# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Iwamoto, Takeaki' 'Ohnishi, Nobuyoshi' 'Gui, Zhenyu' 'Ishida, Shintaro' 'Isobe, Hiroyuki' 'Maeda, Satoshi' 'Ohno, Koichi' 'Kira, Mitsuo' _publ_contact_author_name 'Iwamoto, Takeaki' _publ_contact_author_email iwamoto@m.tains.tohoku.ac.jp _publ_section_title ; Synthesis and Structure of Stable Base-Free Dialkylsilanimines ; _publ_contact_author_address ; Department of Chemistry, Graduate School of Science, Tohoku University, Aoba-ku, Sendai 980-8578, Japan ; _publ_contact_author_fax +81-22-795-7714 _publ_contact_author_phone +81-22-795-7714 # Attachment '- CIF_silaimines.cif' data_N-benzylsilanimines _database_code_depnum_ccdc_archive 'CCDC 766385' #TrackingRef '- CIF_silaimines.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H47 N Si5' _chemical_formula_weight 478.07 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' Si Si 0.0817 0.0704 '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 10.844(2) _cell_length_b 11.874(3) _cell_length_c 13.349(3) _cell_angle_alpha 115.304(2) _cell_angle_beta 95.635(2) _cell_angle_gamma 107.048(2) _cell_volume 1435.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 0.260 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9499 _exptl_absorpt_correction_T_max 0.9871 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13815 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5027 _reflns_number_gt 4087 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0462P)^2^+0.6223P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5027 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 C1 C 1.3121(2) 0.9488(2) 0.91252(19) 0.0315(6) Uani 1 1 d . . . H1 H 1.3063 1.0013 0.9878 0.035(7) Uiso 1 1 calc R . . C2 C 1.2731(2) 0.9740(2) 0.82493(19) 0.0270(5) Uani 1 1 d . . . H2 H 1.2409 1.0444 0.8403 0.027(6) Uiso 1 1 calc R . . C3 C 1.2808(2) 0.8969(2) 0.71466(18) 0.0218(5) Uani 1 1 d . . . H3 H 1.2531 0.9145 0.6549 0.028(6) Uiso 1 1 calc R . . C4 C 1.3595(2) 0.8466(2) 0.88969(19) 0.0311(6) Uani 1 1 d . . . H4 H 1.3868 0.8291 0.9496 0.040(7) Uiso 1 1 calc R . . C5 C 1.3673(2) 0.7696(2) 0.77978(18) 0.0243(5) Uani 1 1 d . . . H5 H 1.3994 0.6991 0.7647 0.034(7) Uiso 1 1 calc R . . C6 C 1.3285(2) 0.7946(2) 0.69098(17) 0.0199(5) Uani 1 1 d . . . C7 C 1.3395(3) 0.7080(2) 0.57200(18) 0.0301(6) Uani 1 1 d . . . H6 H 1.4351 0.7261 0.5741 0.050(8) Uiso 1 1 calc R . . H7 H 1.2961 0.6124 0.5514 0.046(8) Uiso 1 1 calc R . . N1 N 1.27977(18) 0.73000(18) 0.48369(15) 0.0248(4) Uani 1 1 d . . . Si1 Si 1.22820(6) 