####################################################################### # # 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_120309b _database_code_depnum_ccdc_archive 'CCDC 871431' #TrackingRef 'compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H39 N O6 S Si' _chemical_formula_sum 'C29 H39 N O6 S Si' _chemical_formula_weight 557.76 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' 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' 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 10.9625(16) _cell_length_b 12.4135(17) _cell_length_c 12.6502(18) _cell_angle_alpha 115.7800(10) _cell_angle_beta 94.564(2) _cell_angle_gamma 100.874(2) _cell_volume 1496.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1807 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 20.62 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9334 _exptl_absorpt_correction_T_max 0.9740 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8864 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4898 _reflns_number_gt 3139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker apex II' _computing_cell_refinement 'Bruker apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0837P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4898 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 N1 N 0.1902(2) 1.0998(2) 1.1078(2) 0.0476(6) Uani 1 1 d . . . O1 O 0.1132(2) 0.5138(2) 0.9087(2) 0.0805(8) Uani 1 1 d . . . O2 O 0.2964(3) 0.4698(2) 0.9619(2) 0.0791(8) Uani 1 1 d . . . O3 O 0.1523(2) 1.2095(2) 1.3110(2) 0.0786(8) Uani 1 1 d . . . O4 O 0.1079(2) 1.2839(2) 1.1620(2) 0.0812(8) Uani 1 1 d . . . O5 O 0.2708(2) 1.14525(19) 0.80971(19) 0.0600(6) Uani 1 1 d . . . O6 O 0.23104(19) 0.89211(19) 0.63171(17) 0.0551(6) Uani 1 1 d . . . S1 S 0.18549(8) 1.23261(8) 1.21421(8) 0.0587(3) Uani 1 1 d . . . Si1 Si 0.15418(9) 0.78603(8) 0.49840(8) 0.0547(3) Uani 1 1 d . . . C1 C 0.2247(3) 1.0925(3) 0.9940(2) 0.0437(7) Uani 1 1 d . . . H1 H 0.2958 1.1625 1.0116 0.052 Uiso 1 1 calc R . . C2 C 0.1178(3) 1.0885(3) 0.9074(3) 0.0507(8) Uani 1 1 d . . . H2A H 0.0425 1.0279 0.8992 0.061 Uiso 1 1 calc R . . H2B H 0.0984 1.1685 0.9372 0.061 Uiso 1 1 calc R . . C3 C 0.1577(3) 1.0544(3) 0.7883(3) 0.0502(8) Uani 1 1 d . . . H3 H 0.0923 1.0589 0.7340 0.060 Uiso 1 1 calc R . . C4 C 0.1741(3) 0.9230(3) 0.7364(2) 0.0480(8) Uani 1 1 d . . . H4 H 0.0896 0.8671 0.7119 0.058 Uiso 1 1 calc R . . C5 C 0.2477(3) 0.9008(3) 0.8270(3) 0.0457(7) Uani 1 1 d . . . H5 H 0.2807 0.8317 0.8005 0.055 Uiso 1 1 calc R . . C6 C 0.2675(3) 0.9755(2) 0.9430(2) 0.0404(7) Uani 1 1 d . . . C7 C 