# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_15 _database_code_depnum_ccdc_archive 'CCDC 876925' #TrackingRef 'depYLOBC.cif' _chemical_compound_source 'LOC ETH Zurich' _exptl_crystal_description Cube _exptl_crystal_size_max .39 _exptl_crystal_size_mid .27 _exptl_crystal_size_min .045 _exptl_crystal_F_000 592 _exptl_crystal_colour Colourless _diffrn_ambient_temperature 100 _cell_measurement_temperature 100 _refine_ls_hydrogen_treatment refall # Submission details _diffrn_measurement_device KappaCCD _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.04575 _diffrn_orient_matrix_UB_12 0.08162 _diffrn_orient_matrix_UB_13 -0.05185 _diffrn_orient_matrix_UB_21 -0.00804 _diffrn_orient_matrix_UB_22 -0.03317 _diffrn_orient_matrix_UB_23 -0.05931 _diffrn_orient_matrix_UB_31 -0.07715 _diffrn_orient_matrix_UB_32 0.05745 _diffrn_orient_matrix_UB_33 -0.02167 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 567.758 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z '-X,+Y+ 1/2,-Z' _symmetry_space_group_name_H-M 'P 21 ' _symmetry_cell_setting Monoclinic _chemical_formula_moiety 'C31 H25 N O4 S2 Si ' _chemical_formula_sum 'C31 H25 N O4 S2 Si ' _chemical_name_systematic ; ? ; _cell_length_a 9.5751(3) _cell_length_b 14.6142(5) _cell_length_c 10.3886(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.503(2) _cell_angle_gamma 90.00 _cell_volume 1419.23(8) _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_number 14801 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_min 4.30 _diffrn_reflns_theta_full 27.46 _cell_measurement_reflns_used 38935 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _diffrn_measurement_method CCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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' _exptl_absorpt_coefficient_mu 0.267 _reflns_number_total 5814 _reflns_number_gt 5460 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-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^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.07(5) _refine_ls_number_reflns 5814 _refine_ls_number_parameters 452 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.003 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 0.17349(5) 0.44433(4) 0.86548(5) 0.01965(12) Uani 1 1 d . . . S2 S 0.20244(5) 0.62586(4) 0.75095(5) 0.02139(12) Uani 1 1 d . . . Si3 Si -0.70167(6) 0.31306(5) 0.35012(6) 0.02502(15) Uani 1 1 d . . . O24 O 0.15349(17) 0.35710(12) 0.80216(17) 