0.65461(5) 0.34836(5) 0.01667(14) Uani 1 1 d . . . C8 C 1.1434(2) 0.71803(19) 0.26788(16) 0.0167(4) Uani 1 1 d . . . C9 C 1.2286(2) 0.49625(19) 0.22992(17) 0.0171(4) Uani 1 1 d . . . C10 C 1.1453(2) 0.6249(2) 0.14226(17) 0.0183(4) Uani 1 1 d . . . H48 H 1.0698 0.6151 0.0870 0.022 Uiso 1 1 calc R . . H49 H 1.2293 0.6667 0.1267 0.022 Uiso 1 1 calc R . . C11 C 1.1343(2) 0.4842(2) 0.12558(17) 0.0179(4) Uani 1 1 d . . . H50 H 1.1587 0.4357 0.0542 0.021 Uiso 1 1 calc R . . H51 H 1.0408 0.4316 0.1176 0.021 Uiso 1 1 calc R . . Si2 Si 0.96610(6) 0.70023(6) 0.28178(5) 0.02107(15) Uani 1 1 d . . . Si3 Si 1.25319(6) 0.90037(6) 0.31708(5) 0.02400(16) Uani 1 1 d . . . Si4 Si 1.39926(6) 0.50289(6) 0.20371(5) 0.02002(15) Uani 1 1 d . . . Si5 Si 1.14725(6) 0.35061(6) 0.25891(5) 0.02093(15) Uani 1 1 d . . . C12 C 0.9526(2) 0.7357(2) 0.42979(19) 0.0295(5) Uani 1 1 d . . . H12 H 1.0189 0.8244 0.4854 0.058(9) Uiso 1 1 calc R . . H13 H 0.9688 0.6672 0.4456 0.054(8) Uiso 1 1 calc R . . H14 H 0.8628 0.7342 0.4360 0.045(8) Uiso 1 1 calc R . . C13 C 0.8408(2) 0.5276(2) 0.17819(19) 0.0252(5) Uani 1 1 d . . . H15 H 0.8548 0.4626 0.2003 0.043(7) Uiso 1 1 calc R . . H16 H 0.8520 0.5035 0.1006 0.029(6) Uiso 1 1 calc R . . H17 H 0.7504 0.5267 0.1797 0.034(7) Uiso 1 1 calc R . . C14 C 0.9048(2) 0.8121(2) 0.2420(2) 0.0345(6) Uani 1 1 d . . . H18 H 0.8121 0.7963 0.2466 0.060(9) Uiso 1 1 calc R . . H19 H 0.9096 0.7921 0.1636 0.045(8) Uiso 1 1 calc R . . H20 H 0.9608 0.9062 0.2951 0.050(8) Uiso 1 1 calc R . . C15 C 1.2325(2) 1.0180(2) 0.4556(2) 0.0301(5) Uani 1 1 d . . . H21 H 1.2593 0.9965 0.5155 0.042(7) Uiso 1 1 calc R . . H22 H 1.1388 1.0090 0.4470 0.047(8) Uiso 1 1 calc R . . H23 H 1.2886 1.1104 0.4772 0.062(9) Uiso 1 1 calc R . . C16 C 1.2171(3) 0.9457(3) 0.2021(2) 0.0418(7) Uani 1 1 d . . . H24 H 1.1305 0.9559 0.1986 0.051(9) Uiso 1 1 calc R . . H25 H 1.2146 0.8745 0.1280 0.075(10) Uiso 1 1 calc R . . H26 H 1.2872 1.0304 0.2195 0.062(9) Uiso 1 1 calc R . . C17 C 1.4346(2) 0.9253(2) 0.3407(2) 0.0356(6) Uani 1 1 d . . . H27 H 1.4888 1.0209 0.3898 0.052(8) Uiso 1 1 calc R . . H28 H 1.4572 0.8938 0.2668 0.065(9) Uiso 1 1 calc R . . H29 H 1.4527 0.8743 0.3780 0.075(11) Uiso 1 1 calc R . . C18 C 1.5272(2) 0.5742(2) 0.34181(19) 0.0291(5) Uani 1 1 d . . . H30 H 1.6152 0.5818 0.3268 0.061(9) Uiso 1 1 calc R . . H31 H 1.5037 0.5148 0.3759 0.074(10) Uiso 1 1 calc R . . H32 H 1.5297 0.6632 0.3950 0.043(7) Uiso 1 1 calc R . . C19 C 1.4608(2) 0.6088(2) 0.1345(2) 0.0295(5) Uani 1 1 d . . . H33 H 1.4754 0.7024 0.1870 0.055(8) Uiso 1 