data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof. Martin Oestreich' _publ_contact_author_email MARTIN.OESTREICH@UNI-MUENSTER.DE _publ_section_title ; Kinetic resolution of donor-functionalised tertiary alcohols by Cu-H-catalysed stereoselective silylation using a strained silicon-stereogenic silane ; loop_ _publ_author_name 'Martin Oestreich' 'Roland Frohlich' 'Betul Karatas' 'Sebastian Rendler' data_ost4337 _database_code_depnum_ccdc_archive 'CCDC 668297' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 Cl N O Si2' _chemical_formula_weight 518.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 10.2053(4) _cell_length_b 10.5866(5) _cell_length_c 16.1920(8) _cell_angle_alpha 72.052(2) _cell_angle_beta 80.971(2) _cell_angle_gamma 62.274(4) _cell_volume 1472.97(12) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4778 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 2.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6233 _exptl_absorpt_correction_T_max 0.6702 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17954 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.90 _diffrn_reflns_theta_max 68.18 _reflns_number_total 5153 _reflns_number_gt 4833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0586P)^2^+0.6423P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5153 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1114 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.52410(5) 0.02189(5) 0.24245(3) 0.03581(14) Uani 1 1 d . . . C2 C 0.6986(2) -0.1262(2) 0.29830(12) 0.0409(4) Uani 1 1 d . . . C3 C 0.7246(2) -0.2429(2) 0.37348(13) 0.0498(5) Uani 1 1 d . . . H3 H 0.6448 -0.2587 0.4040 0.060 Uiso 1 1 calc R . . C4 C 0.8669(3) -0.3354(2) 0.40336(14) 0.0595(6) Uani 1 1 d . . . H4 H 0.8839 -0.4148 0.4534 0.071 Uiso 1 1 calc R . . C5 C 0.9842(3) -0.3113(2) 0.35984(17) 0.0615(6) Uani 1 1 d . . . H5 H 1.0805 -0.3727 0.3814 0.074 Uiso 1 1 calc R . . C6 C 0.9612(2) -0.1979(3) 0.28500(17) 0.0589(6) Uani 1 1 d . . . H6 H 1.0419 -0.1828 0.2555 0.071 Uiso 1 1 calc R . . C7 C 0.8190(2) -0.1054(2) 0.25278(13) 0.0460(4) Uani 1 1 d . . . C8 C 0.7845(2) 0.0173(2) 0.16917(14) 0.0542(5) Uani 1 1 d . . . H8A H 0.8081 -0.0250 0.1197 0.065 Uiso 1 1 calc R . . H8B H 0.8457 0.0684 0.1641 0.065 Uiso 1 1 calc R . . C9 C 0.6195(2) 0.1290(2) 0.16731(13) 0.0480(4) Uani 1 1 d . . . H9A H 0.5811 0.1667 0.1084 0.058 Uiso 1 1 calc R . . H9B H 0.6052 0.2129 0.1876 0.058 Uiso 1 1 calc R . . C10 C 0.4322(2) -0.0505(2) 0.18932(13) 0.0458(4) Uani 1 1 d . . . C11 C 0.5443(3) -0.1350(3) 0.12702(17) 0.0705(7) Uani 1 1 d . . . H11A H 0.4983 -0.1737 0.0996 0.106 Uiso 1 1 calc R . . H11B H 0.6297 -0.2163 0.1593 0.106 Uiso 1 1 calc R . . H11C H 0.5757 -0.0682 0.0828 0.106 Uiso 1 1 calc R . . C12 C 0.2969(3) 0.0772(3) 0.13877(16) 0.0653(6) Uani 1 1 d . . . H12A H 0.2513 0.0382 0.1113 0.098 Uiso 1 1 calc R . . H12B H 0.3274 0.1447 0.0946 0.098 Uiso 1 1 calc R . . H12C H 0.2261 0.1298 0.1783 0.098 Uiso 1 1 calc R . . C13 C 0.3826(3) -0.1555(3) 0.25938(16) 0.0643(6) Uani 1 1 d . . . H13A H 0.3141 -0.1025 0.2995 0.096 Uiso 1 1 calc R . . H13B H 0.4683 -0.2381 0.2907 0.096 Uiso 1 1 calc R . . H13C H 0.3341 -0.1922 0.2324 0.096 Uiso 1 1 calc R . . O14 O 0.40147(13) 0.10539(13) 0.31072(8) 0.0384(3) Uani 1 1 d . . . C15 C 0.34466(19) 0.25068(18) 0.32108(11) 0.0371(4) Uani 1 1 d . . . C16 C 0.30152(19) 0.36252(19) 0.23606(12) 0.0399(4) Uani 1 1 d . . . C17 C 0.2610(2) 0.4539(2) 0.16822(12) 0.0450(4) Uani 1 1 d . . . Si18 Si 0.18889(6) 0.59597(6) 0.06573(3) 0.04771(16) Uani 1 1 d . . . C19 C -0.0116(3) 0.6484(3) 0.0639(2) 0.0843(8) Uani 1 1 d . . . H19A H -0.0246 0.5620 0.0669 0.126 Uiso 1 1 calc R . . H19B H -0.0537 0.7241 0.0106 0.126 Uiso 1 1 calc R . . H19C H -0.0613 0.6866 0.1133 0.126 Uiso 1 1 calc R . . C20 C 0.2163(4) 0.7581(3) 0.06475(17) 0.0800(8) Uani 1 1 d . . . H20A H 0.1622 0.7971 0.1132 0.120 Uiso 1 1 calc R . . H20B H 0.1802 0.8343 0.0107 0.120 Uiso 1 1 calc R . . H20C H 0.3209 0.7277 0.0698 0.120 Uiso 1 1 calc R . . C21 C 0.2915(3) 0.5177(3) -0.02572(16) 0.0738(7) Uani 1 1 d . . . H21A H 0.3965 0.4849 -0.0203 0.111 Uiso 1 1 calc R . . H21B H 0.2571 0.5931 -0.0802 0.111 Uiso 1 1 calc R . . H21C H 0.2746 0.4343 -0.0245 0.111 Uiso 1 1 calc R . . C22 C 0.45549(19) 0.26555(19) 0.36631(11) 0.0377(4) Uani 1 1 d . . . C23 C 0.5546(2) 0.1427(2) 0.42525(12) 0.0418(4) Uani 1 1 d . . . H23 H 0.5578 0.0494 0.4334 0.050 Uiso 1 1 calc R . . C24 C 0.6484(2) 0.1552(2) 0.47221(12) 0.0455(4) Uani 1 1 d . . . H24 H 0.7144 0.0716 0.5121 0.055 Uiso 1 1 calc R . . C25 C 0.6432(2) 0.2919(2) 0.45936(12) 0.0449(4) Uani 1 1 d . . . C26 C 0.5458(2) 0.4158(2) 0.40201(14) 0.0517(5) Uani 1 1 d . . . H26 H 0.5429 0.5087 0.3944 0.062 Uiso 1 1 calc R . . C27 C 0.4525(2) 0.4020(2) 0.35572(13) 0.0481(4) Uani 1 1 d . . . H27 H 0.3861 0.4864 0.3165 0.058 Uiso 1 1 calc R . . Cl28 Cl 0.76637(6) 0.30705(7) 0.51465(4) 0.06073(17) Uani 1 1 d . . . C29 C 0.20591(19) 0.2726(2) 0.38120(11) 0.0393(4) Uani 1 1 d . . . H29A H 0.2374 0.2014 0.4381 0.047 Uiso 1 1 calc R . . H29B H 0.1629 0.3722 0.3895 0.047 Uiso 1 1 calc R . . C30 C 0.0876(2) 0.2542(2) 0.34856(12) 0.0419(4) Uani 1 1 d . . . N31 N 0.09102(18) 0.12041(19) 0.37802(12) 0.0532(4) Uani 1 1 d . . . C32 C -0.0135(3) 0.1012(3) 0.35087(19) 0.0674(6) Uani 1 1 d . . . H32 H -0.0123 0.0073 0.3713 0.081 Uiso 1 1 calc R . . C33 C -0.1230(3) 0.2111(3) 0.29466(18) 0.0705(7) Uani 1 1 d . . . H33 H -0.1938 0.1921 0.2766 0.085 Uiso 1 1 calc R . . C34 C -0.1271(2) 0.3485(3) 0.26546(15) 0.0650(6) Uani 1 1 d . . . H34 H -0.2015 0.4260 0.2275 0.078 Uiso 1 1 calc R . . C35 C -0.0206(2) 0.3717(3) 0.29240(13) 0.0515(5) Uani 1 1 d . . . H35 H -0.0210 0.4652 0.2732 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0342(3) 0.0355(2) 0.0337(2) -0.00761(18) -0.00299(18) -0.01246(19) C2 0.0383(9) 0.0407(9) 0.0384(9) -0.0132(7) -0.0045(7) -0.0105(7) C3 0.0509(11) 0.0452(10) 0.0418(10) -0.0123(8) -0.0046(8) -0.0104(9) C4 0.0638(14) 0.0465(11) 0.0506(12) -0.0145(9) -0.0205(10) -0.0034(10) C5 0.0481(12) 0.0504(12) 0.0786(15) -0.0281(11) -0.0258(11) -0.0019(10) C6 0.0390(11) 0.0589(13) 0.0832(16) -0.0347(12) -0.0028(10) -0.0152(10) C7 0.0372(10) 0.0463(10) 0.0543(11) -0.0211(9) -0.0011(8) -0.0136(8) C8 0.0469(11) 0.0576(12) 0.0576(12) -0.0174(10) 0.0100(9) -0.0250(10) C9 0.0466(11) 0.0468(10) 0.0453(10) -0.0065(8) 0.0014(8) -0.0207(9) C10 0.0467(10) 0.0474(10) 0.0453(10) -0.0170(8) -0.0040(8) -0.0187(9) C11 0.0701(15) 0.0861(17) 0.0700(15) -0.0478(14) 0.0060(12) -0.0321(13) C12 0.0625(14) 0.0677(14) 0.0659(14) -0.0165(11) -0.0242(11) -0.0231(12) C13 0.0743(15) 0.0636(14) 0.0693(15) -0.0162(11) -0.0049(12) -0.0422(12) O14 0.0386(6) 0.0351(6) 0.0399(6) -0.0108(5) -0.0002(5) -0.0149(5) C15 0.0372(9) 0.0330(8) 0.0367(9) -0.0080(7) -0.0036(7) -0.0119(7) C16 0.0371(9) 0.0392(9) 0.0414(10) -0.0110(8) -0.0022(7) -0.0148(8) C17 0.0450(10) 0.0451(10) 0.0413(10) -0.0067(8) -0.0056(8) -0.0186(8) Si18 0.0550(3) 0.0472(3) 0.0371(3) -0.0027(2) -0.0114(2) -0.0216(3) C19 0.0619(16) 0.0876(19) 0.0842(19) -0.0065(15) -0.0286(14) -0.0196(14) C20 0.125(2) 0.0678(15) 0.0570(14) -0.0091(12) 0.0037(15) -0.0574(17) C21 0.0911(19) 0.0868(18) 0.0488(13) -0.0209(12) -0.0026(12) -0.0417(15) C22 0.0371(9) 0.0379(9) 0.0359(9) -0.0091(7) -0.0006(7) -0.0154(7) C23 0.0463(10) 0.0387(9) 0.0404(9) -0.0043(7) -0.0055(8) -0.0213(8) C24 0.0444(10) 0.0475(10) 0.0413(10) -0.0048(8) -0.0084(8) -0.0197(8) C25 0.0428(10) 0.0550(11) 0.0434(10) -0.0163(8) -0.0005(8) -0.0251(9) C26 0.0567(12) 0.0423(10) 0.0613(12) -0.0144(9) -0.0070(10) -0.0241(9) C27 0.0496(11) 0.0362(9) 0.0537(11) -0.0074(8) -0.0111(9) -0.0150(8) Cl28 0.0578(3) 0.0759(4) 0.0647(3) -0.0246(3) -0.0087(2) -0.0369(3) C29 0.0382(9) 0.0392(9) 0.0372(9) -0.0122(7) -0.0010(7) -0.0131(7) C30 0.0347(9) 0.0485(10) 0.0403(9) -0.0176(8) 