0.3230(3) 0.9567(3) 1.0451(2) 0.0453(7) Uani 1 1 d . . . H7 H 0.4106 1.0064 1.0746 0.054 Uiso 1 1 calc R . . C8 C 0.2433(3) 1.0148(3) 1.1398(3) 0.0621(9) Uani 1 1 d . . . H8A H 0.1761 0.9513 1.1394 0.074 Uiso 1 1 calc R . . H8B H 0.2957 1.0596 1.2188 0.074 Uiso 1 1 calc R . . C9 C 0.3213(3) 0.8258(3) 1.0195(2) 0.0434(7) Uani 1 1 d . . . C10 C 0.2084(3) 0.7328(3) 0.9693(3) 0.0497(8) Uani 1 1 d . . . H10 H 0.1340 0.7488 0.9460 0.060 Uiso 1 1 calc R . . C11 C 0.2111(3) 0.6193(3) 0.9559(3) 0.0526(8) Uani 1 1 d . . . C12 C 0.1640(4) 0.4281(3) 0.9336(4) 0.0864(13) Uani 1 1 d . . . H12A H 0.1315 0.4211 1.0000 0.104 Uiso 1 1 calc R . . H12B H 0.1392 0.3473 0.8644 0.104 Uiso 1 1 calc R . . C13 C 0.3208(3) 0.5931(3) 0.9873(3) 0.0557(8) Uani 1 1 d . . . C14 C 0.4328(3) 0.6796(3) 1.0339(3) 0.0602(9) Uani 1 1 d . . . H14 H 0.5069 0.6610 1.0538 0.072 Uiso 1 1 calc R . . C15 C 0.4306(3) 0.7971(3) 1.0503(3) 0.0524(8) Uani 1 1 d . . . H15 H 0.5053 0.8590 1.0832 0.063 Uiso 1 1 calc R . . C16 C 0.3391(3) 1.3280(3) 1.2596(3) 0.0537(8) Uani 1 1 d . . . C17 C 0.4241(4) 1.3233(4) 1.3410(4) 0.0993(16) Uani 1 1 d . . . H17 H 0.4001 1.2716 1.3752 0.119 Uiso 1 1 calc R . . C18 C 0.5460(4) 1.3957(5) 1.3724(5) 0.127(2) Uani 1 1 d . . . H18 H 0.6036 1.3917 1.4280 0.152 Uiso 1 1 calc R . . C19 C 0.5848(4) 1.4732(3) 1.3240(3) 0.0771(11) Uani 1 1 d . . . C20 C 0.4994(4) 1.4772(3) 1.2435(3) 0.0644(10) Uani 1 1 d . . . H20 H 0.5237 1.5294 1.2099 0.077 Uiso 1 1 calc R . . C21 C 0.3768(3) 1.4056(3) 1.2100(3) 0.0606(9) Uani 1 1 d . . . H21 H 0.3197 1.4097 1.1541 0.073 Uiso 1 1 calc R . . C22 C 0.7205(4) 1.5521(4) 1.3607(4) 0.1190(19) Uani 1 1 d . . . H22A H 0.7408 1.5996 1.4460 0.178 Uiso 1 1 calc R . . H22B H 0.7287 1.6069 1.3251 0.178 Uiso 1 1 calc R . . H22C H 0.7771 1.4995 1.3339 0.178 Uiso 1 1 calc R . . C23 C 0.3041(4) 1.1623(3) 0.7124(3) 0.0775(11) Uani 1 1 d . . . H23A H 0.3537 1.1061 0.6719 0.116 Uiso 1 1 calc R . . H23B H 0.3525 1.2457 0.7404 0.116 Uiso 1 1 calc R . . H23C H 0.2290 1.1470 0.6583 0.116 Uiso 1 1 calc R . . C24 C 0.0085(4) 0.8248(4) 0.4577(4) 0.0880(13) Uani 1 1 d . . . H24A H -0.0471 0.8250 0.5127 0.132 Uiso 1 1 calc R . . H24B H -0.0328 0.7645 0.3783 0.132 Uiso 1 1 calc R . . H24C H 0.0298 0.9050 0.4612 0.132 Uiso 1 1 calc R . . C25 C 0.1091(4) 0.6344(3) 0.4973(4) 0.0964(14) Uani 1 1 d . . . H25A H 0.1823 0.6172 0.5274 0.145 Uiso 1 1 calc R . . H25B H 0.0746 0.5713 0.4171 0.145 Uiso 1 1 calc R . . H25C H 0.0468 0.6359 0.5469 0.145 Uiso 1 1 calc R . . C26 C 0.2662(4) 0.7863(3) 0.3940(3) 0.0727(10) Uani 1 1 d . . . C27 C 0.2963(5) 0.9100(4) 0.3893(5) 