0.0275(4) Uani 1 1 d . . . O25 O 0.09752(15) 0.46203(11) 0.96758(14) 0.0225(3) Uani 1 1 d . . . O26 O 0.34314(16) 0.61460(12) 0.72776(14) 0.0253(3) Uani 1 1 d . . . O27 O 0.10066(17) 0.68231(12) 0.66450(15) 0.0279(4) Uani 1 1 d . . . N28 N 0.12515(19) 0.52167(14) 0.74307(18) 0.0225(4) Uani 1 1 d . . . C4 C 0.4048(2) 0.54342(15) 0.9959(2) 0.0183(4) Uani 1 1 d . . . C5 C 0.3572(2) 0.46588(15) 0.9233(2) 0.0200(4) Uani 1 1 d . . . C6 C 0.4500(2) 0.39768(17) 0.8929(2) 0.0258(5) Uani 1 1 d . . . C7 C 0.5929(2) 0.40658(17) 0.9401(2) 0.0276(5) Uani 1 1 d . . . C8 C 0.7991(2) 0.49297(18) 1.0659(2) 0.0281(5) Uani 1 1 d . . . C9 C 0.8544(3) 0.56858(18) 1.1356(3) 0.0302(5) Uani 1 1 d . . . C10 C 0.7631(3) 0.63960(17) 1.1574(2) 0.0291(5) Uani 1 1 d . . . C11 C 0.6179(2) 0.63300(16) 1.1117(2) 0.0241(4) Uani 1 1 d . . . C12 C 0.5559(2) 0.55457(15) 1.0423(2) 0.0193(4) Uani 1 1 d . . . C13 C 0.6496(2) 0.48370(17) 1.0166(2) 0.0231(4) Uani 1 1 d . . . C14 C 0.3020(2) 0.61538(15) 1.01969(19) 0.0178(4) Uani 1 1 d . . . C15 C 0.2101(2) 0.65847(16) 0.9157(2) 0.0201(4) Uani 1 1 d . . . C16 C 0.1084(2) 0.72423(15) 0.9343(2) 0.0232(5) Uani 1 1 d . . . C17 C 0.1000(2) 0.74930(17) 1.0584(2) 0.0239(4) Uani 1 1 d . . . C18 C 0.1828(3) 0.73445(17) 1.2998(2) 0.0283(5) Uani 1 1 d . . . C19 C 0.2666(3) 0.69311(17) 1.4065(2) 0.0283(5) Uani 1 1 d . . . C20 C 0.3602(3) 0.62241(18) 1.3893(2) 0.0284(5) Uani 1 1 d . . . C21 C 0.3722(2) 0.59545(16) 1.2649(2) 0.0229(4) Uani 1 1 d . . . C22 C 0.2910(2) 0.63956(15) 1.1519(2) 0.0197(4) Uani 1 1 d . . . C23 C 0.1913(2) 0.70811(16) 1.1698(2) 0.0214(4) Uani 1 1 d . . . C29 C -0.0193(2) 0.50632(17) 0.6675(2) 0.0232(5) Uani 1 1 d . . . C30 C -0.1372(2) 0.52208(17) 0.7209(2) 0.0251(5) Uani 1 1 d . . . C31 C -0.2718(2) 0.49493(17) 0.6519(2) 0.0261(5) Uani 1 1 d . . . C32 C -0.2877(2) 0.45167(17) 0.5303(2) 0.0258(5) Uani 1 1 d . . . C33 C -0.1680(3) 0.4395(2) 0.4753(2) 0.0388(6) Uani 1 1 d . . . C34 C -0.0340(3) 0.4662(2) 0.5446(2) 0.0381(7) Uani 1 1 d . . . C35 C -0.4235(3) 0.41331(18) 0.4651(2) 0.0290(5) Uani 1 1 d . . . C36 C -0.5341(3) 0.37613(18) 0.4151(2) 0.0303(5) Uani 1 1 d . . . C37 C -0.7417(3) 0.2452(2) 0.4897(3) 0.0385(6) Uani 1 1 d . . . C38 C -0.8455(3) 0.39816(19) 0.2895(2) 0.0287(5) Uani 1 1 d . . . C39 C -0.6724(3) 0.2409(2) 0.2107(3) 0.0367(6) Uani 1 1 d . . . H6 H 0.409(3) 0.344(2) 0.845(3) 0.033(7) Uiso 1 1 d . . . H7 H 0.658(3) 0.358(2) 0.929(3) 0.030(7) Uiso 1 1 d . . . H8 