0.0036(7) -0.0144(8) N31 0.0421(9) 0.0519(10) 0.0690(11) -0.0208(8) 0.0023(8) -0.0217(8) C32 0.0515(13) 0.0733(15) 0.0944(18) -0.0366(14) 0.0071(12) -0.0352(12) C33 0.0476(13) 0.107(2) 0.0774(16) -0.0456(15) 0.0057(11) -0.0395(14) C34 0.0436(12) 0.0960(19) 0.0504(12) -0.0198(12) -0.0051(9) -0.0256(12) C35 0.0415(10) 0.0612(12) 0.0462(11) -0.0129(9) -0.0023(8) -0.0187(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O14 1.6457(12) . ? Si1 C2 1.8656(18) . ? Si1 C9 1.8761(19) . ? Si1 C10 1.881(2) . ? C2 C3 1.396(3) . ? C2 C7 1.403(3) . ? C3 C4 1.381(3) . ? C4 C5 1.379(4) . ? C5 C6 1.377(4) . ? C6 C7 1.392(3) . ? C7 C8 1.511(3) . ? C8 C9 1.542(3) . ? C10 C12 1.530(3) . ? C10 C13 1.531(3) . ? C10 C11 1.539(3) . ? O14 C15 1.424(2) . ? C15 C16 1.480(2) . ? C15 C22 1.529(2) . ? C15 C29 1.552(2) . ? C16 C17 1.195(3) . ? C17 Si18 1.8365(19) . ? Si18 C21 1.854(3) . ? Si18 C19 1.857(3) . ? Si18 C20 1.859(3) . ? C22 C27 1.388(3) . ? C22 C23 1.392(2) . ? C23 C24 1.386(3) . ? C24 C25 1.373(3) . ? C25 C26 1.377(3) . ? C25 Cl28 1.7430(19) . ? C26 C27 1.382(3) . ? C29 C30 1.502(3) . ? C30 N31 1.333(3) . ? C30 C35 1.390(3) . ? N31 C32 1.333(3) . ? C32 C33 1.374(4) . ? C33 C34 1.366(4) . ? C34 C35 1.377(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 O14 Si1 C2 111.52(7) . . ? O14 Si1 C9 116.09(8) . . ? C2 Si1 C9 93.51(9) . . ? O14 Si1 C10 106.59(8) . . ? C2 Si1 C10 112.95(8) . . ? C9 Si1 C10 115.95(9) . . ? C3 C2 C7 119.18(17) . . ? C3 C2 Si1 131.91(15) . . ? C7 C2 Si1 108.89(14) . . ? C4 C3 C2 120.4(2) . . ? C5 C4 C3 120.1(2) . . ? C6 C5 C4 120.4(2) . . ? C5 C6 C7 120.3(2) . . ? C6 C7 C2 119.5(2) . . ? C6 C7 C8 123.83(19) . . ? C2 C7 C8 116.63(17) . . ? C7 C8 C9 110.41(16) . . ? C8 C9 Si1 105.04(13) . . ? C12 C10 C13 109.06(19) . . ? C12 C10 C11 109.68(19) . . ? C13 C10 C11 109.71(19) . . ? C12 C10 Si1 110.47(14) . . ? C13 C10 Si1 109.13(14) . . ? C11 C10 Si1 108.77(15) . . ? C15 O14 Si1 132.14(11) . . ? O14 C15 C16 110.36(14) . . ? O14 C15 C22 111.40(13) . . ? C16 C15 C22 111.34(14) . . ? O14 C15 C29 106.08(14) . . ? C16 C15 C29 109.70(14) . . ? C22 C15 C29 107.78(14) . . ? C17 C16 C15 177.40(19) . . ? C16 C17 Si18 177.07(18) . . ? C17 Si18 C21 108.72(11) . . ? C17 Si18 C19 107.16(12) . . ? C21 Si18 C19 111.75(14) . . ? C17 Si18 C20 108.00(11) . . ? C21 Si18 C20 110.79(13) . . ? C19 Si18 C20 110.26(15) . . ? C27 C22 C23 118.22(17) . . ? C27 C22 C15 121.53(16) . . ? C23 C22 C15 120.03(15) . . ? C24 C23 C22 121.30(17) . . ? C25 C24 C23 118.78(17) . . ? C24 C25 C26 121.39(18) . . ? C24 C25 Cl28 119.04(15) . . ? C26 C25 Cl28 119.54(15) . . ? C25 C26 C27 119.29(18) . . ? C26 C27 C22 121.01(18) . . ? C30 C29 C15 114.99(14) . . ? N31 C30 C35 122.42(18) . . ? N31 C30 C29 116.15(16) . . ? C35 C30 C29 121.41(18) . . ? C30 N31 C32 117.51(19) . . ? N31 C32 C33 123.6(2) . . ? C34 C33 C32 118.7(2) . . ? C33 C34 C35 119.0(2) . . ? C34 C35 C30 118.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O14 Si1 C2 C3 49.6(2) . . . . ? C9 Si1 C2 C3 169.45(19) . . . . ? C10 Si1 C2 C3 -70.4(2) . . . . ? O14 Si1 C2 C7 -128.81(13) . . . . ? C9 Si1 C2 C7 -8.96(15) . . . . ? C10 Si1 C2 C7 111.18(14) . . . . ? C7 C2 C3 C4 0.9(3) . . . . ? Si1 C2 C3 C4 -177.35(16) . . . . ? C2 C3 C4 C5 1.2(3) . . . . ? C3 C4 C5 C6 -1.9(3) . . . . ? C4 C5 C6 C7 0.5(3) . . . . ? C5 C6 C7 C2 1.6(3) . . . . ? C5 C6 C7 C8 -177.2(2) . . . . ? C3 C2 C7 C6 -2.3(3) . . . . ? Si1 C2 C7 C6 176.37(15) . . . . ? C3 C2 C7 C8 176.60(18) . . . . ? Si1 C2 C7 C8 -4.8(2) . . . . ? C6 C7 C8 C9 -161.12(19) . . . . ? C2 C7 C8 C9 20.1(3) . . . . ? C7 C8 C9 Si1 -24.4(2) . . . . ? O14 Si1 C9 C8 135.07(13) . . . . ? C2 Si1 C9 C8 19.01(15) . . . . ? C10 Si1 C9 C8 -98.65(15) . . . . ? O14 Si1 C10 C12 61.63(17) . . . . ? C2 Si1 C10 C12 -175.57(15) . . . . ? C9 Si1 C10 C12 -69.31(18) . . . . ? O14 Si1 C10 C13 -58.27(16) . . . . ? C2 Si1 C10 C13 64.54(17) . . . . ? C9 Si1 C10 C13 170.80(14) . . . . ? O14 Si1 C10 C11 -177.93(15) . . . . ? C2 Si1 C10 C11 -55.13(18) . . . . ? C9 Si1 C10 C11 51.13(18) . . . . ? C2 Si1 O14 C15 110.09(15) . . . . ? C9 Si1 O14 C15 4.64(17) . . . . ? C10 Si1 O14 C15 -126.22(15) . . . . ? Si1 O14 C15 C16 47.6(2) . . . . ? Si1 O14 C15 C22 -76.56(18) . . . . ? Si1 O14 C15 C29 166.42(11) . . . . ? O14 C15 C22 C27 155.79(17) . . . . ? C16 C15 C22 C27 32.1(2) . . . . ? C29 C15 C22 C27 -88.2(2) . . . . ? O14 C15 C22 C23 -29.6(2) . . . . ? C16 C15 C22 C23 -153.27(16) . . . . ? C29 C15 C22 C23 86.38(19) . . . . ? C27 C22 C23 C24 -0.2(3) . . . . ? C15 C22 C23 C24 -174.95(17) . . . . ? C22 C23 C24 C25 -0.4(3) . . . . ? C23 C24 C25 C26 0.9(3) . . . . ? C23 C24 C25 Cl28 -177.24(15) . . . . ? C24 C25 C26 C27 -0.7(3) . . . . ? Cl28 C25 C26 C27 177.39(16) . . . . ? C25 C26 C27 C22 0.1(3) . . . . ? C23 C22 C27 C26 0.3(3) . . . . ? C15 C22 C27 C26 175.03(18) . . . . ? O14 C15 C29 C30 -57.76(18) . . . . ? C16 C15 C29 C30 61.4(2) . . . . ? C22 C15 C29 C30 -177.18(14) . . . . ? C15 C29 C30 N31 95.01(19) . . . . ? C15 C29 C30 C35 -86.4(2) . . . . ? C35 C30 N31 C32 0.7(3) . . . . ? C29 C30 N31 C32 179.33(18) . . . . ? C30 N31 C32 C33 0.1(3) . . . . ? N31 C32 C33 C34 -0.9(4) . . . . ? C32 C33 C34 C35 0.8(4) . . . . ? C33 C34 C35 C30 0.0(3) . . . . ? N31 C30 C35 C34 -0.8(3) . . . . ? C29 C30 C35 C34 -179.28(18) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 68.18 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.331 _refine_diff_density_min -0.164 _refine_diff_density_rms 0.038 # Attachment 'OST4341.CIF' data_ost4341 _database_code_depnum_ccdc_archive 'CCDC 668298' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H39 N O2 Si2' _chemical_formula_weight 513.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.6545(4) _cell_length_b 21.6938(6) _cell_length_c 19.1708(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.885(1) _cell_angle_gamma 90.00 _cell_volume 5964.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14170 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 1.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7003 _exptl_absorpt_correction_T_max 0.7840 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \ scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55533 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 68.00 _reflns_number_total 10655 _reflns_number_gt 8195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Group C30 to c35 in molecule a refined with split positions using geometrical (AFIX 66) and thermal (ISOR) restraints. ; _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^)+(0.0522P)^2^+3.9486P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10655 _refine_ls_number_parameters 694 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.050 _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 Si1A Si 0.69290(4) 0.89423(3) 0.68112(3) 0.03790(16) Uani 1 1 d . . . C2A C 0.72963(17) 0.82283(11) 0.64066(13) 0.0421(6) Uani 1 1 d . . . C3A C 0.6800(2) 0.77529(12) 0.60060(15) 0.0528(7) Uani 1 1 d . . . H3A H 0.6146 0.7744 0.5936 0.063 Uiso 1 1 calc R . . C4A C 0.7258(2) 0.72951(14) 0.57118(17) 0.0653(8) Uani 1 1 d . . . H4A H 0.6915 0.6978 0.5443 0.078 Uiso 1 1 calc R . . C5A C 0.8217(2) 0.73032(15) 0.58122(18) 0.0689(9) Uani 1 1 d . . . H5A H 0.8526 0.6992 0.5610 0.083 Uiso 1 1 calc R . . C6A C 0.8723(2) 0.77639(14) 0.62070(17) 0.0625(8) Uani 1 1 d . . . H6A H 0.9377 0.7765 0.6277 0.075 Uiso 1 1 calc R . . C7A C 0.82698(18) 0.82296(12) 0.65043(14) 0.0475(6) Uani 1 1 d . . . C8A C 0.87860(19) 0.87566(14) 0.69253(16) 0.0602(8) Uani 1 1 d . . . H8A1 H 0.9053 0.9022 0.6605 0.072 Uiso 1 1 calc R . . H8A2 H 0.9300 0.8593 0.7287 0.072 Uiso 1 1 calc R . . C9A C 0.81352(17) 0.91416(12) 0.72924(14) 0.0466(6) Uani 1 1 d . . . H9A1 H 0.8255 0.9583 0.7251 0.056 Uiso 1 1 calc R . . H9A2 H 0.8225 0.9034 0.7799 0.056 Uiso 1 1 calc R . . C10A C 0.64208(18) 