0.1202(18) Uani 1 1 d . . . H27A H 0.3517 0.9063 0.3334 0.180 Uiso 1 1 calc R . . H27B H 0.3366 0.9752 0.4671 0.180 Uiso 1 1 calc R . . H27C H 0.2194 0.9258 0.3645 0.180 Uiso 1 1 calc R . . C28 C 0.2072(6) 0.6809(5) 0.2685(4) 0.154(2) Uani 1 1 d . . . H28A H 0.1308 0.6949 0.2399 0.232 Uiso 1 1 calc R . . H28B H 0.1881 0.6038 0.2718 0.232 Uiso 1 1 calc R . . H28C H 0.2657 0.6781 0.2153 0.232 Uiso 1 1 calc R . . C29 C 0.3922(5) 0.7679(5) 0.4368(5) 0.1230(18) Uani 1 1 d . . . H29A H 0.4497 0.7708 0.3841 0.184 Uiso 1 1 calc R . . H29B H 0.3779 0.6892 0.4367 0.184 Uiso 1 1 calc R . . H29C H 0.4277 0.8323 0.5162 0.184 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 N1 0.0453(16) 0.0463(14) 0.0472(14) 0.0197(12) 0.0087(11) 0.0071(11) O1 0.0686(17) 0.0599(15) 0.110(2) 0.0498(15) -0.0143(15) -0.0037(13) O2 0.087(2) 0.0609(16) 0.0984(19) 0.0440(14) 0.0073(15) 0.0241(14) O3 0.0644(17) 0.0879(18) 0.0639(15) 0.0215(13) 0.0300(12) 0.0009(13) O4 0.0598(17) 0.0798(17) 0.0924(18) 0.0234(14) 0.0049(13) 0.0357(13) O5 0.0556(15) 0.0628(14) 0.0661(14) 0.0434(12) 0.0002(11) -0.0057(11) O6 0.0482(14) 0.0699(14) 0.0442(12) 0.0294(11) 0.0077(10) 0.0001(10) S1 0.0436(5) 0.0603(5) 0.0591(6) 0.0157(4) 0.0138(4) 0.0111(4) Si1 0.0555(6) 0.0538(6) 0.0515(5) 0.0263(4) 0.0044(4) 0.0034(4) C1 0.0372(17) 0.0441(17) 0.0479(17) 0.0229(14) 0.0056(13) 0.0020(13) C2 0.0433(19) 0.0511(18) 0.059(2) 0.0277(16) 0.0072(15) 0.0103(14) C3 0.0399(19) 0.0573(19) 0.0569(19) 0.0348(16) -0.0031(14) 0.0035(15) C4 0.0416(19) 0.0537(18) 0.0450(18) 0.0266(15) 0.0016(14) -0.0034(14) C5 0.0457(19) 0.0489(17) 0.0483(18) 0.0282(15) 0.0110(14) 0.0087(14) C6 0.0326(17) 0.0449(16) 0.0461(17) 0.0253(14) 0.0069(13) 0.0043(13) C7 0.0409(18) 0.0493(17) 0.0472(17) 0.0262(15) 0.0038(14) 0.0060(14) C8 0.079(3) 0.064(2) 0.053(2) 0.0338(18) 0.0180(18) 0.0217(18) C9 0.0396(18) 0.0554(18) 0.0432(16) 0.0299(15) 0.0074(13) 0.0113(14) C10 0.0373(19) 0.0573(19) 0.062(2) 0.0361(17) 0.0022(15) 0.0099(15) C11 0.048(2) 0.0515(19) 0.059(2) 0.0297(17) -0.0005(15) 0.0059(16) C12 0.104(4) 0.059(2) 0.101(3) 0.046(2) 0.005(3) 0.013(2) C13 0.068(3) 0.053(2) 0.057(2) 0.0317(17) 0.0127(17) 0.0237(18) C14 0.051(2) 0.077(2) 0.065(2) 0.0383(19) 0.0110(17) 0.0291(19) C15 0.0395(19) 0.065(2) 0.0575(19) 0.0332(17) 0.0068(15) 0.0124(15) C16 0.053(2) 0.0474(18) 0.0499(19) 0.0153(15) 0.0066(15) 0.0072(15) C17 0.074(3) 0.121(4) 0.113(3) 0.087(3) -0.019(3) -0.024(3) C18 0.075(3) 0.162(5) 0.153(5) 0.123(4) -0.049(3) -0.048(3) C19 0.066(3) 0.073(2) 0.077(3) 0.036(2) -0.002(2) -0.017(2) C20 0.075(3) 0.0491(19) 0.066(2) 