1 calc R . . H34 H 1.3942 0.5768 0.0635 0.041(7) Uiso 1 1 calc R . . H35 H 1.5449 0.6028 0.1167 0.037(7) Uiso 1 1 calc R . . C20 C 1.3896(2) 0.3314(2) 0.09894(19) 0.0266(5) Uani 1 1 d . . . H36 H 1.4768 0.3370 0.0827 0.051(8) Uiso 1 1 calc R . . H37 H 1.3224 0.2967 0.0276 0.044(7) Uiso 1 1 calc R . . H38 H 1.3646 0.2709 0.1318 0.038(7) Uiso 1 1 calc R . . C21 C 1.2680(2) 0.3236(2) 0.34871(19) 0.0277(5) Uani 1 1 d . . . H39 H 1.2189 0.2543 0.3670 0.043(7) Uiso 1 1 calc R . . H40 H 1.3168 0.4076 0.4199 0.042(7) Uiso 1 1 calc R . . H41 H 1.3313 0.2947 0.3061 0.041(7) Uiso 1 1 calc R . . C22 C 1.0204(2) 0.3852(2) 0.3405(2) 0.0301(6) Uani 1 1 d . . . H42 H 0.9537 0.3995 0.2972 0.080(11) Uiso 1 1 calc R . . H43 H 1.0646 0.4657 0.4152 0.039(7) Uiso 1 1 calc R . . H44 H 0.9763 0.3084 0.3520 0.042(7) Uiso 1 1 calc R . . C23 C 1.0617(2) 0.1915(2) 0.1200(2) 0.0328(6) Uani 1 1 d . . . H45 H 1.0183 0.1179 0.1355 0.046(8) Uiso 1 1 calc R . . H46 H 1.1276 0.1707 0.0772 0.072(10) Uiso 1 1 calc R . . H47 H 0.9943 0.2028 0.0744 0.064(9) 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 C1 0.0412(15) 0.0305(13) 0.0178(12) 0.0059(10) 0.0080(11) 0.0153(11) C2 0.0317(13) 0.0227(12) 0.0273(13) 0.0100(10) 0.0098(10) 0.0133(10) C3 0.0229(12) 0.0230(11) 0.0199(11) 0.0113(10) 0.0043(9) 0.0080(9) C4 0.0398(15) 0.0354(14) 0.0182(12) 0.0136(11) 0.0028(10) 0.0144(11) C5 0.0282(12) 0.0261(12) 0.0191(11) 0.0102(10) 0.0036(9) 0.0128(10) C6 0.0171(11) 0.0197(11) 0.0188(11) 0.0073(9) 0.0024(9) 0.0050(9) C7 0.0419(15) 0.0358(14) 0.0175(12) 0.0101(10) 0.0065(10) 0.0255(12) N1 0.0306(11) 0.0271(10) 0.0179(10) 0.0091(8) 0.0039(8) 0.0158(9) Si1 0.0175(3) 0.0173(3) 0.0151(3) 0.0066(2) 0.0036(2) 0.0083(2) C8 0.0196(11) 0.0163(10) 0.0141(10) 0.0063(9) 0.0032(8) 0.0083(9) C9 0.0156(10) 0.0164(10) 0.0172(11) 0.0062(9) 0.0030(8) 0.0066(8) C10 0.0191(11) 0.0197(11) 0.0152(11) 0.0072(9) 0.0031(9) 0.0083(9) C11 0.0182(11) 0.0188(11) 0.0148(10) 0.0060(9) 0.0034(8) 0.0077(9) Si2 0.0204(3) 0.0253(3) 0.0199(3) 0.0099(3) 0.0050(2) 0.0132(3) Si3 0.0314(4) 0.0164(3) 0.0220(3) 0.0081(3) 0.0069(3) 0.0078(3) Si4 0.0180(3) 0.0212(3) 0.0180(3) 0.0055(3) 0.0039(2) 0.0096(3) Si5 0.0225(3) 0.0180(3) 0.0215(3) 0.0096(3) 0.0025(3) 0.0075(3) C12 0.0271(13) 0.0393(14) 0.0241(12) 0.0119(11) 0.0111(10) 0.0186(11) C13 0.0186(12) 0.0338(13) 0.0241(12) 0.0135(11) 0.0056(9) 0.0112(10) C14 0.0327(14) 0.0350(14) 0.0372(15) 0.0150(12) 0.0024(11) 0.0200(12) C15 0.0356(14) 0.0203(12) 0.0295(13) 0.0077(10) 0.0046(11) 0.0115(11) C16 0.065(2) 0.0275(14) 0.0332(15) 