H 0.854(3) 0.444(3) 1.051(3) 0.046(9) Uiso 1 1 d . . . H9 H 0.958(3) 0.570(2) 1.173(3) 0.030(7) Uiso 1 1 d . . . H11 H 0.565(3) 0.679(2) 1.129(2) 0.020(6) Uiso 1 1 d . . . H16 H 0.048(4) 0.760(3) 0.861(3) 0.050(9) Uiso 1 1 d . . . H17 H 0.031(3) 0.793(2) 1.063(2) 0.025(7) Uiso 1 1 d . . . H18 H 0.115(3) 0.785(2) 1.309(3) 0.034(7) Uiso 1 1 d . . . H19 H 0.257(3) 0.710(2) 1.491(3) 0.032(7) Uiso 1 1 d . . . H21 H 0.436(3) 0.5437(18) 1.254(2) 0.017(6) Uiso 1 1 d . . . H30 H -0.131(3) 0.549(2) 0.796(3) 0.038(8) Uiso 1 1 d . . . H31 H -0.353(3) 0.508(2) 0.688(3) 0.029(7) Uiso 1 1 d . . . H33 H -0.182(4) 0.411(3) 0.385(4) 0.064(11) Uiso 1 1 d . . . H34 H 0.060(3) 0.452(3) 0.518(3) 0.051(9) Uiso 1 1 d . . . H37A H -0.753(3) 0.284(2) 0.559(3) 0.036(8) Uiso 1 1 d . . . H37B H -0.831(4) 0.200(3) 0.463(3) 0.050(9) Uiso 1 1 d . . . H37C H -0.666(4) 0.200(3) 0.530(4) 0.068(11) Uiso 1 1 d . . . H38A H -0.834(3) 0.456(2) 0.344(3) 0.034(8) Uiso 1 1 d . . . H38B H -0.942(4) 0.375(3) 0.283(3) 0.051(9) Uiso 1 1 d . . . H38C H -0.849(4) 0.412(3) 0.197(4) 0.061(11) Uiso 1 1 d . . . H39A H -0.638(3) 0.293(3) 0.144(3) 0.049(9) Uiso 1 1 d . . . H39B H -0.762(4) 0.210(3) 0.174(3) 0.054(10) Uiso 1 1 d . . . H39C H -0.602(4) 0.194(3) 0.248(3) 0.054(10) Uiso 1 1 d . . . H10 H 0.798(4) 0.697(3) 1.200(3) 0.055(10) Uiso 1 1 d . . . H20 H 0.421(3) 0.597(2) 1.461(3) 0.044(9) Uiso 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 S1 0.0170(2) 0.0184(2) 0.0233(2) 0.0002(2) 0.00388(18) -0.0024(2) S2 0.0199(2) 0.0228(3) 0.0209(2) 0.0033(2) 0.00324(18) -0.0029(2) Si3 0.0201(3) 0.0255(3) 0.0270(3) -0.0010(2) -0.0002(2) -0.0016(2) O24 0.0248(8) 0.0218(8) 0.0344(9) -0.0049(7) 0.0028(7) -0.0050(7) O25 0.0179(7) 0.0267(9) 0.0241(7) 0.0039(6) 0.0072(6) -0.0007(6) O26 0.0230(7) 0.0293(9) 0.0250(7) 0.0032(6) 0.0081(6) -0.0046(7) O27 0.0271(8) 0.0309(10) 0.0231(7) 0.0087(7) 0.0000(6) -0.0017(7) N28 0.0188(8) 0.0261(10) 0.0216(8) 0.0023(7) 0.0020(7) -0.0024(8) C4 0.0184(9) 0.0171(10) 0.0201(9) 0.0035(8) 0.0056(7) 0.0003(8) C5 0.0175(9) 0.0193(11) 0.0232(10) 0.0007(8) 0.0040(8) 0.0000(8) C6 0.0242(11) 0.0220(12) 0.0322(12) -0.0065(9) 0.0081(9) -0.0005(9) C7 0.0225(11) 0.0218(11) 0.0401(13) -0.0036(10) 0.0105(10) 0.0056(9) C8 0.0200(11) 0.0249(13) 0.0403(13) 0.0007(10) 0.0089(9) 0.0046(9) C9 0.0186(11) 0.0288(13) 0.0422(14) 0.0055(10) 0.0048(10) -0.0022(10) C10 0.0239(11) 0.0227(12) 0.0395(12) 0.0000(10) 0.0039(9) -0.0044(10) C11 0.0220(10) 