7(2) . . . . ? C29 Si1 C22 C21 -119(6) . . . . ? C29 Si1 C23 C24 -165.9(2) . . . . ? C29 Si1 C23 C25 65.9(2) . . . . ? C29 Si1 C26 C27 178.53(19) . . . . ? C29 Si1 C26 C28 -53.7(2) . . . . ? C32 C11 C12 C13 0.3(4) . . . . ? C32 C11 C12 C17 -178.1(2) . . . . ? C33 Si2 C34 C35 163.6(3) . . . . ? C33 Si2 C34 C36 -69.4(3) . . . . ? C33 Si2 C37 C38 -163.4(3) . . . . ? C33 Si2 C37 C39 -29.8(4) . . . . ? C33 Si2 C40 C41 -57.1(3) . . . . ? C33 Si2 C40 C42 66.9(3) . . . . ? C34 Si2 C33 C32 -77(10) . . . . ? C34 Si2 C37 C38 80.3(3) . . . . ? C34 Si2 C37 C39 -146.1(4) . . . . ? C34 Si2 C40 C41 57.8(3) . . . . ? C34 Si2 C40 C42 -178.1(3) . . . . ? C37 Si2 C33 C32 164(10) . . . . ? C37 Si2 C34 C35 -79.6(3) . . . . ? C37 Si2 C34 C36 47.5(3) . . . . ? C37 Si2 C40 C41 -176.6(2) . . . . ? C37 Si2 C40 C42 -52.6(3) . . . . ? C40 Si2 C33 C32 40(10) . . . . ? C40 Si2 C34 C35 49.1(3) . . . . ? C40 Si2 C34 C36 176.1(2) . . . . ? C40 Si2 C37 C38 -44.8(3) . . . . ? C40 Si2 C37 C39 88.8(4) . . . . ? S1 C1 C2 C3 179.9(2) . . . . ? S1 C1 C6 C5 179.9(2) . . . . ? S1 C1 C6 C7 -0.9(3) . . . . ? S1 C8 C9 C10 -177.02(19) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 942190' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H52 S Si2' _chemical_formula_sum 'C42 H52 S Si2' _chemical_formula_weight 645.08 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' S S 0.1246 0.1234 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.545(2) _cell_length_b 17.738(4) _cell_length_c 25.019(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.907(4) _cell_angle_gamma 90.00 _cell_volume 3791.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10912 _cell_measurement_theta_min 1.4073 _cell_measurement_theta_max 27.4773 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7292 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25390 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8638 _reflns_number_gt 7329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _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^)+(0.0342P)^2^+4.4420P] 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 8638 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0985 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1742 _refine_ls_goodness_of_fit_ref 1.234 _refine_ls_restrained_S_all 1.234 _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 S1 S 0.93422(11) 0.27450(6) 0.04704(4) 0.0448(3) Uani 1 1 d . . . Si1 Si 0.52196(10) 0.70946(5) 0.16259(4) 0.0287(2) Uani 1 1 d . . . Si2 Si 0.26003(10) 0.06176(5) 0.10735(4) 0.0302(2) Uani 1 1 d . . . C1 C 1.0426(4) 0.3584(2) 0.04330(15) 0.0412(9) Uani 1 1 d . . . C2 C 1.1909(4) 0.3654(3) 0.02189(16) 0.0539(11) Uani 1 1 d . . . H2 H 1.2425 0.3230 0.0071 0.065 Uiso 1 1 calc R . . C3 C 1.2619(4) 0.4356(3) 0.02257(17) 0.0571(12) Uani 1 1 d . . . H3 H 1.3628 0.4413 0.0077 0.069 Uiso 1 1 calc R . . C4 C 1.1883(4) 0.4976(3) 0.04458(16) 0.0515(11) Uani 1 1 d . . . H4 H 1.2393 0.5452 0.0448 0.062 Uiso 1 1 calc R . . C5 C 1.0403(4) 0.4906(2) 0.06635(14) 0.0420(9) Uani 1 1 d . . . H5 H 0.9907 0.5333 0.0816 0.050 Uiso 1 1 calc R . . C6 C 0.9658(4) 0.4216(2) 0.06581(13) 0.0340(8) Uani 1 1 d . . . C7 C 0.8114(4) 0.40027(19) 0.08507(13) 0.0310(7) Uani 1 1 d . . . C8 C 0.7784(4) 0.32199(19) 0.07769(13) 0.0320(7) Uani 1 1 d . . . C9 C 0.6415(4) 0.28993(18) 0.09358(13) 0.0310(7) Uani 1 1 d . . . H9 H 0.6236 0.2376 0.0884 0.037 Uiso 1 1 calc R . . C10 C 0.5257(4) 0.33567(17) 0.11803(12) 0.0272(7) Uani 1 1 d . . . C11 C 0.3818(4) 0.30478(17) 0.13498(13) 0.0274(7) Uani 1 1 d . . . C12 C 0.2694(4) 0.35047(17) 0.16090(12) 0.0274(7) Uani 1 1 d . . . C13 C 0.1253(4) 0.32051(19) 0.17934(14) 0.0340(8) Uani 1 1 d . . . H13 H 0.1041 0.2683 0.1751 0.041 Uiso 1 1 calc R . . C14 C 0.0177(4) 0.3655(2) 0.20287(15) 0.0396(8) Uani 1 1 d . . . H14 H -0.0778 0.3445 0.2149 0.048 Uiso 1 1 calc R . . C15 C 0.0470(4) 0.4436(2) 0.20958(14) 0.0394(8) Uani 1 1 d . . . H15 H -0.0290 0.4747 0.2260 0.047 Uiso 1 1 calc R . . C16 C 0.1828(4) 0.47433(19) 0.19273(14) 0.0344(8) Uani 1 1 d . . . H16 H 0.2009 0.5267 0.1976 0.041 Uiso 1 1 calc R . . C17 C 0.2992(4) 0.42915(17) 0.16772(12) 0.0277(7) Uani 1 1 d . . . C18 C 0.4395(4) 0.46077(17) 0.14893(12) 0.0259(7) Uani 1 1 d . . . C19 C 0.5549(3) 0.41472(17) 0.12518(12) 0.0264(7) Uani 1 1 d . . . C20 C 0.6999(4) 0.44538(18) 0.10819(13) 0.0300(7) Uani 1 1 d . . . H20 H 0.7200 0.4977 0.1128 0.036 Uiso 1 1 calc R . . C21 C 0.4646(4) 0.54036(18) 0.15295(13) 0.0299(7) Uani 1 1 d . . . C22 C 0.4821(4) 0.60763(18) 0.15639(14) 0.0328(7) Uani 1 1 d . . . C23 C 0.7395(4) 0.7192(2) 0.15247(16) 0.0407(9) Uani 1 1 d . . . H23 H 0.7613 0.7003 0.1157 0.049 Uiso 1 1 calc R . . C24 C 0.7940(5) 0.8019(2) 0.1545(2) 0.0622(13) Uani 1 1 d . . . H24A H 0.7310 0.8319 0.1293 0.093 Uiso 1 1 calc R . . H24B H 0.9044 0.8047 0.1448 0.093 Uiso 1 1 calc R . . H24C H 0.7811 0.8216 0.1908 0.093 Uiso 1 1 calc R . . C25 C 0.8357(4) 0.6709(2) 0.1913(2) 0.0582(12) Uani 1 1 d . . . H25C H 0.8205 0.6888 0.2279 0.087 Uiso 1 1 calc R . . H25B H 0.9468 0.6744 0.1824 0.087 Uiso 1 1 calc R . . H25A H 0.8017 0.6182 0.1885 0.087 Uiso 1 1 calc R . . C26 C 0.4630(4) 0.74156(18) 0.23137(14) 0.0338(7) Uani 1 1 d . . . H26 H 0.5546 0.7319 0.2558 0.041 Uiso 1 1 calc R . . C27 C 0.3241(5) 0.6989(2) 0.25473(16) 0.0472(10) Uani 1 1 d . . . H27B H 0.2293 0.7102 0.2337 0.071 Uiso 1 1 calc R . . H27C H 0.3093 0.7147 0.2919 0.071 Uiso 1 1 calc R . . H27A H 0.3448 0.6446 0.2536 0.071 Uiso 1 1 calc R . . C28 C 0.4315(5) 0.82691(19) 0.23309(15) 0.0426(9) Uani 1 1 d . . . H28B H 0.5234 0.8541 0.2203 0.064 Uiso 1 1 calc R . . H28C H 0.4103 0.8422 0.2699 0.064 Uiso 1 1 calc R . . H28A H 0.3407 0.8388 0.2102 0.064 Uiso 1 1 calc R . . C29 C 0.4078(4) 0.75929(19) 0.10780(13) 0.0345(8) Uani 1 1 d . . . H29 H 0.4259 0.8146 0.1125 0.041 Uiso 1 1 calc R . . C30 C 0.4646(5) 0.7381(2) 0.05194(15) 0.0521(10) Uani 1 1 d . . . H30A H 0.4537 0.6836 0.0467 0.078 Uiso 1 1 calc R . . H30C H 0.5747 0.7525 0.0485 0.078 Uiso 1 1 calc R . . H30B H 0.4015 0.7648 0.0249 0.078 Uiso 1 1 calc R . . C31 C 0.2320(4) 0.7458(3) 0.11144(16) 0.0538(11) Uani 1 1 d . . . H31B H 0.1779 0.7725 0.0822 0.081 Uiso 1 1 calc R . . H31C H 0.1947 0.7647 0.1458 0.081 Uiso 1 1 calc R . . H31A H 0.2104 0.6917 0.1086 0.081 Uiso 1 1 calc R . . C32 C 0.3471(4) 0.22644(18) 0.12629(13) 0.0298(7) Uani 1 1 d . . . C33 C 0.3134(4) 0.16134(18) 0.11806(14) 0.0331(8) Uani 1 1 d . . . C34 C 0.0464(4) 0.0486(2) 0.12046(17) 0.0440(9) Uani 1 1 d . . . H34 H -0.0095 0.0576 0.0856 0.053 Uiso 1 1 calc R . . C35 C -0.0228(5) 0.1035(2) 0.1599(2) 0.0600(13) Uani 1 1 d . . . H35A H -0.1343 0.0925 0.1642 0.090 Uiso 1 1 calc R . . H35B H -0.0103 0.1551 0.1466 0.090 Uiso 1 1 calc R . . H35C H 0.0315 0.0984 0.1945 0.090 Uiso 1 1 calc R . . C36 C 0.0088(4) -0.0334(2) 0.13670(18) 0.0509(11) Uani 1 1 d . . . H36A H 0.0478 -0.0681 0.1094 0.076 Uiso 1 1 calc R . . H36B H -0.1047 -0.0395 0.1398 0.076 Uiso 1 1 calc R . . H36C H 0.0596 -0.0448 0.1712 0.076 Uiso 1 1 calc R . . C37 C 0.3028(5) 0.0397(2) 0.03470(15) 0.0452(9) Uani 1 1 d . . . H37 H 0.4184 0.0450 0.0305 0.054 Uiso 1 1 calc R . . C38 C 0.2269(6) 0.0953(3) -0.00332(17) 0.0662(13) Uani 1 1 d . . . H38B H 0.2557 0.0830 -0.0401 0.099 Uiso 1 1 calc R . . H38C H 0.2629 0.1463 0.0054 0.099 Uiso 1 1 calc R . . H38A H 0.1129 0.0927 0.0000 0.099 Uiso 1 1 calc R . . C39 C 0.2622(5) -0.0419(2) 0.02033(17) 0.0551(11) Uani 1 1 d . . . H39A H 0.1495 -0.0499 0.0243 0.083 Uiso 1 1 calc R . . H39C H 0.3198 -0.0761 0.0442 0.083 Uiso 1 1 calc R . . H39B H 0.2914 -0.0518 -0.0167 0.083 Uiso 1 1 calc R . . C40 C 0.3887(4) 0.0043(2) 0.15286(15) 0.0383(8) Uani 1 1 d . . . H40 H 0.3563 -0.0497 0.1490 0.046 Uiso 1 1 calc R . . C41 C 0.5601(5) 0.0096(3) 0.1384(2) 0.0647(13) Uani 1 1 d . . . H41A H 0.5756 -0.0129 0.1031 0.097 Uiso 1 1 calc R . . H41C H 0.6236 -0.0176 0.1651 0.097 Uiso 