0.0184(12) 0.0106(13) 0.0129(13) C17 0.0303(14) 0.0222(12) 0.0383(15) 0.0063(12) 0.0123(12) 0.0003(11) C18 0.0200(12) 0.0329(13) 0.0250(13) 0.0063(11) 0.0024(10) 0.0105(10) C19 0.0276(13) 0.0326(13) 0.0321(14) 0.0144(11) 0.0168(11) 0.0151(11) C20 0.0295(13) 0.0267(12) 0.0223(12) 0.0070(10) 0.0045(10) 0.0169(10) C21 0.0352(13) 0.0258(12) 0.0263(13) 0.0141(11) 0.0053(11) 0.0152(11) C22 0.0264(13) 0.0330(14) 0.0397(15) 0.0252(12) 0.0104(11) 0.0100(11) C23 0.0341(14) 0.0205(12) 0.0307(14) 0.0083(11) -0.0024(11) 0.0024(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 C1 C4 1.381(3) . ? C1 C2 1.383(3) . ? C1 H1 0.9500 . ? C2 C3 1.389(3) . ? C2 H2 0.9500 . ? C3 C6 1.383(3) . ? C3 H3 0.9500 . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 C7 1.519(3) . ? C7 N1 1.446(3) . ? C7 H6 0.9900 . ? C7 H7 0.9900 . ? N1 Si1 1.5823(18) . ? Si1 C8 1.863(2) . ? Si1 C9 1.871(2) . ? C8 C10 1.572(3) . ? C8 Si2 1.908(2) . ? C8 Si3 1.912(2) . ? C9 C11 1.572(3) . ? C9 Si4 1.902(2) . ? C9 Si5 1.914(2) . ? C10 C11 1.554(3) . ? C10 H48 0.9900 . ? C10 H49 0.9900 . ? C11 H50 0.9900 . ? C11 H51 0.9900 . ? Si2 C12 1.867(2) . ? Si2 C13 1.880(2) . ? Si2 C14 1.881(2) . ? Si3 C15 1.865(2) . ? Si3 C16 1.874(3) . ? Si3 C17 1.874(2) . ? Si4 C19 1.872(2) . ? Si4 C18 1.875(2) . ? Si4 C20 1.878(2) . ? Si5 C22 1.869(2) . ? Si5 C23 1.873(2) . ? Si5 C21 1.877(2) . ? C12 H12 0.9800 . ? C12 H13 0.9800 . ? C12 H14 0.9800 . ? C13 H15 0.9800 . ? C13 H16 0.9800 . ? C13 H17 0.9800 . ? C14 H18 0.9800 . ? C14 H19 0.9800 . ? C14 H20 0.9800 . ? C15 H21 0.9800 . ? C15 H22 0.9800 . ? C15 H23 0.9800 . ? C16 H24 0.9800 . ? C16 H25 0.9800 . ? C16 H26 0.9800 . ? C17 H27 0.9800 . ? C17 H28 0.9800 . ? C17 H29 0.9800 . ? C18 H30 0.9800 . ? C18 H31 0.9800 . ? C18 H32 0.9800 . ? C19 H33 0.9800 . ? C19 H34 0.9800 . ? C19 H35 0.9800 . ? C20 H36 0.9800 . ? C20 H37 0.9800 . ? C20 H38 0.9800 . ? C21 H39 0.9800 . ? C21 H40 0.9800 . ? C21 H41 0.9800 . ? C22 H42 0.9800 . ? C22 H43 0.9800 . ? C22 H44 0.9800 . ? C23 H45 0.9800 . ? C23 H46 0.9800 . ? C23 H47 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 C1 C2 119.5(2) . . ? C4 C1 H1 120.3 . . ? C2 C1 H1 120.3 . . ? C1 C2 C3 120.3(2) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C6 C3 C2 120.6(2) . . ? C6 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C1 C4 C5 120.3(2) . . ? C1 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C3 C6 C5 118.68(19) . . ? C3 C6 C7 122.60(19) . . ? C5 C6 C7 118.72(19) . . ? N1 C7 C6 114.01(18) . . ? N1 C7 H6 108.8 . . ? C6 C7 H6 108.8 . . ? N1 C7 H7 