0.0165(11) 0.0336(11) 0.0003(9) 0.0054(8) 0.0001(9) C12 0.0164(9) 0.0189(10) 0.0230(10) 0.0018(8) 0.0052(8) 0.0010(8) C13 0.0178(10) 0.0231(11) 0.0292(11) 0.0008(9) 0.0066(8) 0.0016(9) C14 0.0166(9) 0.0148(10) 0.0221(9) 0.0000(8) 0.0044(7) -0.0008(8) C15 0.0199(10) 0.0170(10) 0.0224(10) -0.0006(8) 0.0023(8) -0.0040(8) C16 0.0179(10) 0.0186(11) 0.0316(12) 0.0034(8) 0.0018(9) 0.0005(8) C17 0.0193(10) 0.0188(10) 0.0349(11) 0.0009(9) 0.0089(9) 0.0028(9) C18 0.0305(12) 0.0242(12) 0.0340(12) -0.0036(9) 0.0152(10) -0.0019(10) C19 0.0366(13) 0.0258(12) 0.0256(11) -0.0043(9) 0.0134(10) -0.0034(11) C20 0.0344(12) 0.0259(12) 0.0241(10) -0.0002(10) 0.0048(9) -0.0019(11) C21 0.0247(11) 0.0209(11) 0.0224(10) 0.0012(8) 0.0034(8) 0.0005(9) C22 0.0177(9) 0.0189(11) 0.0232(10) 0.0009(8) 0.0060(8) -0.0016(8) C23 0.0191(10) 0.0173(10) 0.0293(11) -0.0011(9) 0.0082(8) -0.0022(8) C29 0.0198(10) 0.0280(12) 0.0201(10) 0.0027(8) 0.0005(8) -0.0058(9) C30 0.0244(11) 0.0256(12) 0.0237(11) -0.0034(9) 0.0021(9) 0.0010(9) C31 0.0197(10) 0.0264(12) 0.0312(12) 0.0009(9) 0.0035(9) 0.0024(9) C32 0.0228(10) 0.0253(12) 0.0259(10) 0.0028(9) -0.0019(8) -0.0048(10) C33 0.0298(12) 0.0622(18) 0.0232(11) -0.0096(13) 0.0035(9) -0.0095(13) C34 0.0282(12) 0.064(2) 0.0233(11) -0.0088(12) 0.0076(10) -0.0087(12) C35 0.0267(12) 0.0258(12) 0.0314(12) 0.0039(9) -0.0007(9) 0.0004(9) C36 0.0253(11) 0.0290(13) 0.0325(12) 0.0037(10) -0.0030(9) -0.0001(10) C37 0.0390(15) 0.0375(15) 0.0362(14) 0.0076(12) 0.0021(12) -0.0058(13) C38 0.0235(11) 0.0358(14) 0.0255(12) -0.0002(10) 0.0024(9) 0.0017(10) C39 0.0306(13) 0.0331(15) 0.0465(16) -0.0103(12) 0.0083(12) 0.0011(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O24 1.4282(18) . ? S1 O25 1.4336(15) . ? S1 N28 1.6894(19) . ? S1 C5 1.760(2) . ? S2 O26 1.4285(15) . ? S2 O27 1.4345(16) . ? S2 N28 1.687(2) . ? S2 C15 1.763(2) . ? Si3 C36 1.847(2) . ? Si3 C37 1.864(3) . ? Si3 C38 1.861(3) . ? Si3 C39 1.861(3) . ? N28 C29 1.452(3) . ? C4 C5 1.382(3) . ? C4 C12 1.431(3) . ? C4 C14 1.497(3) . ? C5 C6 1.415(3) . ? C6 C7 1.356(3) . ? C6 H6 0.96(3) . ? C7 C13 1.417(3) . ? C7 H7 0.97(3) . ? C8 C9 1.364(4) . ? C8 C13 1.419(3) . ? C8 H8 0.92(4) . ? C9 C10 1.406(4) . ? C9 H9 0.99(3) . ? C10 C11 1.372(3) . ? C10 H10 0.97(4) . ? C11 C12 1.415(3) . ? C11 H11 0.88(3) . ? C12 C13 1.433(3) . ? C14 C15 1.388(3) . ? C14 C22 1.444(3) . ? C15 C16 1.411(3) . ? C16 C17 1.359(3) . ? C16 H16 1.00(3) . ? C17 C23 1.424(3) . ? C17 