0.0284(18) 0.0097(19) 0.0042(18) C21 0.063(2) 0.0501(19) 0.064(2) 0.0251(17) 0.0014(17) 0.0122(17) C22 0.082(3) 0.132(4) 0.127(4) 0.079(3) -0.018(3) -0.041(3) C23 0.084(3) 0.078(2) 0.080(3) 0.054(2) 0.010(2) -0.004(2) C24 0.072(3) 0.105(3) 0.083(3) 0.044(2) -0.008(2) 0.021(2) C25 0.103(4) 0.070(3) 0.124(4) 0.053(3) 0.035(3) 0.011(2) C26 0.080(3) 0.080(3) 0.055(2) 0.030(2) 0.0210(19) 0.010(2) C27 0.157(5) 0.129(4) 0.125(4) 0.093(4) 0.073(4) 0.040(3) C28 0.176(6) 0.162(5) 0.060(3) 0.006(3) 0.044(3) -0.001(4) C29 0.096(4) 0.172(5) 0.156(5) 0.104(4) 0.074(3) 0.060(4) _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 N1 C8 1.478(4) . ? N1 C1 1.486(4) . ? N1 S1 1.626(2) . ? O1 C11 1.382(4) . ? O1 C12 1.423(4) . ? O2 C13 1.386(4) . ? O2 C12 1.405(5) . ? O3 S1 1.433(2) . ? O4 S1 1.430(2) . ? O5 C23 1.401(4) . ? O5 C3 1.427(3) . ? O6 C4 1.439(3) . ? O6 Si1 1.647(2) . ? S1 C16 1.752(3) . ? Si1 C25 1.847(3) . ? Si1 C24 1.849(4) . ? Si1 C26 1.874(4) . ? C1 C6 1.496(4) . ? C1 C2 1.518(4) . ? C1 H1 0.9800 . ? C2 C3 1.504(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.524(4) . ? C3 H3 0.9800 . ? C4 C5 1.501(4) . ? C4 H4 0.9800 . ? C5 C6 1.323(4) . ? C5 H5 0.9300 . ? C6 C7 1.511(4) . ? C7 C9 1.509(4) . ? C7 C8 1.541(4) . ? C7 H7 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C15 1.387(4) . ? C9 C10 1.402(4) . ? C10 C11 1.350(4) . ? C10 H10 0.9300 . ? C11 C13 1.376(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.358(5) . ? C14 C15 1.386(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.361(5) . ? C16 C21 1.382(4) . ? C17 C18 1.380(5) . ? C17 H17 0.9300 . ? C18 C19 1.372(5) . ? C18 H18 0.9300 . ? C19 C20 1.351(5) . ? C19 C22 1.527(5) . ? C20 C21 1.380(5) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.536(5) . ? C26 C29 1.536(6) . ? C26 C28 1.537(6) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? 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 C8 N1 C1 110.5(2) . . ? C8 N1 S1 118.6(2) . . ? C1 N1 S1 119.41(18) . . ? C11 O1 C12 104.4(3) . . ? C13 O2 C12 104.7(3) . . ? C23 O5 C3 117.5(2) . . ? C4 O6 Si1 122.17(18) . . ? O4 S1 O3 120.55(17) . . ? O4 S1 N1 106.60(14) . . ? O3 S1 N1 105.91(14) . . ? O4 S1 C16 107.69(16) . . ? O3 S1 C16 108.19(15) . . ? N1 S1 C16 107.22(14) . . ? O6 Si1 C25 110.01(16) . . ? O6 Si1 C24 110.54(16) . . ? C25 Si1 C24 108.3(2) . . ? O6 Si1 C26 105.34(14) . . ? C25 Si1 C26 111.90(19) . . ? C24 Si1 C26 110.78(18) . . ? N1 C1 C6 102.7(2) . . ? N1 C1 C2 114.8(2) . . ? C6 C1 C2 111.0(2) . . ? N1 C1 H1 109.4 . . ? C6 C1 H1 109.4 . . ? C2 C1 H1 109.4 . . ? C3 C2 C1 108.7(2) . . ? C3 