1 1 calc R . . H41B H 0.5920 0.0626 0.1378 0.097 Uiso 1 1 calc R . . C42 C 0.3680(5) 0.0265(2) 0.21195(16) 0.0542(11) Uani 1 1 d . . . H42B H 0.3911 0.0803 0.2164 0.081 Uiso 1 1 calc R . . H42C H 0.4399 -0.0031 0.2345 0.081 Uiso 1 1 calc R . . H42A H 0.2600 0.0166 0.2225 0.081 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 S1 0.0382(5) 0.0497(6) 0.0466(6) -0.0058(5) 0.0051(4) 0.0098(4) Si1 0.0302(4) 0.0203(4) 0.0356(5) 0.0007(4) 0.0013(4) -0.0025(4) Si2 0.0275(4) 0.0235(5) 0.0396(5) -0.0019(4) 0.0013(4) -0.0044(4) C1 0.0327(18) 0.056(2) 0.035(2) 0.0068(18) -0.0009(15) 0.0017(17) C2 0.037(2) 0.084(3) 0.041(2) 0.009(2) 0.0074(18) 0.011(2) C3 0.0282(19) 0.098(4) 0.045(2) 0.017(2) 0.0037(17) -0.004(2) C4 0.0328(19) 0.078(3) 0.043(2) 0.021(2) -0.0038(17) -0.012(2) C5 0.0320(18) 0.058(2) 0.036(2) 0.0083(18) -0.0037(15) -0.0077(17) C6 0.0225(15) 0.052(2) 0.0278(17) 0.0109(16) 0.0000(13) -0.0007(15) C7 0.0284(16) 0.0345(18) 0.0299(17) 0.0047(14) -0.0023(14) -0.0010(14) C8 0.0299(16) 0.0374(19) 0.0286(17) 0.0004(15) -0.0026(14) 0.0053(14) C9 0.0355(17) 0.0244(16) 0.0329(18) -0.0017(14) -0.0036(14) -0.0004(13) C10 0.0311(16) 0.0246(16) 0.0258(16) -0.0009(13) -0.0012(13) -0.0027(13) C11 0.0309(16) 0.0217(15) 0.0295(17) 0.0040(13) -0.0023(13) -0.0016(12) C12 0.0302(16) 0.0251(16) 0.0268(16) 0.0038(13) -0.0027(13) -0.0038(13) C13 0.0322(17) 0.0309(18) 0.039(2) 0.0035(15) 0.0017(15) -0.0099(14) C14 0.0330(18) 0.048(2) 0.038(2) 0.0033(17) 0.0059(16) -0.0071(16) C15 0.0417(19) 0.041(2) 0.036(2) -0.0045(16) 0.0094(16) 0.0023(16) C16 0.0367(18) 0.0310(18) 0.0356(19) -0.0038(15) 0.0026(15) -0.0010(14) C17 0.0329(16) 0.0248(16) 0.0252(16) 0.0009(13) -0.0025(13) -0.0003(13) C18 0.0298(16) 0.0198(15) 0.0280(16) 0.0017(13) -0.0019(13) -0.0031(12) C19 0.0266(15) 0.0259(16) 0.0266(16) 0.0034(13) -0.0046(13) -0.0033(12) C20 0.0345(17) 0.0258(17) 0.0298(17) 0.0048(14) -0.0022(14) -0.0014(13) C21 0.0300(16) 0.0268(17) 0.0329(18) -0.0015(14) 0.0008(14) -0.0014(13) C22 0.0323(17) 0.0284(18) 0.0378(19) 0.0014(15) 0.0023(15) -0.0023(14) C23 0.0378(19) 0.0329(19) 0.051(2) 0.0043(17) 0.0011(17) -0.0045(15) C24 0.041(2) 0.042(2) 0.104(4) 0.015(2) -0.002(2) -0.0133(18) C25 0.032(2) 0.050(3) 0.092(4) 0.013(2) -0.004(2) -0.0026(18) C26 0.0404(18) 0.0279(17) 0.0330(18) 0.0019(14) -0.0022(15) 0.0019(14) C27 0.055(2) 0.045(2) 0.041(2) 0.0031(18) 0.0111(19) -0.0003(19) C28 0.061(2) 0.0294(19) 0.038(2) -0.0043(16) 0.0010(18) 0.0010(17) C29 0.0425(19) 0.0300(18) 0.0309(18) 0.0010(14) 0.0006(15) 0.0050(15) C30 0.064(3) 0.059(3) 0.033(2) -0.0025(19) 0.0013(19) 0.004(2) C31 0.044(2) 0.073(3) 0.044(2) 