108.8 . . ? C6 C7 H7 108.8 . . ? H6 C7 H7 107.6 . . ? C7 N1 Si1 138.07(15) . . ? N1 Si1 C8 123.13(9) . . ? N1 Si1 C9 134.84(9) . . ? C8 Si1 C9 102.02(9) . . ? C10 C8 Si1 100.40(12) . . ? C10 C8 Si2 111.94(13) . . ? Si1 C8 Si2 113.80(10) . . ? C10 C8 Si3 110.27(13) . . ? Si1 C8 Si3 108.29(10) . . ? Si2 C8 Si3 111.57(10) . . ? C11 C9 Si1 100.37(13) . . ? C11 C9 Si4 111.01(13) . . ? Si1 C9 Si4 114.79(10) . . ? C11 C9 Si5 110.06(13) . . ? Si1 C9 Si5 108.85(10) . . ? Si4 C9 Si5 111.22(10) . . ? C11 C10 C8 110.82(16) . . ? C11 C10 H48 109.5 . . ? C8 C10 H48 109.5 . . ? C11 C10 H49 109.5 . . ? C8 C10 H49 109.5 . . ? H48 C10 H49 108.1 . . ? C10 C11 C9 111.14(16) . . ? C10 C11 H50 109.4 . . ? C9 C11 H50 109.4 . . ? C10 C11 H51 109.4 . . ? C9 C11 H51 109.4 . . ? H50 C11 H51 108.0 . . ? C12 Si2 C13 108.15(11) . . ? C12 Si2 C14 109.24(11) . . ? C13 Si2 C14 103.03(11) . . ? C12 Si2 C8 111.56(10) . . ? C13 Si2 C8 112.11(9) . . ? C14 Si2 C8 112.34(10) . . ? C15 Si3 C16 111.39(12) . . ? C15 Si3 C17 106.67(11) . . ? C16 Si3 C17 105.56(13) . . ? C15 Si3 C8 111.75(10) . . ? C16 Si3 C8 110.00(11) . . ? C17 Si3 C8 111.26(10) . . ? C19 Si4 C18 107.28(11) . . ? C19 Si4 C20 104.38(11) . . ? C18 Si4 C20 111.20(10) . . ? C19 Si4 C9 112.60(10) . . ? C18 Si4 C9 110.95(10) . . ? C20 Si4 C9 110.24(10) . . ? C22 Si5 C23 108.59(12) . . ? C22 Si5 C21 105.76(11) . . ? C23 Si5 C21 108.82(11) . . ? C22 Si5 C9 109.92(10) . . ? C23 Si5 C9 109.96(10) . . ? C21 Si5 C9 113.62(10) . . ? Si2 C12 H12 109.5 . . ? Si2 C12 H13 109.5 . . ? H12 C12 H13 109.5 . . ? Si2 C12 H14 109.5 . . ? H12 C12 H14 109.5 . . ? H13 C12 H14 109.5 . . ? Si2 C13 H15 109.5 . . ? Si2 C13 H16 109.5 . . ? H15 C13 H16 109.5 . . ? Si2 C13 H17 109.5 . . ? H15 C13 H17 109.5 . . ? H16 C13 H17 109.5 . . ? Si2 C14 H18 109.5 . . ? Si2 C14 H19 109.5 . . ? H18 C14 H19 109.5 . . ? Si2 C14 H20 109.5 . . ? H18 C14 H20 109.5 . . ? H19 C14 H20 109.5 . . ? Si3 C15 H21 109.5 . . ? Si3 C15 H22 109.5 . . ? H21 C15 H22 109.5 . . ? Si3 C15 H23 109.5 . . ? H21 C15 H23 109.5 . . ? H22 C15 H23 109.5 . . ? Si3 C16 H24 109.5 . . ? Si3 C16 H25 109.5 . . ? H24 C16 H25 109.5 . . ? Si3 C16 H26 109.5 . . ? H24 C16 H26 109.5 . . ? H25 C16 H26 109.5 . . ? Si3 C17 H27 109.5 . . ? Si3 C17 H28 109.5 . . ? H27 C17 H28 109.5 . . ? Si3 C17 H29 109.5 . . ? H27 C17 H29 109.5 . . ? H28 C17 H29 109.5 . . ? Si4 C18 H30 109.5 . . ? Si4 C18 H31 109.5 . . ? H30 C18 H31 109.5 . . ? Si4 C18 H32 109.5 . . ? H30 C18 H32 109.5 . . ? H31 C18 H32 109.5 . . ? Si4 C19 H33 109.5 . . ? Si4 C19 H34 109.5 . . ? H33 