H17 0.93(3) . ? C18 C19 1.361(4) . ? C18 C23 1.423(3) . ? C18 H18 1.00(3) . ? C19 C20 1.405(4) . ? C19 H19 0.93(3) . ? C20 C21 1.379(3) . ? C20 H20 0.92(3) . ? C21 C22 1.415(3) . ? C21 H21 1.00(3) . ? C22 C23 1.424(3) . ? C29 C30 1.381(3) . ? C29 C34 1.384(3) . ? C30 C31 1.390(3) . ? C30 H30 0.87(3) . ? C31 C32 1.392(3) . ? C31 H31 0.95(3) . ? C32 C33 1.398(3) . ? C32 C35 1.443(3) . ? C33 C34 1.384(3) . ? C33 H33 1.01(4) . ? C34 H34 1.01(3) . ? C35 C36 1.203(3) . ? C37 H37A 0.94(3) . ? C37 H37B 1.07(4) . ? C37 H37C 1.00(4) . ? C38 H38A 1.01(3) . ? C38 H38B 0.97(4) . ? C38 H38C 0.98(4) . ? C39 H39A 1.12(4) . ? C39 H39B 0.97(4) . ? C39 H39C 0.98(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O24 S1 O25 117.58(10) . . ? O24 S1 N28 105.24(10) . . ? O24 S1 C5 109.96(10) . . ? O25 S1 N28 109.64(10) . . ? O25 S1 C5 110.18(10) . . ? N28 S1 C5 103.18(10) . . ? O26 S2 O27 119.89(10) . . ? O26 S2 N28 107.92(10) . . ? O26 S2 C15 110.62(10) . . ? O27 S2 N28 104.90(10) . . ? O27 S2 C15 109.41(10) . . ? N28 S2 C15 102.52(10) . . ? C36 Si3 C37 106.85(12) . . ? C36 Si3 C38 108.11(12) . . ? C36 Si3 C39 107.58(12) . . ? C38 Si3 C37 110.91(14) . . ? C39 Si3 C37 113.26(15) . . ? C39 Si3 C38 109.90(12) . . ? S2 N28 S1 121.43(11) . . ? C29 N28 S1 112.16(15) . . ? C29 N28 S2 121.46(16) . . ? C5 C4 C12 117.81(19) . . ? C5 C4 C14 121.00(18) . . ? C12 C4 C14 121.14(19) . . ? C4 C5 S1 121.31(16) . . ? C4 C5 C6 123.4(2) . . ? C6 C5 S1 115.27(16) . . ? C5 C6 H6 119.0(17) . . ? C7 C6 C5 119.0(2) . . ? C7 C6 H6 121.9(17) . . ? C6 C7 C13 120.8(2) . . ? C6 C7 H7 120.5(17) . . ? C13 C7 H7 118.4(17) . . ? C9 C8 C13 120.9(2) . . ? C9 C8 H8 124(2) . . ? C13 C8 H8 115(2) . . ? C8 C9 C10 120.0(2) . . ? C8 C9 H9 118.2(18) . . ? C10 C9 H9 121.7(18) . . ? C9 C10 H10 123(2) . . ? C11 C10 C9 120.7(2) . . ? C11 C10 H10 116(2) . . ? C10 C11 C12 121.1(2) . . ? C10 C11 H11 117.5(17) . . ? C12 C11 H11 121.4(17) . . ? C4 C12 C13 118.9(2) . . ? C11 C12 C4 123.1(2) . . ? C11 C12 C13 118.02(19) . . ? C7 C13 C8 120.8(2) . . ? C7 C13 C12 120.00(19) . . ? C8 C13 C12 119.2(2) . . ? C15 C14 C4 121.24(18) . . ? C15 C14 C22 117.72(19) . . ? C22 C14 C4 120.99(18) . . ? C14 C15 S2 121.30(17) . . ? C14 C15 C16 122.82(19) . . ? C16 C15 S2 115.62(16) . . ? C15 C16 H16 124(2) . . ? C17 C16 C15 119.9(2) . . ? C17 C16 H16 116(2) . . ? C16 C17 C23 120.3(2) . . ? C16 C17 H17 115.2(16) . . ? C23 C17 H17 124.4(16) . . ? C19 C18 C23 120.6(2) . . ? C19 C18 H18 