0.003(2) -0.0076(18) 0.008(2) C32 0.0277(16) 0.0304(17) 0.0313(17) 0.0003(14) -0.0004(13) -0.0025(13) C33 0.0300(16) 0.0270(17) 0.042(2) -0.0033(15) 0.0021(15) -0.0035(13) C34 0.0335(18) 0.040(2) 0.058(3) -0.0031(18) 0.0058(18) -0.0072(16) C35 0.042(2) 0.049(3) 0.089(4) -0.017(2) 0.026(2) -0.0093(19) C36 0.043(2) 0.036(2) 0.075(3) -0.005(2) 0.014(2) -0.0131(17) C37 0.049(2) 0.047(2) 0.040(2) -0.0035(18) -0.0002(18) -0.0070(18) C38 0.088(4) 0.068(3) 0.043(3) 0.009(2) 0.006(2) -0.001(3) C39 0.060(3) 0.052(3) 0.053(3) -0.020(2) 0.006(2) -0.013(2) C40 0.042(2) 0.0281(18) 0.044(2) -0.0038(16) -0.0047(17) 0.0011(15) C41 0.043(2) 0.067(3) 0.084(4) 0.003(3) -0.001(2) 0.016(2) C42 0.074(3) 0.042(2) 0.046(2) -0.0031(19) -0.009(2) -0.003(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 S1 C1 1.757(4) . ? S1 C8 1.761(3) . ? Si1 C22 1.844(3) . ? Si1 C23 1.888(4) . ? Si1 C26 1.889(3) . ? Si1 C29 1.889(3) . ? Si2 C33 1.843(3) . ? Si2 C40 1.872(4) . ? Si2 C34 1.874(4) . ? Si2 C37 1.901(4) . ? C1 C2 1.389(5) . ? C1 C6 1.420(5) . ? C2 C3 1.384(6) . ? C2 H2 0.9500 . ? C3 C4 1.386(6) . ? C3 H3 0.9500 . ? C4 C5 1.390(5) . ? C4 H4 0.9500 . ? C5 C6 1.379(5) . ? C5 H5 0.9500 . ? C6 C7 1.462(4) . ? C7 C20 1.379(4) . ? C7 C8 1.428(5) . ? C8 C9 1.366(4) . ? C9 C10 1.425(4) . ? C9 H9 0.9500 . ? C10 C11 1.418(4) . ? C10 C19 1.435(4) . ? C11 C12 1.421(4) . ? C11 C32 1.437(4) . ? C12 C13 1.425(4) . ? C12 C17 1.428(4) . ? C13 C14 1.359(5) . ? C13 H13 0.9500 . ? C14 C15 1.418(5) . ? C14 H14 0.9500 . ? C15 C16 1.355(5) . ? C15 H15 0.9500 . ? C16 C17 1.429(4) . ? C16 H16 0.9500 . ? C17 C18 1.411(4) . ? C18 C19 1.418(4) . ? C18 C21 1.431(4) . ? C19 C20 1.424(4) . ? C20 H20 0.9500 . ? C21 C22 1.206(4) . ? C23 C25 1.527(5) . ? C23 C24 1.538(5) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25C 0.9800 . ? C25 H25B 0.9800 . ? C25 H25A 0.9800 . ? C26 C27 1.531(5) . ? C26 C28 1.538(4) . ? C26 H26 1.0000 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 H27A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C28 H28A 0.9800 . ? C29 C31 1.526(5) . ? C29 C30 1.533(5) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30C 0.9800 . ? C30 H30B 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C31 H31A 0.9800 . ? C32 C33 1.207(4) . ? C34 C35 1.513(5) . ? C34 C36 1.547(5) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.510(6) . ? C37 C39 1.528(5) . ? C37 H37 1.0000 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C38 H38A 0.9800 . ? C39 H39A 0.9800 . ? C39 H39C 0.9800 . ? C39 H39B 0.9800 . ? C40 C41 1.518(5) . ? C40 C42 1.543(5) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41C 