C19 H34 109.5 . . ? Si4 C19 H35 109.5 . . ? H33 C19 H35 109.5 . . ? H34 C19 H35 109.5 . . ? Si4 C20 H36 109.5 . . ? Si4 C20 H37 109.5 . . ? H36 C20 H37 109.5 . . ? Si4 C20 H38 109.5 . . ? H36 C20 H38 109.5 . . ? H37 C20 H38 109.5 . . ? Si5 C21 H39 109.5 . . ? Si5 C21 H40 109.5 . . ? H39 C21 H40 109.5 . . ? Si5 C21 H41 109.5 . . ? H39 C21 H41 109.5 . . ? H40 C21 H41 109.5 . . ? Si5 C22 H42 109.5 . . ? Si5 C22 H43 109.5 . . ? H42 C22 H43 109.5 . . ? Si5 C22 H44 109.5 . . ? H42 C22 H44 109.5 . . ? H43 C22 H44 109.5 . . ? Si5 C23 H45 109.5 . . ? Si5 C23 H46 109.5 . . ? H45 C23 H46 109.5 . . ? Si5 C23 H47 109.5 . . ? H45 C23 H47 109.5 . . ? H46 C23 H47 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 C4 C1 C2 C3 0.3(4) . . . . ? C1 C2 C3 C6 -0.5(3) . . . . ? C2 C1 C4 C5 -0.3(4) . . . . ? C1 C4 C5 C6 0.5(4) . . . . ? C2 C3 C6 C5 0.7(3) . . . . ? C2 C3 C6 C7 -179.7(2) . . . . ? C4 C5 C6 C3 -0.6(3) . . . . ? C4 C5 C6 C7 179.7(2) . . . . ? C3 C6 C7 N1 -7.8(3) . . . . ? C5 C6 C7 N1 171.9(2) . . . . ? C6 C7 N1 Si1 -161.39(19) . . . . ? C7 N1 Si1 C8 175.2(2) . . . . ? C7 N1 Si1 C9 -4.6(3) . . . . ? N1 Si1 C8 C10 167.85(13) . . . . ? C9 Si1 C8 C10 -12.34(14) . . . . ? N1 Si1 C8 Si2 -72.40(14) . . . . ? C9 Si1 C8 Si2 107.41(11) . . . . ? N1 Si1 C8 Si3 52.28(15) . . . . ? C9 Si1 C8 Si3 -127.91(10) . . . . ? N1 Si1 C9 C11 169.85(13) . . . . ? C8 Si1 C9 C11 -9.93(14) . . . . ? N1 Si1 C9 Si4 -71.07(17) . . . . ? C8 Si1 C9 Si4 109.15(11) . . . . ? N1 Si1 C9 Si5 54.31(17) . . . . ? C8 Si1 C9 Si5 -125.47(10) . . . . ? Si1 C8 C10 C11 32.41(18) . . . . ? Si2 C8 C10 C11 -88.68(17) . . . . ? Si3 C8 C10 C11 146.48(14) . . . . ? C8 C10 C11 C9 -44.7(2) . . . . ? Si1 C9 C11 C10 30.79(18) . . . . ? Si4 C9 C11 C10 -91.02(17) . . . . ? Si5 C9 C11 C10 145.41(14) . . . . ? C10 C8 Si2 C12 151.37(14) . . . . ? Si1 C8 Si2 C12 38.39(14) . . . . ? Si3 C8 Si2 C12 -84.51(13) . . . . ? C10 C8 Si2 C13 29.91(16) . . . . ? Si1 C8 Si2 C13 -83.08(13) . . . . ? Si3 C8 Si2 C13 154.02(10) . . . . ? C10 C8 Si2 C14 -85.57(16) . . . . ? Si1 C8 Si2 C14 161.45(11) . . . . ? Si3 C8 Si2 C14 38.54(14) . . . . ? C10 C8 Si3 C15 170.75(14) . . . . ? Si1 C8 Si3 C15 -80.30(13) . . . . ? Si2 C8 Si3 C15 45.70(14) . . . . ? C10 C8 Si3 C16 46.48(17) . . . . ? Si1 C8 Si3 C16 155.43(12) . . . . ? Si2 C8 Si3 C16 -78.57(14) . . . . ? C10 C8 Si3 C17 -70.13(16) . . . . ? Si1 C8 Si3 C17 38.82(14) . . . . ? Si2 C8 Si3 C17 164.82(11) . . . . ? C11 C9 Si4 C19 40.57(17) . . . . ? Si1 C9 Si4 C19 -72.38(14) . . . . ? Si5 C9 Si4 C19 163.48(10) . . . . ? C11 C9 