0.95165(12) 0.61020(14) 0.0483(6) Uani 1 1 d . . . C11A C 0.6220(2) 1.01293(13) 0.64342(18) 0.0665(8) Uani 1 1 d . . . H11A H 0.5963 1.0419 0.6060 0.100 Uiso 1 1 calc R . . H11B H 0.6794 1.0294 0.6716 0.100 Uiso 1 1 calc R . . H11C H 0.5776 1.0064 0.6738 0.100 Uiso 1 1 calc R . . C12A C 0.7134(2) 0.96300(15) 0.56280(16) 0.0709(9) Uani 1 1 d . . . H12A H 0.7293 0.9241 0.5434 0.106 Uiso 1 1 calc R . . H12B H 0.7692 0.9816 0.5910 0.106 Uiso 1 1 calc R . . H12C H 0.6866 0.9905 0.5241 0.106 Uiso 1 1 calc R . . C13A C 0.5521(2) 0.92571(16) 0.56384(17) 0.0741(9) Uani 1 1 d . . . H13A H 0.5304 0.9532 0.5240 0.111 Uiso 1 1 calc R . . H13B H 0.5046 0.9222 0.5922 0.111 Uiso 1 1 calc R . . H13C H 0.5644 0.8853 0.5461 0.111 Uiso 1 1 calc R . . O14A O 0.61186(10) 0.88708(7) 0.72871(8) 0.0391(4) Uani 1 1 d . . . C15A C 0.60420(16) 0.85051(10) 0.78937(12) 0.0360(5) Uani 1 1 d . B . C16A C 0.69056(16) 0.81442(11) 0.81430(12) 0.0377(5) Uani 1 1 d . . . C17A C 0.76086(17) 0.78581(11) 0.83406(13) 0.0431(6) Uani 1 1 d . . . Si8A Si 0.87033(5) 0.74414(4) 0.86751(4) 0.04916(19) Uani 1 1 d . . . C19A C 0.8560(3) 0.69977(18) 0.94745(19) 0.0876(11) Uani 1 1 d . . . H19A H 0.8408 0.7278 0.9828 0.131 Uiso 1 1 calc R . . H19B H 0.9136 0.6784 0.9672 0.131 Uiso 1 1 calc R . . H19C H 0.8061 0.6700 0.9340 0.131 Uiso 1 1 calc R . . C20A C 0.9652(2) 0.80144(18) 0.8918(2) 0.0872(11) Uani 1 1 d . . . H20A H 0.9821 0.8172 0.8488 0.131 Uiso 1 1 calc R . . H20B H 1.0191 0.7820 0.9215 0.131 Uiso 1 1 calc R . . H20C H 0.9442 0.8351 0.9178 0.131 Uiso 1 1 calc R . . C21A C 0.8933(2) 0.69214(17) 0.79632(19) 0.0805(10) Uani 1 1 d . . . H21A H 0.8471 0.6595 0.7884 0.121 Uiso 1 1 calc R . . H21B H 0.9550 0.6744 0.8107 0.121 Uiso 1 1 calc R . . H21C H 0.8897 0.7154 0.7526 0.121 Uiso 1 1 calc R . . C22A C 0.52041(15) 0.80672(10) 0.76798(12) 0.0365(5) Uani 1 1 d . . . C23A C 0.49669(16) 0.76375(11) 0.81587(13) 0.0400(5) Uani 1 1 d . . . C24A C 0.42116(17) 0.72440(12) 0.79459(15) 0.0486(6) Uani 1 1 d . . . H24A H 0.4062 0.6954 0.8269 0.058 Uiso 1 1 calc R . . C25A C 0.36813(18) 0.72780(13) 0.72641(16) 0.0550(7) Uani 1 1 d . . . H25A H 0.3173 0.7010 0.7122 0.066 Uiso 1 1 calc R . . C26A C 0.38951(18) 0.77031(13) 0.67917(15) 0.0536(7) Uani 1 1 d . . . H26A H 0.3528 0.7731 0.6329 0.064 Uiso 1 1 calc R . . C27A C 0.46540(17) 0.80906(11) 0.70001(13) 0.0438(6) Uani 1 1 d . . . H27A H 0.4799 0.8377 0.6671 0.053 Uiso 1 1 calc R . . O28A O 0.55110(12) 0.76331(8) 0.88286(9) 0.0525(5) Uani 1 1 d . . . C28A C 0.5346(2) 0.71726(13) 0.93106(15) 0.0630(8) Uani 1 1 d . . . H28A H 0.4756 0.7252 0.9448 0.094 Uiso 1 1 calc R . . H28B H 0.5844 0.7178 0.9731 0.094 Uiso 1 1 calc R . . H28C H 0.5325 0.6772 0.9083 0.094 Uiso 1 1 calc R . . C29A C 0.58543(17) 0.89597(11) 0.84720(13) 0.0422(6) Uani 1 1 d . . . H29A H 0.5248 0.9158 0.8303 0.051 Uiso 1 1 calc R A 1 H29B H 0.5821 0.8728 0.8905 0.051 Uiso 1 1 calc R A 1 C30A C 0.6596(3) 0.94510(16) 0.8654(2) 0.0343(17) Uani 0.578(9) 1 d PGU B 1 N31A N 0.7392(3) 0.92924(15) 0.9151(3) 0.0647(17) Uani 0.578(9) 1 d PGU B 1 C32A C 0.8127(3) 0.9708(2) 0.9321(3) 0.0740(19) Uani 0.578(9) 1 d PGU B 1 H32A H 0.8665 0.9601 0.9657 0.089 Uiso 0.578(9) 1 calc PR B 1 C33A C 0.8064(4) 1.0282(2) 0.8992(3) 0.076(2) Uani 0.578(9) 1 d PGU B 1 H33A H 0.8561 1.0563 0.9107 0.091 Uiso 0.578(9) 1 calc PR B 1 C34A C 0.7268(5) 1.04406(17) 0.8495(2) 0.077(2) Uani 0.578(9) 1 d PGU B 1 H34A H 0.7225 1.0829 0.8273 0.092 Uiso 0.578(9) 1 calc PR B 1 C35A C 0.6533(4) 1.00251(18) 0.83257(19) 0.0602(17) Uani 0.578(9) 1 d PGU B 1 H35A H 0.5995 1.0132 0.7989 0.072 Uiso 0.578(9) 1 calc PR B 1 C30C C 0.6464(5) 0.9464(2) 0.8623(4) 0.083(5) Uani 0.422(9) 1 d PGU B 2 N31C N 0.6083(4) 1.0035(3) 0.8397(3) 0.060(2) Uani 0.422(9) 1 d PGU B 2 C32C C 0.6640(6) 1.0560(2) 0.8497(3) 0.075(3) Uani 0.422(9) 1 d PGU B 2 H32C H 0.6382 1.0946 0.8344 0.090 Uiso 0.422(9) 1 calc PR B 2 C33C C 0.7577(5) 1.0514(3) 0.8822(4) 0.074(3) Uani 0.422(9) 1 d PGU B 2 H33C H 0.7953 1.0868 0.8889 0.089 Uiso 0.422(9) 1 calc PR B 2 C34C C 0.7958(4) 0.9943(4) 0.9048(4) 0.073(3) Uani 0.422(9) 1 d PGU B 2 H34C H 0.8591 0.9912 0.9267 0.088 Uiso 0.422(9) 1 calc PR B 2 C35C C 0.7402(5) 0.9418(3) 0.8948(5) 0.067(3) Uani 0.422(9) 1 d PGU B 2 H35C H 0.7659 0.9032 0.9100 0.080 Uiso 0.422(9) 1 calc PR B 2 Si1B Si 0.19290(4) 0.96843(3) 0.67808(3) 0.03516(16) Uani 1 1 d . . . C2B C 0.22940(17) 1.04203(11) 0.64160(13) 0.0418(6) Uani 1 1 d . . . C3B C 0.1798(2) 1.08855(12) 0.60088(14) 0.0520(7) Uani 1 1 d . . . H3B H 0.1144 1.0859 0.5878 0.062 Uiso 1 1 calc R . . C4B C 0.2250(3) 1.13879(14) 0.57926(17) 0.0667(9) Uani 1 1 d . . . H4B H 0.1909 1.1704 0.5522 0.080 Uiso 1 1 calc R . . C5B C 0.3214(3) 1.14177(15) 0.59810(19) 0.0755(10) Uani 1 1 d . . . H5B H 0.3528 1.1756 0.5834 0.091 Uiso 1 1 calc R . . C6B C 0.3713(2) 1.09623(16) 0.63769(19) 0.0715(9) Uani 1 1 d . . . H6B H 0.4367 1.0989 0.6497 0.086 Uiso 1 1 calc R . . C7B C 0.32669(19) 1.04606(13) 0.66035(15) 0.0533(7) Uani 1 1 d . . . C8B C 0.37831(19) 0.99420(16) 0.70484(19) 0.0694(9) Uani 1 1 d . . . H8B1 H 0.4221 1.0117 0.7456 0.083 Uiso 1 1 calc R . . H8B2 H 0.4144 0.9709 0.6760 0.083 Uiso 1 1 calc R . . C9B C 0.31139(16) 0.95046(12) 0.73199(14) 0.0474(6) Uani 1 1 d . . . H9B1 H 0.3134 0.9574 0.7828 0.057 Uiso 1 1 calc R . . H9B2 H 0.3279 0.9074 0.7252 0.057 Uiso 1 1 calc R . . C10B C 0.15063(17) 0.90911(11) 0.60687(12) 0.0406(5) Uani 1 1 d . . . C11B C 0.0607(2) 0.93076(15) 0.55716(15) 0.0646(8) Uani 1 1 d . . . H11D H 0.0403 0.8998 0.5207 0.097 Uiso 1 1 calc R . . H11E H 0.0722 0.9693 0.5348 0.097 Uiso 1 1 calc R . . H11F H 0.0126 0.9368 0.5845 0.097 Uiso 1 1 calc R . . C12B C 0.2265(2) 0.90016(13) 0.56296(15) 0.0569(7) Uani 1 1 d . . . H12D H 0.2840 0.8872 0.5942 0.085 Uiso 1 1 calc R . . H12E H 0.2366 0.9387 0.5401 0.085 Uiso 1 1 calc R . . H12F H 0.2066 0.8689 0.5269 0.085 Uiso 1 1 calc R . . C13B C 0.1334(2) 0.84755(12) 0.64057(15) 0.0541(7) Uani 1 1 d . . . H13D H 0.0881 0.8531 0.6704 0.081 Uiso 1 1 calc R . . H13E H 0.1914 0.8325 0.6693 0.081 Uiso 1 1 calc R . . H13F H 0.1098 0.8179 0.6033 0.081 Uiso 1 1 calc R . . O14B O 0.10585(10) 0.97526(7) 0.71983(8) 0.0374(4) Uani 1 1 d . . . C15B C 0.09484(15) 1.01005(10) 0.78038(12) 0.0359(5) Uani 1 1 d . . . C16B C 0.17974(16) 1.04609(11) 0.80999(12) 0.0376(5) Uani 1 1 d . . . C17B C 0.24878(18) 1.07418(12) 0.83599(14) 0.0462(6) Uani 1 1 d . . . Si8B Si 0.35179(6) 1.11485(4) 0.88492(5) 0.0647(2) Uani 1 1 d . . . C19B C 0.4305(3) 1.0563(2) 0.9371(3) 0.1208(17) Uani 1 1 d . . . H19D H 0.3958 1.0317 0.9649 0.181 Uiso 1 1 calc R . . H19E H 0.4815 1.0770 0.9688 0.181 Uiso 1 1 calc R . . H19F H 0.4554 1.0298 0.9047 0.181 Uiso 1 1 calc R . . C20B C 0.4087(3) 1.1574(2) 0.8219(2) 0.1116(15) Uani 1 1 d . . . H20D H 0.4346 1.1282 0.7929 0.167 Uiso 1 1 calc R . . H20E H 0.4582 1.1829 0.8484 0.167 Uiso 1 1 calc R . . H20F H 0.3631 1.1832 0.7915 0.167 Uiso 1 1 calc R . . C21B C 0.3120(3) 1.16922(17) 0.94677(19) 0.0970(13) Uani 1 1 d . . . H21D H 0.2751 1.2016 0.9197 0.146 Uiso 1 1 calc R . . H21E H 0.3657 1.1872 0.9783 0.146 Uiso 1 1 calc R . . H21F H 0.2744 1.1473 0.9748 0.146 Uiso 1 1 calc R . . C22B C 0.01155(16) 1.05391(11) 0.75832(13) 0.0401(5) Uani 1 1 d . . . C23B C -0.01269(18) 1.09654(12) 0.80623(15) 0.0497(6) Uani 1 1 d . . . C24B C -0.0856(2) 1.13750(13) 0.78439(19) 0.0625(8) Uani 1 1 d . . . H24B H -0.1005 1.1665 0.8167 0.075 Uiso 1 1 calc R . . C25B C -0.1361(2) 1.13563(14) 0.7156(2) 0.0673(9) Uani 1 1 d . . . H25B H -0.1850 1.1638 0.7009 0.081 Uiso 1 1 calc R . . C26B C -0.11566(19) 1.09295(13) 0.66830(18) 0.0627(8) Uani 1 1 d . . . H26B H -0.1517 1.0909 0.6217 0.075 Uiso 1 1 calc R . . C27B C -0.04133(17) 1.05271(12) 0.68972(15) 0.0472(6) Uani 1 1 d . . . H27B H -0.0267 1.0241 0.6569 0.057 Uiso 1 1 calc R . . O28B O 0.03939(15) 1.09488(9) 