122.0(16) . . ? C23 C18 H18 117.4(16) . . ? C18 C19 C20 120.2(2) . . ? C18 C19 H19 119.1(18) . . ? C20 C19 H19 120.6(18) . . ? C19 C20 H20 120(2) . . ? C21 C20 C19 120.9(2) . . ? C21 C20 H20 119(2) . . ? C20 C21 C22 120.3(2) . . ? C20 C21 H21 120.1(13) . . ? C22 C21 H21 119.6(13) . . ? C21 C22 C14 122.5(2) . . ? C21 C22 C23 118.42(19) . . ? C23 C22 C14 119.05(19) . . ? C18 C23 C17 120.4(2) . . ? C18 C23 C22 119.4(2) . . ? C22 C23 C17 120.1(2) . . ? C30 C29 N28 121.5(2) . . ? C30 C29 C34 120.8(2) . . ? C34 C29 N28 117.3(2) . . ? C29 C30 C31 119.6(2) . . ? C29 C30 H30 123(2) . . ? C31 C30 H30 118(2) . . ? C30 C31 C32 120.3(2) . . ? C30 C31 H31 119.3(17) . . ? C32 C31 H31 120.4(17) . . ? C31 C32 C33 119.4(2) . . ? C31 C32 C35 120.9(2) . . ? C33 C32 C35 119.6(2) . . ? C32 C33 H33 119(2) . . ? C34 C33 C32 120.1(2) . . ? C34 C33 H33 121(2) . . ? C29 C34 C33 119.8(2) . . ? C29 C34 H34 114.6(18) . . ? C33 C34 H34 125.2(19) . . ? C36 C35 C32 175.7(3) . . ? C35 C36 Si3 175.4(2) . . ? Si3 C37 H37A 110.8(19) . . ? Si3 C37 H37B 114.4(18) . . ? Si3 C37 H37C 115(2) . . ? H37A C37 H37B 111(3) . . ? H37A C37 H37C 106(3) . . ? H37B C37 H37C 99(3) . . ? Si3 C38 H38A 112.6(16) . . ? Si3 C38 H38B 115(2) . . ? Si3 C38 H38C 110(2) . . ? H38A C38 H38B 109(3) . . ? H38A C38 H38C 111(3) . . ? H38B C38 H38C 100(3) . . ? Si3 C39 H39A 102.2(18) . . ? Si3 C39 H39B 107(2) . . ? Si3 C39 H39C 107(2) . . ? H39A C39 H39B 115(3) . . ? H39A C39 H39C 117(3) . . ? H39B C39 H39C 108(3) . . ? 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 S1 N28 C29 C30 69.7(3) . . . . ? S1 N28 C29 C34 -103.7(2) . . . . ? S1 C5 C6 C7 -176.42(19) . . . . ? S2 N28 C29 C30 -85.7(2) . . . . ? S2 N28 C29 C34 100.9(3) . . . . ? S2 C15 C16 C17 175.80(18) . . . . ? O24 S1 N28 S2 -148.83(13) . . . . ? O24 S1 N28 C29 55.73(17) . . . . ? O24 S1 C5 C4 -175.80(17) . . . . ? O24 S1 C5 C6 2.7(2) . . . . ? O25 S1 N28 S2 83.82(14) . . . . ? O25 S1 N28 C29 -71.61(18) . . . . ? O25 S1 C5 C4 -44.6(2) . . . . ? O25 S1 C5 C6 133.87(17) . . . . ? O26 S2 N28 S1 73.89(14) . . . . ? O26 S2 N28 C29 -132.94(17) . . . . ? O26 S2 C15 C14 -45.0(2) . . . . ? O26 S2 C15 C16 140.75(17) . . . . ? O27 S2 N28 S1 -157.20(12) . . . . ? O27 S2 N28 C29 -4.0(2) . . . . ? O27 S2 C15 C14 -179.18(17) . . . . ? O27 S2 C15 C16 6.5(2) . . . . ? N28 S1 C5 C4 72.35(19) . . . . ? N28 S1 C5 C6 -109.14(18) . . . . ? N28 S2 C15 C14 69.87(19) . . . . ? N28 S2 C15 C16 -104.40(17) . . . . ? N28 C29 C30 