Si4 C18 160.82(14) . . . . ? Si1 C9 Si4 C18 47.87(14) . . . . ? Si5 C9 Si4 C18 -76.26(13) . . . . ? C11 C9 Si4 C20 -75.54(16) . . . . ? Si1 C9 Si4 C20 171.51(11) . . . . ? Si5 C9 Si4 C20 47.37(13) . . . . ? C11 C9 Si5 C22 -79.53(16) . . . . ? Si1 C9 Si5 C22 29.58(13) . . . . ? Si4 C9 Si5 C22 157.02(11) . . . . ? C11 C9 Si5 C23 39.97(17) . . . . ? Si1 C9 Si5 C23 149.08(11) . . . . ? Si4 C9 Si5 C23 -83.49(13) . . . . ? C11 C9 Si5 C21 162.20(13) . . . . ? Si1 C9 Si5 C21 -88.69(12) . . . . ? Si4 C9 Si5 C21 38.75(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.366 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.053 #===END data_N-phenylsilanimines _database_code_depnum_ccdc_archive 'CCDC 766386' #TrackingRef '- CIF_silaimines.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H45 N Si5' _chemical_formula_weight 464.04 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1616(9) _cell_length_b 20.601(2) _cell_length_c 14.7242(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.9340(10) _cell_angle_gamma 90.00 _cell_volume 2772.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9010 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 28.54 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.267 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9362 _exptl_absorpt_correction_T_max 0.9738 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31160 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0140 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6356 _reflns_number_gt 5835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.0391P)^2^+0.8921P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6356 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.003 _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 0.88570(3) 0.222294(13) 1.123056(19) 0.01279(7) Uani 1 1 d . . . Si2 Si 0.77298(3) 0.364924(14) 1.15401(2) 0.01487(7) Uani 1 1 d . . . Si3 Si 1.06777(3) 0.336233(14) 1.06366(2) 0.01575(7) Uani 1 1 d . . . Si4 Si 0.86238(3) 0.125186(14) 0.95790(2) 0.01712(7) Uani 1 1 d . . . Si5 Si 0.62666(3) 0.128130(14) 1.10531(2) 0.01659(7) Uani 1 1 d . . . N1 N 0.98462(10) 0.20140(5) 1.21079(6) 0.01889(19) Uani 1 1 d . . . C1 C 1.03248(12) 0.14946(5) 1.26362(7) 0.0175(2) Uani 1 1 d . . . C2 C 1.16521(13) 0.11841(6) 1.24881(8) 0.0235(2) Uani 1 1 d . . . H1 H 1.2232 0.1341 1.2024 0.028 Uiso 1 1 calc R . . C3 C 1.21355(15) 0.06526(6) 1.30066(9) 0.0302(3) Uani 1 1 d . . . H2 H 1.3030 0.0447 1.2886 0.036 Uiso 1 1 calc R . . C4 C 1.13260(16) 0.04194(6) 1.36983(9) 0.0318(3) Uani 