0.87425(11) 0.0654(6) Uani 1 1 d . . . C28B C 0.0283(3) 1.14241(16) 0.92228(19) 0.0821(10) Uani 1 1 d . . . H28D H 0.0312 1.1821 0.8995 0.123 Uiso 1 1 calc R . . H28E H 0.0777 1.1398 0.9645 0.123 Uiso 1 1 calc R . . H28F H -0.0316 1.1380 0.9358 0.123 Uiso 1 1 calc R . . C29B C 0.07430(17) 0.96269(11) 0.83605(13) 0.0434(6) Uani 1 1 d . . . H29C H 0.0624 0.9850 0.8777 0.052 Uiso 1 1 calc R . . H29D H 0.0176 0.9397 0.8153 0.052 Uiso 1 1 calc R . . C30B C 0.15258(18) 0.91790(12) 0.85990(13) 0.0461(6) Uani 1 1 d . . . N31B N 0.14936(18) 0.86527(11) 0.82334(13) 0.0619(6) Uani 1 1 d . . . C32B C 0.2215(3) 0.82637(16) 0.84235(19) 0.0836(11) Uani 1 1 d . . . H32B H 0.2205 0.7892 0.8170 0.100 Uiso 1 1 calc R . . C33B C 0.2960(3) 0.8376(2) 0.8961(2) 0.0946(13) Uani 1 1 d . . . H33B H 0.3451 0.8090 0.9069 0.114 Uiso 1 1 calc R . . C34B C 0.2983(3) 0.8906(2) 0.9339(2) 0.0901(12) Uani 1 1 d . . . H34B H 0.3488 0.8993 0.9715 0.108 Uiso 1 1 calc R . . C35B C 0.2246(2) 0.93182(15) 0.91601(16) 0.0656(8) Uani 1 1 d . . . H35B H 0.2239 0.9686 0.9418 0.079 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 Si1A 0.0405(4) 0.0350(4) 0.0402(3) 0.0024(3) 0.0130(3) -0.0044(3) C2A 0.0452(14) 0.0410(14) 0.0424(13) 0.0016(11) 0.0139(11) -0.0046(11) C3A 0.0562(16) 0.0476(16) 0.0567(16) -0.0042(13) 0.0167(13) -0.0076(13) C4A 0.083(2) 0.0481(18) 0.0671(19) -0.0141(15) 0.0215(17) -0.0064(16) C5A 0.080(2) 0.059(2) 0.073(2) -0.0097(16) 0.0296(18) 0.0096(17) C6A 0.0566(17) 0.065(2) 0.070(2) -0.0040(16) 0.0240(15) 0.0096(15) C7A 0.0490(15) 0.0490(16) 0.0476(14) -0.0006(12) 0.0169(12) -0.0010(12) C8A 0.0461(15) 0.068(2) 0.0689(19) -0.0121(16) 0.0177(14) -0.0085(14) C9A 0.0460(14) 0.0463(15) 0.0502(15) -0.0026(12) 0.0163(12) -0.0094(11) C10A 0.0578(16) 0.0400(14) 0.0475(14) 0.0084(12) 0.0116(12) -0.0066(12) C11A 0.075(2) 0.0454(17) 0.081(2) 0.0128(15) 0.0200(17) 0.0069(15) C12A 0.097(2) 0.064(2) 0.0577(18) 0.0161(15) 0.0318(18) -0.0081(17) C13A 0.078(2) 0.070(2) 0.064(2) 0.0251(17) -0.0081(17) -0.0067(17) O14A 0.0398(9) 0.0368(9) 0.0424(9) 0.0081(7) 0.0128(7) 0.0013(7) C15A 0.0381(12) 0.0319(12) 0.0392(12) 0.0052(10) 0.0110(10) 0.0002(10) C16A 0.0381(13) 0.0352(13) 0.0402(13) 0.0017(10) 0.0093(10) -0.0027(10) C17A 0.0419(14) 0.0395(14) 0.0481(14) 0.0027(11) 0.0094(11) -0.0033(11) Si8A 0.0376(4) 0.0555(5) 0.0534(4) 0.0121(3) 0.0072(3) 0.0050(3) C19A 0.080(2) 0.103(3) 0.077(2) 0.042(2) 0.0118(19) 0.015(2) C20A 0.0528(19) 0.107(3) 0.096(3) 0.003(2) 0.0020(18) -0.0158(19) C21A 0.075(2) 0.079(2) 0.092(3) 0.002(2) 0.0273(19) 0.0286(18) C22A 0.0343(12) 0.0331(12) 0.0431(13) 0.0014(10) 0.0100(10) 0.0027(10) C23A 0.0385(13) 0.0366(13) 0.0453(14) 0.0025(11) 0.0093(11) 0.0006(10) C24A 0.0476(14) 0.0398(15) 0.0610(17) 0.0044(12) 0.0172(13) -0.0074(11) C25A 0.0403(14) 0.0499(17) 0.0712(19) -0.0038(14) 0.0031(13) -0.0108(12) C26A 0.0458(15) 0.0523(17) 0.0576(17) -0.0009(13) -0.0013(13) -0.0023(13) C27A 0.0424(13) 0.0410(14) 0.0472(14) 0.0025(11) 0.0076(11) 0.0009(11) O28A 0.0597(11) 0.0507(11) 0.0451(10) 0.0115(8) 0.0066(9) -0.0148(9) C28A 0.085(2) 0.0492(17) 0.0534(17) 0.0163(14) 0.0113(15) -0.0088(15) C29A 0.0487(14) 0.0359(13) 0.0454(14) -0.0007(11) 0.0178(11) -0.0023(11) C30A 0.047(3) 0.031(3) 0.030(3) -0.0082(19) 0.020(2) -0.017(2) N31A 0.066(3) 0.062(3) 0.063(3) -0.013(2) 0.006(2) -0.015(2) C32A 0.074(3) 0.072(4) 0.068(3) -0.007(3) -0.006(3) -0.018(3) C33A 0.085(4) 0.059(4) 0.084(4) -0.001(3) 0.015(3) -0.020(3) C34A 0.095(4) 0.066(3) 0.067(4) 0.011(3) 0.011(3) -0.017(3) C35A 0.072(3) 0.047(3) 0.061(3) 0.002(2) 0.014(3) -0.018(3) C30C 0.089(6) 0.085(6) 0.076(6) -0.006(4) 0.020(4) 0.008(4) N31C 0.074(4) 0.047(3) 0.061(3) 0.002(2) 0.017(3) -0.019(3) C32C 0.088(5) 0.059(4) 0.076(4) -0.005(3) 0.016(4) -0.019(3) C33C 0.077(5) 0.073(4) 0.070(4) -0.002(4) 0.011(4) -0.020(4) C34C 0.065(4) 0.078(5) 0.073(5) -0.020(4) 0.006(3) -0.010(4) C35C 0.071(4) 0.064(4) 0.071(4) -0.018(3) 0.024(4) -0.016(3) Si1B 0.0341(3) 0.0345(3) 0.0373(3) -0.0012(3) 0.0082(3) 0.0021(3) C2B 0.0456(14) 0.0399(14) 0.0433(13) -0.0056(11) 0.0167(11) -0.0016(11) C3B 0.0595(16) 0.0452(16) 0.0556(16) 0.0025(13) 0.0215(14) 0.0074(13) C4B 0.099(3) 0.0431(17) 0.0667(19) 0.0096(14) 0.0363(18) 0.0064(16) C5B 0.096(3) 0.052(2) 0.091(2) -0.0039(18) 0.048(2) -0.0237(18) C6B 0.0593(19) 0.069(2) 0.090(2) 0.0015(19) 0.0251(18) -0.0179(16) C7B 0.0489(15) 0.0523(17) 0.0611(17) -0.0051(13) 0.0170(13) -0.0095(13) C8B 0.0406(15) 0.077(2) 0.088(2) 0.0096(18) 0.0075(15) -0.0040(15) C9B 0.0395(13) 0.0507(16) 0.0503(15) -0.0018(12) 0.0057(11) 0.0083(11) C10B 0.0446(13) 0.0390(14) 0.0385(13) -0.0031(10) 0.0092(11) 0.0034(11) C11B 0.0674(19) 0.066(2) 0.0526(17) -0.0156(15) -0.0057(14) 0.0101(15) C12B 0.0685(18) 0.0561(18) 0.0533(16) -0.0061(13) 0.0294(14) -0.0030(14) C13B 0.0643(17) 0.0468(16) 0.0553(16) -0.0098(13) 0.0216(14) -0.0090(13) O14B 0.0360(8) 0.0377(9) 0.0393(9) -0.0071(7) 0.0093(7) -0.0023(7) C15B 0.0375(12) 0.0320(12) 0.0395(12) -0.0048(10) 0.0108(10) 0.0006(10) C16B 0.0422(13) 0.0344(13) 0.0358(12) -0.0026(10) 0.0074(10) 0.0033(11) C17B 0.0480(15) 0.0406(14) 0.0477(15) -0.0018(12) 0.0045(12) 0.0027(12) Si8B 0.0553(5) 0.0575(5) 0.0684(5) -0.0047(4) -0.0171(4) -0.0107(4) C19B 0.079(3) 0.104(3) 0.149(4) 0.005(3) -0.047(3) 0.011(2) C20B 0.086(3) 0.126(4) 0.122(4) -0.012(3) 0.020(2) -0.057(3) C21B 0.136(4) 0.073(2) 0.067(2) -0.0161(19) -0.014(2) -0.013(2) C22B 0.0360(12) 0.0340(13) 0.0530(15) 0.0013(11) 0.0153(11) 0.0001(10) C23B 0.0475(15) 0.0421(15) 0.0639(18) -0.0022(13) 0.0217(13) 0.0011(12) C24B 0.0568(17) 0.0449(17) 0.094(2) -0.0014(16) 0.0335(17) 0.0098(13) C25B 0.0471(16) 0.0463(18) 0.109(3) 0.0152(18) 0.0173(18) 0.0129(13) C26B 0.0459(16) 0.0506(18) 0.085(2) 0.0143(16) -0.0029(15) 0.0006(13) C27B 0.0398(13) 0.0403(14) 0.0601(16) 0.0033(12) 0.0069(12) -0.0034(11) O28B 0.0793(14) 0.0603(13) 0.0604(12) -0.0167(10) 0.0231(11) 0.0157(10) C28B 0.101(3) 0.071(2) 0.080(2) -0.0298(19) 0.032(2) 0.0003(19) C29B 0.0494(14) 0.0404(14) 0.0437(14) -0.0010(11) 0.0170(12) 0.0001(11) C30B 0.0594(16) 0.0393(14) 0.0432(14) 0.0069(11) 0.0190(12) 0.0035(12) N31B 0.0890(18) 0.0418(14) 0.0571(14) 0.0024(11) 0.0205(13) 0.0138(12) C32B 0.129(3) 0.061(2) 0.068(2) 0.0140(17) 0.036(2) 0.040(2) C33B 0.106(3) 0.095(3) 0.085(3) 0.040(2) 0.025(2) 0.055(3) C34B 0.088(3) 0.093(3) 0.076(2) 0.030(2) -0.012(2) 0.014(2) C35B 0.082(2) 0.0550(19) 0.0525(17) 0.0114(14) -0.0027(16) 0.0042(16) _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 Si1A O14A 1.6471(15) . ? Si1A C2A 1.861(3) . ? Si1A C9A 1.868(3) . ? Si1A C10A 1.881(3) . ? C2A C3A 1.397(4) . ? C2A C7A 1.400(3) . ? C3A C4A 1.382(4) . ? C4A C5A 1.378(4) . ? C5A C6A 1.375(4) . ? C6A C7A 1.394(4) . ? C7A C8A 1.510(4) . ? C8A C9A 1.543(4) . ? C10A C11A 1.529(4) . ? C10A C13A 1.538(4) . ? C10A C12A 1.539(4) . ? O14A C15A 1.431(3) . ? C15A C16A 1.481(3) . ? C15A C22A 1.540(3) . ? C15A C29A 1.550(3) . ? C16A C17A 1.196(3) . ? C17A Si8A 1.838(3) . ? Si8A C20A 1.852(3) . ? Si8A C21A 1.854(3) . ? Si8A C19A 1.858(3) . ? C22A C27A 1.385(3) . ? C22A C23A 1.401(3) . ? C23A O28A 1.365(3) . ? C23A C24A 1.391(3) . ? C24A C25A 1.378(4) . ? C25A C26A 1.373(4) . ? C26A C27A 1.386(4) . ? O28A C28A 1.415(3) . ? C29A C30C 1.405(5) . ? C29A C30A 1.511(4) . ? C30A N31A 1.3900 . ? C30A C35A 1.3900 . ? N31A C32A 1.3900 . ? C32A C33A 1.3900 . ? C33A C34A 1.3900 . ? C34A C35A 1.3900 . ? C30C N31C 1.3900 . ? C30C C35C 1.3900 . ? N31C C32C 1.3900 . ? C32C C33C 1.3900 . ? C33C C34C 1.3900 . ? C34C C35C 1.3900 . ? Si1B O14B 1.6465(15) . ? Si1B C2B 1.865(2) . ? Si1B C9B 1.870(2) . ? Si1B C10B 1.886(2) . ? C2B C3B 1.387(4) . ? C2B C7B 1.399(4) . ? C3B C4B 1.383(4) . ? C4B C5B 1.386(5) . ? C5B C6B 1.363(5) . ? C6B C7B 1.385(4) . ? C7B C8B 1.517(4) . ? C8B C9B 1.531(4) . ? C10B C13B 1.527(4) . ? C10B C11B 1.533(4) . ? C10B C12B 1.538(3) . ? O14B C15B 1.421(3) . ? C15B C16B 1.480(3) . ? C15B C22B 1.537(3) . ? C15B C29B 1.555(3) . ? C16B C17B 1.198(3) . ? C17B Si8B 1.831(3) . ? Si8B C20B 1.849(4) . ? Si8B C21B 1.850(4) . ? Si8B C19B 1.862(4) . ? C22B C27B 1.382(3) . ? C22B C23B 1.400(3) . ? C23B O28B 1.369(3) . ? C23B C24B 1.387(4) . ? C24B C25B 1.372(4) . ? C25B C26B 1.372(4) . ? C26B C27B 1.390(4) . ? O28B C28B 1.414(3) . ? C29B C30B 1.501(3) . ? C30B N31B 1.335(3) . ? C30B C35B 1.376(4) . ? N31B C32B 1.343(4) . ? C32B C33B 1.359(6) . ? C33B C34B 1.356(6) . ? C34B C35B 1.390(5) . ? 