0.9800 . ? C41 H41B 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C42 H42A 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C8 91.19(17) . . ? C22 Si1 C23 105.05(15) . . ? C22 Si1 C26 108.69(15) . . ? C23 Si1 C26 111.84(17) . . ? C22 Si1 C29 107.74(16) . . ? C23 Si1 C29 110.95(16) . . ? C26 Si1 C29 112.21(15) . . ? C33 Si2 C40 106.99(16) . . ? C33 Si2 C34 109.45(16) . . ? C40 Si2 C34 112.96(18) . . ? C33 Si2 C37 106.61(16) . . ? C40 Si2 C37 110.44(17) . . ? C34 Si2 C37 110.13(18) . . ? C2 C1 C6 120.8(4) . . ? C2 C1 S1 125.5(3) . . ? C6 C1 S1 113.6(3) . . ? C3 C2 C1 118.5(4) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 121.2(4) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.8(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 119.2(3) . . ? C5 C6 C7 130.2(3) . . ? C1 C6 C7 110.6(3) . . ? C20 C7 C8 118.8(3) . . ? C20 C7 C6 128.4(3) . . ? C8 C7 C6 112.8(3) . . ? C9 C8 C7 122.4(3) . . ? C9 C8 S1 125.8(3) . . ? C7 C8 S1 111.8(2) . . ? C8 C9 C10 119.5(3) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 121.3(3) . . ? C11 C10 C19 119.4(3) . . ? C9 C10 C19 119.3(3) . . ? C10 C11 C12 120.8(3) . . ? C10 C11 C32 120.4(3) . . ? C12 C11 C32 118.8(3) . . ? C11 C12 C13 121.9(3) . . ? C11 C12 C17 119.4(3) . . ? C13 C12 C17 118.6(3) . . ? C14 C13 C12 121.0(3) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 120.4(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.5(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 121.1(3) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C18 C17 C12 119.9(3) . . ? C18 C17 C16 121.6(3) . . ? C12 C17 C16 118.4(3) . . ? C17 C18 C19 120.7(3) . . ? C17 C18 C21 119.7(3) . . ? C19 C18 C21 119.6(3) . . ? C18 C19 C20 121.3(3) . . ? C18 C19 C10 119.6(3) . . ? C20 C19 C10 119.1(3) . . ? C7 C20 C19 120.9(3) . . ? C7 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C18 178.5(3) . . ? C21 C22 Si1 176.4(3) . . ? C25 C23 C24 110.8(3) . . ? C25 C23 Si1 112.6(3) . . ? C24 C23 Si1 112.4(3) . . ? C25 C23 H23 106.9 . . ? C24 C23 H23 106.9 . . ? Si1 C23 H23 106.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25C 109.5 . . ? C23 C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? C23 C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? H25B C25 H25A 109.5 . . ? C27 C26 C28 109.8(3) . . ? C27 C26 Si1 114.7(2) . . ? C28 C26 Si1 111.8(2) . . ? C27 C26 H26 106.7 . . ? C28 C26 H26 106.7 . . ? Si1 C26 H26 106.7 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C27 H27A 109.5 . . ? H27B C27 H27A 109.5 . . ? H27C C27 H27A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C28 H28A 109.5 . . ? H28B C28 H28A 