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? C3 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O5 C3 C2 106.0(2) . . ? O5 C3 C4 113.8(2) . . ? C2 C3 C4 109.4(2) . . ? O5 C3 H3 109.2 . . ? C2 C3 H3 109.2 . . ? C4 C3 H3 109.2 . . ? O6 C4 C5 110.5(2) . . ? O6 C4 C3 111.8(2) . . ? C5 C4 C3 112.1(2) . . ? O6 C4 H4 107.4 . . ? C5 C4 H4 107.4 . . ? C3 C4 H4 107.4 . . ? C6 C5 C4 122.7(3) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C1 122.8(2) . . ? C5 C6 C7 128.7(3) . . ? C1 C6 C7 108.3(2) . . ? C9 C7 C6 116.9(2) . . ? C9 C7 C8 112.2(2) . . ? C6 C7 C8 101.8(2) . . ? C9 C7 H7 108.5 . . ? C6 C7 H7 108.5 . . ? C8 C7 H7 108.5 . . ? N1 C8 C7 106.4(2) . . ? N1 C8 H8A 110.5 . . ? C7 C8 H8A 110.5 . . ? N1 C8 H8B 110.5 . . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.6 . . ? C15 C9 C10 119.1(3) . . ? C15 C9 C7 120.2(3) . . ? C10 C9 C7 120.6(3) . . ? C11 C10 C9 117.9(3) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? C10 C11 C13 121.9(3) . . ? C10 C11 O1 128.5(3) . . ? C13 C11 O1 109.6(3) . . ? O2 C12 O1 108.9(3) . . ? O2 C12 H12A 109.9 . . ? O1 C12 H12A 109.9 . . ? O2 C12 H12B 109.9 . . ? O1 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C14 C13 C11 122.2(3) . . ? C14 C13 O2 128.3(3) . . ? C11 C13 O2 109.5(3) . . ? C13 C14 C15 116.4(3) . . ? C13 C14 H14 121.8 . . ? C15 C14 H14 121.8 . . ? C14 C15 C9 122.5(3) . . ? C14 C15 H15 118.8 . . ? C9 C15 H15 118.8 . . ? C17 C16 C21 119.2(3) . . ? C17 C16 S1 120.4(3) . . ? C21 C16 S1 120.4(3) . . ? C16 C17 C18 119.7(4) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 121.8(4) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C20 C19 C18 117.9(4) . . ? C20 C19 C22 121.5(3) . . ? C18 C19 C22 120.5(4) . . ? C19 C20 C21 121.6(3) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C20 C21 C16 119.8(3) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 H23A 109.5 . . ? O5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C29 106.9(4) . . ? C27 C26 C28 109.7(4) . . ? C29 C26 C28 109.5(4) . . ? C27 C26 Si1 111.5(3) . . ? C29 C26 Si1 110.2(3) . . ? C28 C26 Si1 109.0(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 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 N1 S1 O4 -168.5(2) . . . . ? C1 N1 S1 O4 51.6(3) . . . . ? C8 N1 S1 O3 -38.9(3) . . . . ? C1 N1 S1 O3 -178.9(2) . . . . ? C8 N1 S1 C16 76.4(3) . . . . ? C1 N1 S1 C16 -63.5(2) . . . . ? C4 O6 Si1 C25 -61.6(3) . . . . ? C4 O6 Si1 C24 57.9(3) . . . . ? C4 O6 Si1 C26 177.6(2) . . . . ? C8 N1 C1 C6 15.7(3) . . . . ? S1 N1 C1 C6 158.60(19) . . . . ? C8 N1 C1 C2 136.3(3) . . . . ? S1 N1 C1 C2 -80.9(3) . . . . ? N1 