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 O14A Si1A C2A 117.12(10) . . ? O14A Si1A C9A 117.72(10) . . ? C2A Si1A C9A 94.18(11) . . ? O14A Si1A C10A 103.86(10) . . ? C2A Si1A C10A 110.81(12) . . ? C9A Si1A C10A 113.40(12) . . ? C3A C2A C7A 118.4(2) . . ? C3A C2A Si1A 132.9(2) . . ? C7A C2A Si1A 108.46(18) . . ? C4A C3A C2A 120.9(3) . . ? C5A C4A C3A 120.0(3) . . ? C6A C5A C4A 120.3(3) . . ? C5A C6A C7A 120.2(3) . . ? C6A C7A C2A 120.1(3) . . ? C6A C7A C8A 122.6(2) . . ? C2A C7A C8A 117.3(2) . . ? C7A C8A C9A 111.4(2) . . ? C8A C9A Si1A 105.10(17) . . ? C11A C10A C13A 110.1(3) . . ? C11A C10A C12A 108.6(2) . . ? C13A C10A C12A 108.9(2) . . ? C11A C10A Si1A 110.87(19) . . ? C13A C10A Si1A 109.90(18) . . ? C12A C10A Si1A 108.5(2) . . ? C15A O14A Si1A 133.51(14) . . ? O14A C15A C16A 110.51(18) . . ? O14A C15A C22A 108.50(18) . . ? C16A C15A C22A 109.95(18) . . ? O14A C15A C29A 106.48(18) . . ? C16A C15A C29A 111.8(2) . . ? C22A C15A C29A 109.50(18) . . ? C17A C16A C15A 179.2(3) . . ? C16A C17A Si8A 177.6(2) . . ? C17A Si8A C20A 108.29(15) . . ? C17A Si8A C21A 108.66(14) . . ? C20A Si8A C21A 110.66(17) . . ? C17A Si8A C19A 107.69(14) . . ? C20A Si8A C19A 110.31(18) . . ? C21A Si8A C19A 111.12(18) . . ? C27A C22A C23A 117.8(2) . . ? C27A C22A C15A 120.4(2) . . ? C23A C22A C15A 121.9(2) . . ? O28A C23A C24A 123.2(2) . . ? O28A C23A C22A 116.4(2) . . ? C24A C23A C22A 120.4(2) . . ? C25A C24A C23A 120.3(2) . . ? C26A C25A C24A 120.0(2) . . ? C25A C26A C27A 119.7(3) . . ? C22A C27A C26A 121.8(2) . . ? C23A O28A C28A 118.3(2) . . ? C30C C29A C30A 6.3(4) . . ? C30C C29A C15A 116.3(4) . . ? C30A C29A C15A 112.9(2) . . ? N31A C30A C35A 120.0 . . ? N31A C30A C29A 116.5(3) . . ? C35A C30A C29A 123.4(3) . . ? C30A N31A C32A 120.0 . . ? N31A C32A C33A 120.0 . . ? C34A C33A C32A 120.0 . . ? C33A C34A C35A 120.0 . . ? C34A C35A C30A 120.0 . . ? N31C C30C C35C 120.0 . . ? N31C C30C C29A 115.6(4) . . ? C35C C30C C29A 124.4(4) . . ? C30C N31C C32C 120.0 . . ? C33C C32C N31C 120.0 . . ? C34C C33C C32C 120.0 . . ? C33C C34C C35C 120.0 . . ? C34C C35C C30C 120.0 . . ? O14B Si1B C2B 114.59(9) . . ? O14B Si1B C9B 118.32(10) . . ? C2B Si1B C9B 94.61(12) . . ? O14B Si1B C10B 103.98(9) . . ? C2B Si1B C10B 112.93(11) . . ? C9B Si1B C10B 112.77(11) . . ? C3B C2B C7B 119.2(2) . . ? C3B C2B Si1B 132.6(2) . . ? C7B C2B Si1B 108.23(19) . . ? C4B C3B C2B 120.9(3) . . ? C3B C4B C5B 119.0(3) . . ? C6B C5B C4B 120.8(3) . . ? C5B C6B C7B 120.7(3) . . ? C6B C7B C2B 119.4(3) . . ? C6B C7B C8B 123.1(3) . . ? C2B C7B C8B 117.5(2) . . ? C7B C8B C9B 111.8(2) . . ? C8B C9B Si1B 105.66(18) . . ? C13B C10B C11B 109.6(2) . . ? C13B C10B C12B 108.8(2) . . ? C11B C10B C12B 108.9(2) . . ? C13B C10B Si1B 110.41(17) . . ? C11B C10B Si1B 110.69(17) . . ? C12B C10B Si1B 108.41(17) . . ? C15B O14B Si1B 132.41(14) . . ? O14B C15B C16B 111.47(17) . . ? O14B C15B C22B 108.75(18) . . ? C16B C15B C22B 109.61(19) . . ? O14B C15B C29B 106.28(18) . . ? C16B C15B C29B 110.61(19) . . ? C22B C15B C29B 110.06(18) . . ? C17B C16B C15B 177.8(3) . . ? C16B C17B Si8B 173.9(2) . . ? C17B Si8B C20B 109.92(16) . . ? C17B Si8B C21B 107.47(16) . . ? C20B Si8B C21B 110.2(2) . . ? C17B Si8B C19B 107.51(16) . . ? C20B Si8B C19B 112.2(2) . . ? C21B Si8B C19B 109.4(2) . . ? C27B C22B C23B 117.9(2) . . ? C27B C22B C15B 120.5(2) . . ? C23B C22B C15B 121.5(2) . . ? O28B C23B C24B 123.3(3) . . ? O28B C23B C22B 116.1(2) . . ? C24B C23B C22B 120.6(3) . . ? C25B C24B C23B 120.0(3) . . ? C26B C25B C24B 120.5(3) . . ? C25B C26B C27B 119.5(3) . . ? C22B C27B C26B 121.4(3) . . ? C23B O28B C28B 119.0(2) . . ? C30B C29B C15B 113.14(19) . . ? N31B C30B C35B 122.4(3) . . ? N31B C30B C29B 116.8(2) . . ? C35B C30B C29B 120.7(2) . . ? C30B N31B C32B 117.0(3) . . ? N31B C32B C33B 123.9(3) . . ? C34B C33B C32B 119.0(3) . . ? C33B C34B C35B 118.8(4) . . ? C30B C35B C34B 118.9(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 O14A Si1A C2A C3A 48.9(3) . . . . ? C9A Si1A C2A C3A 173.0(3) . . . . ? C10A Si1A C2A C3A -70.0(3) . . . . ? O14A Si1A C2A C7A -136.54(17) . . . . ? C9A Si1A C2A C7A -12.38(19) . . . . ? C10A Si1A C2A C7A 104.61(19) . . . . ? C7A C2A C3A C4A -0.1(4) . . . . ? Si1A C2A C3A C4A 174.1(2) . . . . ? C2A C3A C4A C5A 0.0(5) . . . . ? C3A C4A C5A C6A 0.3(5) . . . . ? C4A C5A C6A C7A -0.5(5) . . . . ? C5A C6A C7A C2A 0.4(4) . . . . ? C5A C6A C7A C8A -178.3(3) . . . . ? C3A C2A C7A C6A -0.1(4) . . . . ? Si1A C2A C7A C6A -175.6(2) . . . . ? C3A C2A C7A C8A 178.7(2) . . . . ? Si1A C2A C7A C8A 3.2(3) . . . . ? C6A C7A C8A C9A -170.7(3) . . . . ? C2A C7A C8A C9A 10.6(4) . . . . ? C7A C8A C9A Si1A -18.3(3) . . . . ? O14A Si1A C9A C8A 141.05(17) . . . . ? C2A Si1A C9A C8A 17.3(2) . . . . ? C10A Si1A C9A C8A -97.5(2) . . . . ? O14A Si1A C10A C11A 59.8(2) . . . . ? C2A Si1A C10A C11A -173.64(18) . . . . ? C9A Si1A C10A C11A -69.2(2) . . . . ? O14A Si1A C10A C13A -62.1(2) . . . . ? C2A Si1A C10A C13A 64.4(2) . . . . ? C9A Si1A C10A C13A 168.9(2) . . . . ? O14A Si1A C10A C12A 178.95(19) . . . . ? C2A Si1A C10A C12A -54.5(2) . . . . ? C9A Si1A C10A C12A 50.0(2) . . . . ? C2A Si1A O14A C15A 56.2(2) . . . . ? C9A Si1A O14A C15A -55.0(2) . . . . ? C10A Si1A O14A C15A 178.8(2) . . . . ? Si1A O14A C15A C16A 3.0(3) . . . . ? Si1A O14A C15A C22A -117.59(19) . . . . ? Si1A O14A C15A C29A 124.64(19) . . . . ? O14A C15A C22A C27A -2.2(3) . . . . ? C16A C15A C22A C27A -123.2(2) . . . . ? C29A C15A C22A C27A 113.6(2) . . . . ? O14A C15A C22A C23A 178.19(19) . . . . ? C16A C15A C22A C23A 57.2(3) . . . . ? C29A C15A C22A C23A -66.0(3) . . . . ? C27A C22A C23A O28A -178.8(2) . . . . ? C15A C22A C23A O28A 0.8(3) . . . . ? C27A C22A C23A C24A 1.1(3) . . . . ? C15A C22A C23A C24A -179.3(2) . . . . ? O28A C23A C24A C25A 179.0(2) . . . . ? C22A C23A C24A C25A -0.8(4) . . . . ? C23A C24A C25A C26A -0.2(4) . . . . ? C24A C25A C26A C27A 1.0(4) . . . . ? C23A C22A C27A C26A -0.3(4) . . . . ? C15A C22A C27A C26A -179.9(2) . . . . ? C25A C26A C27A C22A -0.7(4) . . . . ? C24A C23A O28A C28A 5.4(4) . . . . ? C22A C23A O28A C28A -174.7(2) . . . . ? O14A C15A C29A C30C -50.8(4) . . . . ? C16A C15A C29A C30C 70.0(4) . . . . ? C22A C15A C29A C30C -167.9(4) . . . . ? O14A C15A C29A C30A -56.6(3) . . . . ? C16A C15A C29A C30A 64.2(3) . . . . ? C22A C15A C29A C30A -173.7(2) . . . . ? C30C C29A C30A N31A 152(4) . . . . ? C15A C29A C30A N31A -83.9(3) . . . . ? C30C C29A C30A C35A -31(4) . . . . ? C15A C29A C30A C35A 92.7(3) . . . . ? C35A C30A N31A C32A 0.0 . . . . ? C29A C30A N31A C32A 176.7(3) . . . . ? C30A N31A C32A C33A 0.0 . . . . ? N31A C32A C33A C34A 0.0 . . . . ? C32A C33A C34A C35A 0.0 . . . . ? C33A C34A C35A C30A 0.0 . . . . ? N31A C30A C35A C34A 0.0 . . . . ? C29A C30A C35A C34A -176.5(4) . . . . ? C30A C29A C30C N31C 168(4) . . . . ? C15A C29A C30C N31C 109.6(5) . . . . ? C30A C29A C30C C35C -10(4) . . . . ? C15A C29A C30C C35C -67.8(5) . . . . ? C35C C30C N31C C32C 0.0 . . . . ? C29A C30C N31C C32C -177.6(6) . . . . ? C30C N31C C32C C33C 0.0 . . . . ? N31C C32C C33C C34C 0.0 . . . . ? C32C C33C C34C C35C 0.0 . . . . ? C33C C34C C35C C30C 0.0 . . . . ? N31C C30C C35C C34C 0.0 . . . . ? C29A C30C C35C C34C 177.3(7) . . . . ? O14B Si1B C2B C3B -48.7(3) . . . . ? C9B Si1B C2B C3B -172.7(3) . . . . ? C10B Si1B C2B C3B 70.1(3) . . . . ? O14B Si1B C2B C7B 133.07(17) . . . . ? C9B Si1B C2B C7B 9.0(2) . . . . ? C10B Si1B C2B C7B -108.12(19) . . . . ? C7B C2B C3B C4B -0.5(4) . . . . ? Si1B C2B C3B C4B -178.7(2) . . . . ? C2B C3B C4B C5B 0.8(4) . . . . ? C3B C4B C5B C6B -0.4(5) . . . . ? C4B C5B C6B C7B -0.4(5) . . . . ? C5B C6B C7B C2B 0.7(5) . . . . ? C5B C6B C7B C8B -179.6(3) . . . . ? C3B C2B C7B C6B -0.2(4) . . . . ? Si1B C2B C7B C6B 178.3(2) . . . . ? C3B C2B C7B C8B -179.9(3) . . . . ? Si1B C2B C7B C8B -1.4(3) . . . . ? C6B C7B C8B C9B 171.0(3) . . . . ? C2B C7B C8B C9B -9.3(4) . . . . ? C7B C8B C9B Si1B 14.8(3) . . . . ? O14B Si1B C9B C8B -134.71(19) . . . . ? C2B Si1B C9B C8B -13.5(2) . . . . ? C10B Si1B C9B C8B 103.7(2) . . . . ? O14B Si1B C10B C13B -62.26(18) . . . . ? C2B Si1B C10B C13B 172.94(17) . . . . ? C9B Si1B C10B C13B 67.1(2) . . . . ? O14B Si1B C10B C11B 59.3(2) . . . . ? C2B Si1B C10B C11B -65.5(2) . . . . ? C9B Si1B C10B C11B -171.34(19) . . . . ? O14B Si1B C10B C12B 178.67(17) . . . . ? C2B Si1B C10B C12B 53.9(2) . . . . ? C9B Si1B C10B C12B -51.9(2) . . . . ? C2B Si1B O14B C15B -59.6(2) . . . . ? C9B Si1B O14B C15B 50.7(2) . . . . ? C10B Si1B O14B C15B 176.63(19) . . . . ? Si1B O14B C15B C16B -0.3(3) . . . . ? Si1B O14B C15B C22B 120.63(19) . . . . ? Si1B O14B C15B C29B -120.92(19) . . . . ? O14B C15B C22B C27B 3.0(3) . . . . ? C16B C15B C22B C27B 125.1(2) . . . . ? C29B C15B C22B C27B -113.0(2) . . . . ? O14B C15B C22B C23B -176.3(2) . . . . ? C16B C15B C22B C23B -54.2(3) . . . . ? C29B C15B C22B C23B 67.7(3) . . . . ? C27B C22B C23B O28B 177.9(2) . . . . ? C15B C22B C23B O28B -2.8(3) . . . . ? C27B C22B C23B C24B -2.1(4) . . . . ? C15B C22B C23B C24B 177.2(2) . . . . ? O28B C23B C24B C25B -178.6(3) . . . . ? C22B C23B C24B C25B 1.4(4) . . . . ? C23B C24B C25B C26B 0.8(4) . . . . ? C24B C25B C26B C27B -2.1(4) . . . . ? C23B C22B C27B C26B 0.8(4) . . . . ? C15B C22B C27B C26B -178.6(2) . . . . ? C25B C26B C27B C22B 1.3(4) . . . . ? C24B C23B O28B C28B -9.6(4) . . . . ? C22B C23B O28B C28B 170.4(3) . . . . ? O14B C15B C29B C30B 62.1(3) . . . . ? C16B C15B C29B C30B -59.1(3) . . . . ? C22B C15B C29B C30B 179.7(2) . . . . ? C15B C29B C30B N31B -91.3(3) . . . . ? C15B C29B C30B C35B 87.5(3) . . . . ? C35B C30B N31B C32B -1.8(4) . . . . ? C29B C30B N31B C32B 176.9(2) . . . . ? C30B N31B C32B C33B 0.3(5) . . . . ? N31B C32B C33B C34B 0.8(6) . . . . ? C32B C33B C34B C35B -0.4(6) . . . . ? N31B C30B C35B C34B 2.2(4) . . . . ? C29B C30B C35B C34B -176.5(3) . . . . ? C33B C34B C35B C30B -1.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 68.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.334 _refine_diff_density_min -0.234 _refine_diff_density_rms 0.041 # Attachment 'OST4347.CIF' data_ost4347 _database_code_depnum_ccdc_archive 'CCDC 668299' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H39 N O Si2' _chemical_formula_weight 497.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 '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 10.2158(3) _cell_length_b 10.5173(3) _cell_length_c 16.3911(5) _cell_angle_alpha 72.213(2) _cell_angle_beta 81.203(2) _cell_angle_gamma 61.845(3) _cell_volume 1478.42(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4711 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 1.249 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7058 _exptl_absorpt_correction_T_max 0.7883 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18283 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.91 _diffrn_reflns_theta_max 68.09 _reflns_number_total 5176 _reflns_number_gt 4699 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0622P)^2^+0.5404P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5176 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.02475(5) 0.02234(5) 0.24048(3) 0.03486(14) Uani 1 1 d . . . C2 C 0.19926(19) -0.12495(19) 0.29769(11) 0.0401(4) Uani 1 1 d . . . C3 C 0.2247(2) -0.2379(2) 0.37434(12) 0.0494(5) Uani 1 1 d . . . H3 H 0.1448 -0.2529 0.4043 0.059 Uiso 1 1 calc R . . C4 C 0.3668(3) -0.3278(2) 0.40632(13) 0.0575(5) Uani 1 1 d . . . H4 H 0.3832 -0.4041 0.4577 0.069 Uiso 1 1 calc R . . C5 C 0.4846(2) -0.3060(2) 0.36319(15) 0.0594(6) Uani 1 1 d . . . H5 H 0.5806 -0.3661 0.3861 0.071 Uiso 1 1 calc R . . C6 C 0.4628(2) -0.1965(2) 0.28655(15) 0.0561(5) Uani 1 1 d . . . H6 H 0.5439 -0.1833 0.2571 0.067 Uiso 1 1 calc R . . C7 C 0.3198(2) -0.1056(2) 0.25307(12) 0.0442(4) Uani 1 1 d . . . C8 C 0.2858(2) 0.0158(2) 0.16931(13) 0.0511(5) Uani 1 1 d . . . H8A H 0.3110 -0.0293 0.1213 0.061 Uiso 1 1 calc R . . H8B H 0.3464 0.0677 0.1639 0.061 Uiso 1 1 calc R . . C9 C 0.1199(2) 0.1290(2) 0.16569(12) 0.0458(4) Uani 1 1 d . . . H9A H 0.0823 0.1648 0.1073 0.055 Uiso 1 1 calc R . . H9B H 0.1042 0.2151 0.1846 0.055 Uiso 1 1 calc R . . C10 C -0.0641(2) -0.0529(2) 0.18761(12) 0.0440(4) Uani 1 1 d . . . C11 C 0.0500(3) -0.1409(3) 0.12781(17) 0.0709(7) Uani 1 1 d . . . H11A H 0.0054 -0.1818 0.1013 0.106 Uiso 1 1 calc R . . H11B H 0.1356 -0.2220 0.1607 0.106 Uiso 1 1 calc R . . H11C H 0.0811 -0.0746 0.0837 0.106 Uiso 1 1 calc R . . C12 C -0.1153(3) -0.1565(3) 0.25718(15) 0.0639(6) Uani 1 1 d . . . H12A H -0.1859 -0.1007 0.2952 0.096 Uiso 1 1 calc R . . H12B H -0.0302 -0.2391 0.2897 0.096 Uiso 1 1 calc R . . H12C H -0.1620 -0.1952 0.2305 0.096 Uiso 1 1 calc R . . C13 C -0.1988(3) 0.0752(3) 0.13612(15) 0.0621(6) Uani 1 1 d . . . H13A H -0.1677 0.1420 0.0924 0.093 Uiso 1 1 calc R . . H13B H -0.2708 0.1301 0.1741 0.093 Uiso 1 1 calc R . . H13C H -0.2434 0.0350 0.1091 0.093 Uiso 1 1 calc R . . O14 O -0.10169(13) 0.10866(12) 0.30566(7) 0.0379(3) Uani 1 1 d . . . C15 C -0.15846(18) 0.25492(18) 0.31689(10) 0.0361(4) Uani 1 1 d . . . C16 C -0.20154(18) 0.36786(19) 0.23303(11) 0.0385(4) Uani 1 1 d . . . C17 C -0.2417(2) 0.4596(2) 0.16558(11) 0.0429(4) Uani 1 1 d . . . Si18 Si -0.31359(6) 0.60105(6) 0.06378(3) 0.04529(15) Uani 1 1 d . . . C19 C -0.5137(3) 0.6518(3) 0.06073(18) 0.0802(8) Uani 1 1 d . . . H19A H -0.5245 0.5634 0.0644 0.120 Uiso 1 1 calc R . . H19B H -0.5560 0.7264 0.0075 0.120 Uiso 1 1 calc R . . H19C H -0.5652 0.6921 0.1087 0.120 Uiso 1 1 calc R . . C20 C -0.2903(3) 0.7661(3) 0.06242(16) 0.0751(7) Uani 1 1 d . . . H20A H -0.3426 0.8037 0.1111 0.113 Uiso 1 1 calc R . . H20B H -0.3305 0.8437 0.0098 0.113 Uiso 1 1 calc R . . H20C H -0.1856 0.7373 0.0657 0.113 Uiso 1 1 calc R . . C21 C -0.2082(3) 0.5203(3) -0.02580(14) 0.0701(6) Uani 1 1 d . . . H21A H -0.1034 0.4886 -0.0202 0.105 Uiso 1 1 calc R . . H21B H -0.2436 0.5952 -0.0799 0.105 Uiso 1 1 calc R . . H21C H -0.2227 0.4347 -0.0241 0.105 Uiso 1 1 calc R . . C22 C -0.04682(18) 0.26781(18) 0.36249(10) 0.0367(4) Uani 1 1 d . . . C23 C -0.0463(2) 0.4040(2) 0.35113(13) 0.0462(4) Uani 1 1 d . . . H23 H -0.1103 0.4896 0.3111 0.055 Uiso 1 1 calc R . . C24 C 0.0480(2) 0.4143(2) 0.39845(13) 0.0503(5) Uani 1 1 d . . . H24 H 0.0464 0.5076 0.3901 0.060 Uiso 1 1 calc R . . C25 C 0.1443(2) 0.2913(2) 0.45760(11) 0.0441(4) Uani 1 1 d . . . C26 C 0.1428(2) 0.1557(2) 0.46917(12) 0.0459(4) Uani 1 1 d . . . H26 H 0.2066 0.0704 0.5095 0.055 Uiso 1 1 calc R . . C27 C 0.0491(2) 0.1438(2) 0.42244(11) 0.0422(4) Uani 1 1 d . . . H27 H 0.0503 0.0506 0.4314 0.051 Uiso 1 1 calc R . . C28 C 0.2518(2) 0.3024(3) 0.50560(14) 0.0573(5) Uani 1 1 d . . . H28A H 0.2748 0.2267 0.5601 0.086 Uiso 1 1 calc R . . H28B H 0.2073 0.4008 0.5155 0.086 Uiso 1 1 calc R . . H28C H 0.3423 0.2868 0.4720 0.086 Uiso 1 1 calc R . . C29 C -0.29717(19) 0.27716(19) 0.37568(11) 0.0382(4) Uani 1 1 d . . . H29A H -0.2655 0.2035 0.4314 0.046 Uiso 1 1 calc R . . H29B H -0.3394 0.3768 0.3851 0.046 Uiso 1 1 calc R . . C30 C -0.41689(19) 0.2627(2) 0.34227(11) 0.0406(4) Uani 1 1 d . . . N31 N -0.41487(18) 0.12840(19) 0.36898(12) 0.0538(4) Uani 1 1 d . . . C32 C -0.5219(3) 