109.5 . . ? H28C C28 H28A 109.5 . . ? C31 C29 C30 110.0(3) . . ? C31 C29 Si1 112.4(2) . . ? C30 C29 Si1 112.3(2) . . ? C31 C29 H29 107.3 . . ? C30 C29 H29 107.3 . . ? Si1 C29 H29 107.3 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? H30C C30 H30B 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C31 H31A 109.5 . . ? H31B C31 H31A 109.5 . . ? H31C C31 H31A 109.5 . . ? C33 C32 C11 177.8(4) . . ? C32 C33 Si2 178.4(3) . . ? C35 C34 C36 110.4(3) . . ? C35 C34 Si2 115.2(3) . . ? C36 C34 Si2 111.7(3) . . ? C35 C34 H34 106.3 . . ? C36 C34 H34 106.3 . . ? Si2 C34 H34 106.3 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 112.1(4) . . ? C38 C37 Si2 112.4(3) . . ? C39 C37 Si2 112.0(3) . . ? C38 C37 H37 106.6 . . ? C39 C37 H37 106.6 . . ? Si2 C37 H37 106.6 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C38 H38A 109.5 . . ? H38B C38 H38A 109.5 . . ? H38C C38 H38A 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? H39C C39 H39B 109.5 . . ? C41 C40 C42 109.7(3) . . ? C41 C40 Si2 112.4(3) . . ? C42 C40 Si2 111.6(3) . . ? C41 C40 H40 107.6 . . ? C42 C40 H40 107.6 . . ? Si2 C40 H40 107.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? H41C C41 H41B 109.5 . . ? C40 C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C42 H42A 109.5 . . ? H42B C42 H42A 109.5 . . ? H42C C42 H42A 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 S1 C1 C2 -179.9(3) . . . . ? C8 S1 C1 C6 1.4(3) . . . . ? C6 C1 C2 C3 -0.5(6) . . . . ? S1 C1 C2 C3 -179.1(3) . . . . ? C1 C2 C3 C4 0.7(6) . . . . ? C2 C3 C4 C5 -0.3(6) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? C4 C5 C6 C1 0.5(5) . . . . ? C4 C5 C6 C7 -178.9(3) . . . . ? C2 C1 C6 C5 -0.1(5) . . . . ? S1 C1 C6 C5 178.7(3) . . . . ? C2 C1 C6 C7 179.4(3) . . . . ? S1 C1 C6 C7 -1.8(4) . . . . ? C5 C6 C7 C20 1.1(6) . . . . ? C1 C6 C7 C20 -178.4(3) . . . . ? C5 C6 C7 C8 -179.2(3) . . . . ? C1 C6 C7 C8 1.4(4) . . . . ? C20 C7 C8 C9 -1.2(5) . . . . ? C6 C7 C8 C9 179.0(3) . . . . ? C20 C7 C8 S1 179.4(3) . . . . ? C6 C7 C8 S1 -0.4(4) . . . . ? C1 S1 C8 C9 -179.9(3) . . . . ? C1 S1 C8 C7 -0.6(3) . . . . ? C7 C8 C9 C10 0.6(5) . . . . ? S1 C8 C9 C10 179.9(3) . . . . ? C8 C9 C10 C11 179.8(3) . . . . ? C8 C9 C10 C19 0.4(5) . . . . ? C9 C10 C11 C12 177.9(3) . . . . ? C19 C10 C11 C12 -2.7(5) . . . . ? C9 C10 C11 C32 -2.0(5) . . . . ? C19 C10 C11 C32 177.4(3) . . . . ? C10 C11 C12 C13 -178.6(3) . . . . ? C32 C11 C12 C13 1.3(5) . . . . ? C10 C11 C12 C17 2.8(5) . . . . ? C32 C11 C12 C17 -177.3(3) . . . . ? C11 C12 C13 C14 -178.4(3) . . . . ? C17 C12 C13 C14 0.2(5) . . . . ? C12 C13 C14 C15 -0.1(5) . . . . ? C13 C14 C15 C16 -0.1(6) . . . . ? C14 C15 C16 C17 0.2(6) . . . . ? C11 C12 C17 C18 -0.2(5) . . . . ? C13 C12 C17 C18 -178.8(3) . . . . ? C11 C12 C17 C16 178.5(3) . . . . ? C13 C12 C17 C16 -0.1(5) . . . . ? C15 C16 C17 C18 178.6(3) . . . . ? C15 C16 C17 C12 -0.1(5) . . . . ? C12 C17 C18 C19 -2.6(5) . . . . ? C16 C17 C18 C19 178.8(3) . . . . ? C12 C17 C18 C21 176.2(3) . . . . ? C16 C17 C18 C21 -2.4(5) . . . . ? C17 C18 C19 C20 -177.2(3) . . . . ? C21 C18 C19 C20 4.0(5) . . . . ? C17 C18 C19 C10 2.8(5) . . . . ? C21 C18 C19 C10 -176.0(3) . . . . ? C11 C10 C19 C18 -0.1(4) . . . . ? C9 C10 C19 C18 179.3(3) . . . . ? C11 C10 C19 C20 179.8(3) . . . . ? C9 C10 C19 C20 -0.7(4) . . . . ? C8 C7 C20 C19 0.8(5) . . . . ? C6 C7 C20 C19 -179.5(3) . . . . ? C18 C19 C20 C7 -179.9(3) . . . . ? C10 C19 C20 C7 0.1(5) . . . . ? C17 C18 C21 C22 -22(14) . . . . ? C19 C18 C21 C22 157(13) . . . . ? C18 C21 C22 Si1 165(100) . . . . ? C23 Si1 C22 C21 21(5) . . . . ? C26 Si1 C22 C21 -99(5) . . . . ? C29 Si1 C22 C21 139(5) . . . . ? C22 Si1 C23 C25 -55.9(3) . . . . ? C26 Si1 C23 C25 61.8(3) . . . . ? C29 Si1 C23 C25 -172.0(3) . . . . ? C22 Si1 C23 C24 178.2(3) . . . . ? C26 Si1 C23 C24 -64.1(3) . . . . ? C29 Si1 C23 C24 62.0(3) . . . . ? C22 Si1 C26 C27 -32.1(3) . . . . ? C23 Si1 C26 C27 -147.6(3) . . . . ? C29 Si1 C26 C27 87.0(3) . . . . ? C22 Si1 C26 C28 -157.9(2) . . . . ? C23 Si1 C26 C28 86.5(3) . . . . ? C29 Si1 C26 C28 -38.9(3) . . . . ? C22 Si1 C29 C31 59.7(3) . . . . ? C23 Si1 C29 C31 174.1(3) . . . . ? C26 Si1 C29 C31 -59.9(3) . . . . ? C22 Si1 C29 C30 -65.1(3) . . . . ? C23 Si1 C29 C30 49.4(3) . . . . ? C26 Si1 C29 C30 175.3(3) . . . . ? C10 C11 C32 C33 -123(10) . . . . ? C12 C11 C32 C33 57(10) . . . . ? C11 C32 C33 Si2 -101(16) . . . . ? C40 Si2 C33 C32 -66(12) . . . . ? C34 Si2 C33 C32 57(12) . . . . ? C37 Si2 C33 C32 176(100) . . . . ? C33 Si2 C34 C35 -27.8(4) . . . . ? C40 Si2 C34 C35 91.3(3) . . . . ? C37 Si2 C34 C35 -144.7(3) . . . . ? C33 Si2 C34 C36 -154.8(3) . . . . ? C40 Si2 C34 C36 -35.7(3) . . . . ? C37 Si2 C34 C36 88.3(3) . . . . ? C33 Si2 C37 C38 -52.4(3) . . . . ? C40 Si2 C37 C38 -168.3(3) . . . . ? C34 Si2 C37 C38 66.3(3) . . . . ? C33 Si2 C37 C39 -179.6(3) . . . . ? C40 Si2 C37 C39 64.5(3) . . . . ? C34 Si2 C37 C39 -61.0(3) . . . . ? C33 Si2 C40 C41 -65.0(3) . . . . ? C34 Si2 C40 C41 174.5(3) . . . . ? C37 Si2 C40 C41 50.7(3) . . . . ? C33 Si2 C40 C42 58.8(3) . . . . ? C34 Si2 C40 C42 -61.7(3) . . . . ? C37 Si2 C40 C42 174.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.400 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.058 _database_code_depnum_ccdc_archive 'CCDC 942191'