C1 C2 C3 -168.2(2) . . . . ? C6 C1 C2 C3 -52.3(3) . . . . ? C23 O5 C3 C2 -158.2(3) . . . . ? C23 O5 C3 C4 81.5(3) . . . . ? C1 C2 C3 O5 -57.5(3) . . . . ? C1 C2 C3 C4 65.6(3) . . . . ? Si1 O6 C4 C5 120.4(2) . . . . ? Si1 O6 C4 C3 -114.0(2) . . . . ? O5 C3 C4 O6 -52.6(3) . . . . ? C2 C3 C4 O6 -170.9(2) . . . . ? O5 C3 C4 C5 72.1(3) . . . . ? C2 C3 C4 C5 -46.2(3) . . . . ? O6 C4 C5 C6 141.1(3) . . . . ? C3 C4 C5 C6 15.6(4) . . . . ? C4 C5 C6 C1 -3.5(4) . . . . ? C4 C5 C6 C7 170.6(3) . . . . ? N1 C1 C6 C5 145.1(3) . . . . ? C2 C1 C6 C5 22.0(4) . . . . ? N1 C1 C6 C7 -30.0(3) . . . . ? C2 C1 C6 C7 -153.2(2) . . . . ? C5 C6 C7 C9 -20.0(4) . . . . ? C1 C6 C7 C9 154.8(2) . . . . ? C5 C6 C7 C8 -142.7(3) . . . . ? C1 C6 C7 C8 32.1(3) . . . . ? C1 N1 C8 C7 3.7(3) . . . . ? S1 N1 C8 C7 -139.5(2) . . . . ? C9 C7 C8 N1 -147.2(2) . . . . ? C6 C7 C8 N1 -21.3(3) . . . . ? C6 C7 C9 C15 129.6(3) . . . . ? C8 C7 C9 C15 -113.3(3) . . . . ? C6 C7 C9 C10 -53.2(4) . . . . ? C8 C7 C9 C10 63.9(3) . . . . ? C15 C9 C10 C11 1.5(4) . . . . ? C7 C9 C10 C11 -175.7(3) . . . . ? C9 C10 C11 C13 -1.5(5) . . . . ? C9 C10 C11 O1 -179.7(3) . . . . ? C12 O1 C11 C10 -171.1(3) . . . . ? C12 O1 C11 C13 10.5(4) . . . . ? C13 O2 C12 O1 16.6(4) . . . . ? C11 O1 C12 O2 -16.9(4) . . . . ? C10 C11 C13 C14 0.2(5) . . . . ? O1 C11 C13 C14 178.7(3) . . . . ? C10 C11 C13 O2 -178.9(3) . . . . ? O1 C11 C13 O2 -0.4(4) . . . . ? C12 O2 C13 C14 171.0(4) . . . . ? C12 O2 C13 C11 -10.0(4) . . . . ? C11 C13 C14 C15 1.1(5) . . . . ? O2 C13 C14 C15 180.0(3) . . . . ? C13 C14 C15 C9 -1.0(5) . . . . ? C10 C9 C15 C14 -0.3(4) . . . . ? C7 C9 C15 C14 176.9(3) . . . . ? O4 S1 C16 C17 161.3(3) . . . . ? O3 S1 C16 C17 29.5(4) . . . . ? N1 S1 C16 C17 -84.4(3) . . . . ? O4 S1 C16 C21 -21.1(3) . . . . ? O3 S1 C16 C21 -152.9(3) . . . . ? N1 S1 C16 C21 93.3(3) . . . . ? C21 C16 C17 C18 -0.1(7) . . . . ? S1 C16 C17 C18 177.6(4) . . . . ? C16 C17 C18 C19 0.1(9) . . . . ? C17 C18 C19 C20 0.0(8) . . . . ? C17 C18 C19 C22 -180.0(5) . . . . ? C18 C19 C20 C21 -0.2(7) . . . . ? C22 C19 C20 C21 179.8(4) . . . . ? C19 C20 C21 C16 0.3(5) . . . . ? C17 C16 C21 C20 -0.1(5) . . . . ? S1 C16 C21 C20 -177.8(3) . . . . ? O6 Si1 C26 C27 -64.2(3) . . . . ? C25 Si1 C26 C27 176.3(3) . . . . ? C24 Si1 C26 C27 55.3(3) . . . . ? O6 Si1 C26 C29 54.3(3) . . . . ? C25 Si1 C26 C29 -65.2(4) . . . . ? C24 Si1 C26 C29 173.9(3) . . . . ? O6 Si1 C26 C28 174.5(3) . . . . ? C25 Si1 C26 C28 55.0(4) . . . . ? C24 Si1 C26 C28 -65.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.458 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.049