0.1141(3) 0.34060(18) 0.0686(6) Uani 1 1 d . . . H32 H -0.5214 0.0200 0.3590 0.082 Uiso 1 1 calc R . . C33 C -0.6322(3) 0.2282(3) 0.28632(17) 0.0714(7) Uani 1 1 d . . . H33 H -0.7046 0.2123 0.2677 0.086 Uiso 1 1 calc R . . C34 C -0.6344(2) 0.3658(3) 0.25991(15) 0.0653(6) Uani 1 1 d . . . H34 H -0.7091 0.4466 0.2232 0.078 Uiso 1 1 calc R . . C35 C -0.5256(2) 0.3844(2) 0.28786(12) 0.0509(5) Uani 1 1 d . . . H35 H -0.5249 0.4779 0.2704 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0340(2) 0.0343(2) 0.0327(2) -0.00657(18) -0.00297(18) -0.01321(19) C2 0.0380(9) 0.0396(9) 0.0381(9) -0.0137(7) -0.0035(7) -0.0109(7) C3 0.0495(11) 0.0459(10) 0.0396(10) -0.0100(8) -0.0050(8) -0.0106(8) C4 0.0630(13) 0.0441(11) 0.0472(11) -0.0123(9) -0.0203(10) -0.0041(9) C5 0.0471(11) 0.0483(11) 0.0758(14) -0.0263(11) -0.0245(11) -0.0032(9) C6 0.0377(10) 0.0548(12) 0.0770(14) -0.0288(11) -0.0050(10) -0.0138(9) C7 0.0395(9) 0.0448(10) 0.0489(10) -0.0191(8) -0.0010(8) -0.0154(8) C8 0.0440(10) 0.0546(11) 0.0534(11) -0.0153(9) 0.0087(9) -0.0233(9) C9 0.0449(10) 0.0452(10) 0.0425(10) -0.0063(8) 0.0014(8) -0.0205(8) C10 0.0452(10) 0.0440(10) 0.0446(10) -0.0158(8) -0.0039(8) -0.0184(8) C11 0.0701(15) 0.0823(16) 0.0751(16) -0.0495(14) 0.0042(12) -0.0306(13) C12 0.0757(15) 0.0595(13) 0.0689(14) -0.0125(11) -0.0048(12) -0.0420(12) C13 0.0616(13) 0.0626(13) 0.0630(13) -0.0131(11) -0.0248(11) -0.0239(11) O14 0.0393(6) 0.0344(6) 0.0400(6) -0.0105(5) 0.0007(5) -0.0166(5) C15 0.0368(9) 0.0330(8) 0.0353(8) -0.0084(7) -0.0023(7) -0.0132(7) C16 0.0363(9) 0.0384(9) 0.0402(9) -0.0110(8) -0.0026(7) -0.0154(7) C17 0.0420(9) 0.0436(10) 0.0407(10) -0.0071(8) -0.0047(8) -0.0186(8) Si18 0.0516(3) 0.0454(3) 0.0354(3) -0.0025(2) -0.0102(2) -0.0214(2) C19 0.0562(14) 0.0858(18) 0.0812(17) -0.0075(14) -0.0248(13) -0.0201(13) C20 0.117(2) 0.0648(14) 0.0539(13) -0.0075(11) 0.0026(13) -0.0549(15) C21 0.0851(17) 0.0842(17) 0.0475(12) -0.0219(12) 0.0008(11) -0.0413(14) C22 0.0363(9) 0.0382(9) 0.0346(8) -0.0082(7) -0.0012(7) -0.0167(7) C23 0.0476(10) 0.0356(9) 0.0525(11) -0.0065(8) -0.0110(8) -0.0167(8) C24 0.0542(11) 0.0425(10) 0.0595(12) -0.0116(9) -0.0073(9) -0.0254(9) C25 0.0415(9) 0.0558(11) 0.0409(10) -0.0150(8) 0.0017(8) -0.0260(9) C26 0.0466(10) 0.0484(10) 0.0382(9) -0.0023(8) -0.0090(8) -0.0209(8) C27 0.0494(10) 0.0393(9) 0.0382(9) -0.0026(7) -0.0066(8) -0.0230(8) C28 0.0532(12) 0.0740(14) 0.0562(12) -0.0211(11) -0.0043(9) -0.0346(11) C29 0.0380(9) 0.0388(9) 0.0362(9) -0.0121(7) 0.0001(7) -0.0151(7) C30 0.0353(9) 0.0480(10) 0.0399(9) -0.0183(8) 0.0058(7) -0.0178(8) N31 0.0445(9) 0.0524(9) 0.0709(11) -0.0224(8) 0.0044(8) -0.0249(8) C32 0.0546(13) 0.0743(15) 0.0976(18) -0.0399(14) 0.0083(12) -0.0381(12) C33 0.0499(13) 0.107(2) 0.0801(16) -0.0475(15) 0.0043(12) -0.0413(14) C34 0.0452(11) 0.0933(18) 0.0555(13) -0.0217(12) -0.0066(10) -0.0270(12) C35 0.0431(10) 0.0622(12) 0.0443(10) -0.0133(9) -0.0014(8) -0.0217(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O14 1.6424(12) . ? Si1 C2 1.8641(17) . ? Si1 C9 1.8791(18) . ? Si1 C10 1.8811(18) . ? C2 C3 1.398(3) . ? C2 C7 1.401(3) . ? C3 C4 1.382(3) . ? C4 C5 1.379(3) . ? C5 C6 1.383(3) . ? C6 C7 1.399(3) . ? C7 C8 1.514(3) . ? C8 C9 1.542(3) . ? C10 C13 1.527(3) . ? C10 C12 1.535(3) . ? C10 C11 1.537(3) . ? O14 C15 1.4266(19) . ? C15 C16 1.479(2) . ? C15 C22 1.532(2) . ? C15 C29 1.549(2) . ? C16 C17 1.198(2) . ? C17 Si18 1.8340(18) . ? Si18 C20 1.853(2) . ? Si18 C21 1.858(2) . ? Si18 C19 1.858(3) . ? C22 C23 1.389(2) . ? C22 C27 1.390(2) . ? C23 C24 1.386(3) . ? C24 C25 1.381(3) . ? C25 C26 1.387(3) . ? C25 C28 1.510(3) . ? C26 C27 1.385(3) . ? C29 C30 1.500(2) . ? C30 N31 1.336(2) . ? C30 C35 1.390(3) . ? N31 C32 1.337(3) . ? C32 C33 1.372(4) . ? C33 C34 1.368(4) . ? C34 C35 1.378(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 O14 Si1 C2 111.84(7) . . ? O14 Si1 C9 116.70(7) . . ? C2 Si1 C9 93.51(8) . . ? O14 Si1 C10 106.06(7) . . ? C2 Si1 C10 113.34(8) . . ? C9 Si1 C10 115.30(9) . . ? C3 C2 C7 119.19(17) . . ? C3 C2 Si1 131.82(15) . . ? C7 C2 Si1 108.92(13) . . ? C4 C3 C2 120.3(2) . . ? C5 C4 C3 120.3(2) . . ? C4 C5 C6 120.57(18) . . ? C5 C6 C7 119.8(2) . . ? C6 C7 C2 119.85(18) . . ? C6 C7 C8 123.39(18) . . ? C2 C7 C8 116.76(16) . . ? C7 C8 C9 110.31(15) . . ? C8 C9 Si1 104.94(12) . . ? C13 C10 C12 108.87(18) . . ? C13 C10 C11 109.69(17) . . ? C12 C10 C11 109.94(18) . . ? C13 C10 Si1 110.29(13) . . ? C12 C10 Si1 108.87(13) . . ? C11 C10 Si1 109.17(14) . . ? C15 O14 Si1 132.34(10) . . ? O14 C15 C16 109.81(13) . . ? O14 C15 C22 111.48(13) . . ? C16 C15 C22 111.57(14) . . ? O14 C15 C29 105.95(13) . . ? C16 C15 C29 109.94(13) . . ? C22 C15 C29 107.91(13) . . ? C17 C16 C15 177.50(18) . . ? C16 C17 Si18 176.85(16) . . ? C17 Si18 C20 108.12(10) . . ? C17 Si18 C21 108.87(10) . . ? C20 Si18 C21 110.93(12) . . ? C17 Si18 C19 106.90(11) . . ? C20 Si18 C19 110.36(14) . . ? C21 Si18 C19 111.50(13) . . ? C23 C22 C27 118.14(16) . . ? C23 C22 C15 121.74(15) . . ? C27 C22 C15 119.90(15) . . ? C24 C23 C22 120.40(17) . . ? C25 C24 C23 121.74(17) . . ? C24 C25 C26 117.70(16) . . ? C24 C25 C28 121.22(18) . . ? C26 C25 C28 121.04(18) . . ? C27 C26 C25 121.19(17) . . ? C26 C27 C22 120.84(17) . . ? C30 C29 C15 115.25(14) . . ? N31 C30 C35 122.23(17) . . ? N31 C30 C29 116.57(16) . . ? C35 C30 C29 121.19(17) . . ? C30 N31 C32 117.32(19) . . ? N31 C32 C33 124.0(2) . . ? C34 C33 C32 118.3(2) . . ? C33 C34 C35 119.1(2) . . ? C34 C35 C30 119.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O14 Si1 C2 C3 46.79(19) . . . . ? C9 Si1 C2 C3 167.42(18) . . . . ? C10 Si1 C2 C3 -73.05(19) . . . . ? O14 Si1 C2 C7 -129.92(12) . . . . ? C9 Si1 C2 C7 -9.28(14) . . . . ? C10 Si1 C2 C7 110.24(13) . . . . ? C7 C2 C3 C4 1.0(3) . . . . ? Si1 C2 C3 C4 -175.42(15) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? C3 C4 C5 C6 -1.5(3) . . . . ? C4 C5 C6 C7 0.9(3) . . . . ? C5 C6 C7 C2 0.6(3) . . . . ? C5 C6 C7 C8 -179.34(18) . . . . ? C3 C2 C7 C6 -1.5(3) . . . . ? Si1 C2 C7 C6 175.64(14) . . . . ? C3 C2 C7 C8 178.39(16) . . . . ? Si1 C2 C7 C8 -4.4(2) . . . . ? C6 C7 C8 C9 -160.17(18) . . . . ? C2 C7 C8 C9 19.9(2) . . . . ? C7 C8 C9 Si1 -24.44(19) . . . . ? O14 Si1 C9 C8 135.87(12) . . . . ? C2 Si1 C9 C8 19.25(14) . . . . ? C10 Si1 C9 C8 -98.67(14) . . . . ? O14 Si1 C10 C13 61.56(16) . . . . ? C2 Si1 C10 C13 -175.36(14) . . . . ? C9 Si1 C10 C13 -69.23(17) . . . . ? O14 Si1 C10 C12 -57.84(15) . . . . ? C2 Si1 C10 C12 65.25(16) . . . . ? C9 Si1 C10 C12 171.38(14) . . . . ? O14 Si1 C10 C11 -177.86(14) . . . . ? C2 Si1 C10 C11 -54.78(17) . . . . ? C9 Si1 C10 C11 51.35(17) . . . . ? C2 Si1 O14 C15 107.19(14) . . . . ? C9 Si1 O14 C15 1.20(16) . . . . ? C10 Si1 O14 C15 -128.78(14) . . . . ? Si1 O14 C15 C16 50.15(19) . . . . ? Si1 O14 C15 C22 -74.03(17) . . . . ? Si1 O14 C15 C29 168.83(11) . . . . ? O14 C15 C22 C23 153.68(16) . . . . ? C16 C15 C22 C23 30.5(2) . . . . ? C29 C15 C22 C23 -90.38(19) . . . . ? O14 C15 C22 C27 -31.8(2) . . . . ? C16 C15 C22 C27 -155.00(16) . . . . ? C29 C15 C22 C27 84.13(19) . . . . ? C27 C22 C23 C24 0.2(3) . . . . ? C15 C22 C23 C24 174.79(17) . . . . ? C22 C23 C24 C25 0.3(3) . . . . ? C23 C24 C25 C26 -0.7(3) . . . . ? C23 C24 C25 C28 176.98(19) . . . . ? C24 C25 C26 C27 0.6(3) . . . . ? C28 C25 C26 C27 -177.08(18) . . . . ? C25 C26 C27 C22 -0.1(3) . . . . ? C23 C22 C27 C26 -0.3(3) . . . . ? C15 C22 C27 C26 -174.99(16) . . . . ? O14 C15 C29 C30 -58.41(18) . . . . ? C16 C15 C29 C30 60.18(19) . . . . ? C22 C15 C29 C30 -177.93(14) . . . . ? C15 C29 C30 N31 94.73(19) . . . . ? C15 C29 C30 C35 -86.6(2) . . . . ? C35 C30 N31 C32 0.6(3) . . . . ? C29 C30 N31 C32 179.23(17) . . . . ? C30 N31 C32 C33 -0.1(3) . . . . ? N31 C32 C33 C34 -0.6(4) . . . . ? C32 C33 C34 C35 0.6(4) . . . . ? C33 C34 C35 C30 -0.1(3) . . . . ? N31 C30 C35 C34 -0.5(3) . . . . ? C29 C30 C35 C34 -179.08(18) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 68.09 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.400 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.040 # Attachment 'OST4391.CIF' data_ost4391 _database_code_depnum_ccdc_archive 'CCDC 668300' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 Cl N O Si' _chemical_formula_weight 329.