C31 -171.3(2) . . . . ? N28 C29 C34 C33 171.9(3) . . . . ? C4 C5 C6 C7 2.1(3) . . . . ? C4 C12 C13 C7 3.4(3) . . . . ? C4 C12 C13 C8 -178.0(2) . . . . ? C4 C14 C15 S2 3.9(3) . . . . ? C4 C14 C15 C16 177.7(2) . . . . ? C4 C14 C22 C21 -2.0(3) . . . . ? C4 C14 C22 C23 -179.73(18) . . . . ? C5 S1 N28 S2 -33.54(15) . . . . ? C5 S1 N28 C29 171.02(16) . . . . ? C5 C4 C12 C11 176.7(2) . . . . ? C5 C4 C12 C13 -2.6(3) . . . . ? C5 C4 C14 C15 -57.1(3) . . . . ? C5 C4 C14 C22 120.3(2) . . . . ? C5 C6 C7 C13 -1.2(4) . . . . ? C6 C7 C13 C8 -180.0(2) . . . . ? C6 C7 C13 C12 -1.5(3) . . . . ? C8 C9 C10 C11 1.5(4) . . . . ? C9 C8 C13 C7 177.7(2) . . . . ? C9 C8 C13 C12 -0.8(4) . . . . ? C9 C10 C11 C12 0.4(4) . . . . ? C10 C11 C12 C4 178.2(2) . . . . ? C10 C11 C12 C13 -2.4(3) . . . . ? C11 C12 C13 C7 -175.9(2) . . . . ? C11 C12 C13 C8 2.6(3) . . . . ? C12 C4 C5 S1 178.32(15) . . . . ? C12 C4 C5 C6 -0.1(3) . . . . ? C12 C4 C14 C15 120.0(2) . . . . ? C12 C4 C14 C22 -62.6(3) . . . . ? C13 C8 C9 C10 -1.3(4) . . . . ? C14 C4 C5 S1 -4.5(3) . . . . ? C14 C4 C5 C6 177.2(2) . . . . ? C14 C4 C12 C11 -0.5(3) . . . . ? C14 C4 C12 C13 -179.85(19) . . . . ? C14 C15 C16 C17 1.6(3) . . . . ? C14 C22 C23 C17 2.5(3) . . . . ? C14 C22 C23 C18 -178.0(2) . . . . ? C15 S2 N28 S1 -42.91(15) . . . . ? C15 S2 N28 C29 110.26(18) . . . . ? C15 C14 C22 C21 175.5(2) . . . . ? C15 C14 C22 C23 -2.2(3) . . . . ? C15 C16 C17 C23 -1.4(3) . . . . ? C16 C17 C23 C18 179.8(2) . . . . ? C16 C17 C23 C22 -0.7(3) . . . . ? C18 C19 C20 C21 1.9(4) . . . . ? C19 C18 C23 C17 177.8(2) . . . . ? C19 C18 C23 C22 -1.6(3) . . . . ? C19 C20 C21 C22 0.7(4) . . . . ? C20 C21 C22 C14 178.6(2) . . . . ? C20 C21 C22 C23 -3.7(3) . . . . ? C21 C22 C23 C17 -175.4(2) . . . . ? C21 C22 C23 C18 4.1(3) . . . . ? C22 C14 C15 S2 -173.64(16) . . . . ? C22 C14 C15 C16 0.2(3) . . . . ? C23 C18 C19 C20 -1.4(4) . . . . ? C29 C30 C31 C32 0.4(4) . . . . ? C30 C29 C34 C33 -1.5(4) . . . . ? C30 C31 C32 C33 -2.9(4) . . . . ? C30 C31 C32 C35 172.5(2) . . . . ? C31 C32 C33 C34 3.2(4) . . . . ? C31 C32 C35 C36 -88(4) . . . . ? C32 C33 C34 C29 -1.0(5) . . . . ? C32 C35 C36 Si3 25(6) . . . . ? C33 C32 C35 C36 87(4) . . . . ? C34 C29 C30 C31 1.9(4) . . . . ? C35 C32 C33 C34 -172.2(3) . . . . ? C37 Si3 C36 C35 14(3) . . . . ? C38 Si3 C36 C35 133(3) . . . . ? C39 Si3 C36 C35 -108(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.256 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.050