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.9900(3) _cell_length_b 15.6120(8) _cell_length_c 19.9389(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1864.60(16) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2887 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 2.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6424 _exptl_absorpt_correction_T_max 0.7933 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10021 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 5.26 _diffrn_reflns_theta_max 67.99 _reflns_number_total 3219 _reflns_number_gt 2928 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0393P)^2^+0.6263P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 3219 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Cl1 Cl 0.23502(15) 0.48059(4) 0.98568(3) 0.0735(2) Uani 1 1 d . . . Si1 Si 0.37964(14) 0.18528(7) 1.37428(4) 0.0758(3) Uani 1 1 d . . . O1 O -0.1344(3) 0.15947(12) 1.17092(10) 0.0581(5) Uani 1 1 d . . . H1 H -0.1569 0.1105 1.1857 0.087 Uiso 1 1 calc R . . N1 N 0.0169(4) -0.00234(15) 1.20667(14) 0.0707(7) Uani 1 1 d . . . C1 C 0.0998(4) 0.17380(16) 1.16501(11) 0.0459(5) Uani 1 1 d . . . C2 C 0.1955(4) 0.18774(16) 1.23290(11) 0.0486(5) Uani 1 1 d . . . C3 C 0.2706(4) 0.19212(17) 1.28825(12) 0.0564(6) Uani 1 1 d . . . C4 C 0.6850(6) 0.1744(5) 1.3687(2) 0.158(3) Uani 1 1 d . . . H4A H 0.7218 0.1257 1.3406 0.237 Uiso 1 1 calc R . . H4B H 0.7462 0.1657 1.4132 0.237 Uiso 1 1 calc R . . H4C H 0.7479 0.2261 1.3494 0.237 Uiso 1 1 calc R . . C5 C 0.2600(7) 0.0875(3) 1.4129(2) 0.1140(14) Uani 1 1 d . . . H5A H 0.1001 0.0945 1.4181 0.171 Uiso 1 1 calc R . . H5B H 0.3278 0.0782 1.4565 0.171 Uiso 1 1 calc R . . H5C H 0.2897 0.0386 1.3842 0.171 Uiso 1 1 calc R . . C6 C 0.2904(8) 0.2817(3) 1.42083(17) 0.1224(16) Uani 1 1 d . . . H6A H 0.3653 0.3317 1.4026 0.184 Uiso 1 1 calc R . . H6B H 0.3288 0.2754 1.4678 0.184 Uiso 1 1 calc R . . H6C H 0.1301 0.2888 1.4165 0.184 Uiso 1 1 calc R . . C7 C 0.2161(5) 0.09531(14) 1.13361(12) 0.0500(6) Uani 1 1 d . . . H7A H 0.1434 0.0821 1.0908 0.060 Uiso 1 1 calc R . . H7B H 0.3718 0.1102 1.1240 0.060 Uiso 1 1 calc R . . C8 C 0.2122(4) 0.01648(16) 1.17690(12) 0.0510(6) Uani 1 1 d . . . C9 C 0.3997(5) -0.03298(18) 1.18591(15) 0.0645(7) Uani 1 1 d . . . H9 H 0.5353 -0.0176 1.1655 0.077 Uiso 1 1 calc R . . C10 C 0.3861(6) -0.1053(2) 1.22529(17) 0.0773(9) Uani 1 1 d . . . H10 H 0.5115 -0.1409 1.2308 0.093 Uiso 1 1 calc R . . C11 C 0.1899(6) -0.1251(2) 1.25621(18) 0.0803(10) Uani 1 1 d . . . H11 H 0.1766 -0.1740 1.2833 0.096 Uiso 1 1 calc R . . C12 C 0.0133(6) -0.0713(2) 1.2465(2) 0.0855(10) Uani 1 1 d . . . H12 H -0.1202 -0.0836 1.2693 0.103 Uiso 1 1 calc R . . C13 C 0.1339(4) 0.25131(15) 1.12023(11) 0.0446(5) Uani 1 1 d . . . C14 C -0.0325(4) 0.27699(17) 1.07606(12) 0.0558(6) Uani 1 1 d . . . H14 H -0.1678 0.2466 1.0743 0.067 Uiso 1 1 calc R . . C15 C -0.0006(5) 0.34690(18) 1.03464(13) 0.0595(7) Uani 1 1 d . . . H15 H -0.1137 0.3637 1.0047 0.071 Uiso 1 1 calc R . . C16 C 0.1968(5) 0.39181(16) 1.03726(12) 0.0546(6) Uani 1 1 d . . . C17 C 0.3646(5) 0.36627(17) 1.07995(14) 0.0575(6) Uani 1 1 d . . . H17 H 0.5000 0.3966 1.0813 0.069 Uiso 1 1 calc R . . C18 C 0.3335(4) 0.29581(16) 1.12092(13) 0.0534(6) Uani 1 1 d . . . H18 H 0.4493 0.2780 1.1495 0.064 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 Cl1 0.0963(5) 0.0626(4) 0.0617(4) 0.0127(3) 0.0056(4) 0.0093(4) Si1 0.0604(4) 0.1214(8) 0.0455(4) 0.0085(5) -0.0057(4) -0.0056(5) O1 0.0397(9) 0.0702(12) 0.0644(11) 0.0042(9) -0.0010(8) -0.0041(8) N1 0.0543(13) 0.0681(16) 0.0897(17) 0.0230(13) 0.0071(13) -0.0077(12) C1 0.0392(12) 0.0547(14) 0.0437(11) -0.0023(11) -0.0013(10) -0.0017(11) C2 0.0477(13) 0.0526(13) 0.0455(12) -0.0020(11) 0.0006(10) 0.0009(11) C3 0.0556(14) 0.0619(15) 0.0519(13) -0.0022(12) 0.0011(12) 0.0020(14) C4 0.068(2) 0.320(8) 0.086(3) 0.057(4) -0.016(2) -0.007(4) C5 0.108(3) 0.134(3) 0.100(3) 0.053(3) 0.004(3) 0.020(3) C6 0.152(4) 0.154(4) 0.0602(19) -0.028(2) 0.011(2) -0.038(3) C7 0.0551(14) 0.0487(13) 0.0462(12) -0.0011(10) 0.0011(12) -0.0014(11) C8 0.0533(14) 0.0497(12) 0.0499(12) 0.0009(11) -0.0002(12) -0.0028(12) C9 0.0599(16) 0.0587(16) 0.0747(18) 0.0121(14) 0.0100(15) -0.0009(14) C10 0.076(2) 0.0640(18) 0.092(2) 0.0216(17) -0.0007(19) 0.0037(16) C11 0.077(2) 0.072(2) 0.093(2) 0.0297(18) -0.0069(18) -0.0146(17) C12 0.0635(18) 0.088(2) 0.105(3) 0.033(2) 0.0067(18) -0.0186(19) C13 0.0464(12) 0.0459(12) 0.0414(11) -0.0038(10) -0.0026(11) 0.0033(10) C14 0.0511(14) 0.0648(15) 0.0514(13) -0.0007(13) -0.0071(12) -0.0008(13) C15 0.0579(16) 0.0731(17) 0.0476(14) 0.0052(13) -0.0103(12) 0.0085(14) C16 0.0681(17) 0.0506(13) 0.0451(12) -0.0023(11) 0.0013(12) 0.0115(13) C17 0.0571(15) 0.0518(14) 0.0636(15) 0.0020(13) -0.0021(14) -0.0025(12) C18 0.0520(15) 0.0538(14) 0.0543(13) 0.0046(12) -0.0092(11) -0.0006(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C16 1.741(3) . ? Si1 C3 1.838(3) . ? Si1 C4 1.840(4) . ? Si1 C6 1.848(4) . ? Si1 C5 1.854(4) . ? O1 C1 1.426(3) . ? N1 C12 1.338(4) . ? N1 C8 1.345(3) . ? C1 C2 1.486(3) . ? C1 C13 1.518(3) . ? C1 C7 1.542(3) . ? C2 C3 1.194(3) . ? C7 C8 1.503(3) . ? C8 C9 1.374(4) . ? C9 C10 1.378(4) . ? C10 C11 1.363(5) . ? C11 C12 1.364(5) . ? C13 C18 1.383(3) . ? C13 C14 1.389(3) . ? C14 C15 1.382(4) . ? C15 C16 1.376(4) . ? C16 C17 1.376(4) . ? C17 C18 1.383(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 C3 Si1 C4 107.57(16) . . ? C3 Si1 C6 108.57(17) . . ? C4 Si1 C6 113.2(3) . . ? C3 Si1 C5 107.33(18) . . ? C4 Si1 C5 109.5(3) . . ? C6 Si1 C5 110.5(2) . . ? C12 N1 C8 116.9(3) . . ? O1 C1 C2 109.10(19) . . ? O1 C1 C13 107.81(19) . . ? C2 C1 C13 111.6(2) . . ? O1 C1 C7 110.7(2) . . ? C2 C1 C7 108.19(19) . . ? C13 C1 C7 109.51(18) . . ? C3 C2 C1 174.8(3) . . ? C2 C3 Si1 173.3(3) . . ? C8 C7 C1 114.2(2) . . ? N1 C8 C9 122.0(2) . . ? N1 C8 C7 116.5(2) . . ? C9 C8 C7 121.5(2) . . ? C8 C9 C10 119.1(3) . . ? C11 C10 C9 119.6(3) . . ? C10 C11 C12 117.8(3) . . ? N1 C12 C11 124.5(3) . . ? C18 C13 C14 118.8(2) . . ? C18 C13 C1 120.7(2) . . ? C14 C13 C1 120.5(2) . . ? C15 C14 C13 120.5(2) . . ? C16 C15 C14 119.9(2) . . ? C17 C16 C15 120.2(2) . . ? C17 C16 Cl1 120.0(2) . . ? C15 C16 Cl1 119.7(2) . . ? C16 C17 C18 119.9(3) . . ? C17 C18 C13 120.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C7 C8 -66.8(3) . . . . ? C2 C1 C7 C8 52.7(3) . . . . ? C13 C1 C7 C8 174.5(2) . . . . ? C12 N1 C8 C9 0.8(4) . . . . ? C12 N1 C8 C7 -178.6(3) . . . . ? C1 C7 C8 N1 44.6(3) . . . . ? C1 C7 C8 C9 -134.8(3) . . . . ? N1 C8 C9 C10 1.7(4) . . . . ? C7 C8 C9 C10 -179.0(3) . . . . ? C8 C9 C10 C11 -2.1(5) . . . . ? C9 C10 C11 C12 0.0(6) . . . . ? C8 N1 C12 C11 -3.0(6) . . . . ? C10 C11 C12 N1 2.6(6) . . . . ? O1 C1 C13 C18 160.7(2) . . . . ? C2 C1 C13 C18 41.0(3) . . . . ? C7 C1 C13 C18 -78.8(3) . . . . ? O1 C1 C13 C14 -21.5(3) . . . . ? C2 C1 C13 C14 -141.3(2) . . . . ? C7 C1 C13 C14 99.0(3) . . . . ? C18 C13 C14 C15 -1.4(4) . . . . ? C1 C13 C14 C15 -179.2(2) . . . . ? C13 C14 C15 C16 -0.3(4) . . . . ? C14 C15 C16 C17 1.4(4) . . . . ? C14 C15 C16 Cl1 -179.3(2) . . . . ? C15 C16 C17 C18 -0.8(4) . . . . ? Cl1 C16 C17 C18 179.9(2) . . . . ? C16 C17 C18 C13 -1.0(4) . . . . ? C14 C13 C18 C17 2.1(4) . . . . ? C1 C13 C18 C17 179.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 67.99 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.123 _refine_diff_density_min -0.144 _refine_diff_density_rms 0.033