1 1 d . . . H3 H 1.1649 0.0052 1.4046 0.038 Uiso 1 1 calc R . . C5 C 1.00363(15) 0.07335(6) 1.38727(8) 0.0289(3) Uani 1 1 d . . . H4 H 0.9481 0.0582 1.4351 0.035 Uiso 1 1 calc R . . C6 C 0.95405(13) 0.12661(6) 1.33611(8) 0.0232(2) Uani 1 1 d . . . H5 H 0.8663 0.1478 1.3502 0.028 Uiso 1 1 calc R . . C7 C 0.87368(11) 0.30642(5) 1.07967(7) 0.01302(19) Uani 1 1 d . . . C8 C 0.78580(11) 0.29547(5) 0.98522(7) 0.01473(19) Uani 1 1 d . . . H6 H 0.7282 0.3349 0.9686 0.018 Uiso 1 1 calc R . . H7 H 0.8552 0.2880 0.9376 0.018 Uiso 1 1 calc R . . C9 C 0.68130(11) 0.23639(5) 0.98930(7) 0.0151(2) Uani 1 1 d . . . H8 H 0.6476 0.2232 0.9267 0.018 Uiso 1 1 calc R . . H9 H 0.5944 0.2489 1.0217 0.018 Uiso 1 1 calc R . . C10 C 0.76084(11) 0.17750(5) 1.03993(7) 0.01366(19) Uani 1 1 d . . . C11 C 0.56972(12) 0.35803(6) 1.13123(8) 0.0210(2) Uani 1 1 d . . . H10 H 0.5363 0.3165 1.1547 0.031 Uiso 1 1 calc R . . H11 H 0.5449 0.3603 1.0655 0.031 Uiso 1 1 calc R . . H12 H 0.5217 0.3937 1.1615 0.031 Uiso 1 1 calc R . . C12 C 0.81101(13) 0.45140(5) 1.12398(8) 0.0219(2) Uani 1 1 d . . . H13 H 0.7514 0.4803 1.1592 0.033 Uiso 1 1 calc R . . H14 H 0.7867 0.4582 1.0588 0.033 Uiso 1 1 calc R . . H15 H 0.9149 0.4609 1.1382 0.033 Uiso 1 1 calc R . . C13 C 0.81953(13) 0.35071(6) 1.27816(8) 0.0239(2) Uani 1 1 d . . . H16 H 0.9257 0.3541 1.2910 0.036 Uiso 1 1 calc R . . H17 H 0.7868 0.3073 1.2948 0.036 Uiso 1 1 calc R . . H18 H 0.7705 0.3833 1.3138 0.036 Uiso 1 1 calc R . . C14 C 1.06321(14) 0.39870(6) 0.97134(9) 0.0261(3) Uani 1 1 d . . . H19 H 1.0077 0.4366 0.9897 0.039 Uiso 1 1 calc R . . H20 H 1.0162 0.3804 0.9153 0.039 Uiso 1 1 calc R . . H21 H 1.1634 0.4119 0.9606 0.039 Uiso 1 1 calc R . . C15 C 1.15560(13) 0.36872(6) 1.17209(9) 0.0270(3) Uani 1 1 d . . . H22 H 1.2577 0.3799 1.1635 0.040 Uiso 1 1 calc R . . H23 H 1.1522 0.3357 1.2199 0.040 Uiso 1 1 calc R . . H24 H 1.1031 0.4076 1.1900 0.040 Uiso 1 1 calc R . . C16 C 1.19259(13) 0.26985(6) 1.02857(9) 0.0265(3) Uani 1 1 d . . . H25 H 1.1534 0.2510 0.9708 0.040 Uiso 1 1 calc R . . H26 H 1.1994 0.2361 1.0756 0.040 Uiso 1 1 calc R . . H27 H 1.2901 0.2878 1.0210 0.040 Uiso 1 1 calc R . . C17 C 0.92489(14) 0.17397(6) 0.86047(8) 0.0257(2) Uani 1 1 d . . . H28 H 1.0012 0.2044 0.8830 0.038 Uiso 1 1 calc R . . H29 H 0.8419 0.1982 0.8319 0.038 Uiso 1 1 calc R . . H30 H 0.9642 0.1448 0.8156 0.038 Uiso 1 1 calc R . . C18 C 1.02781(13) 0.08735(6) 1.01736(9) 0.0268(3) Uani 1 1 d . . . H31 H 0.9988 0.0625 1.0700 0.040 Uiso 1 1 calc R . . H32 H 1.0970 0.1214 1.0380 0.040 Uiso 1 1 calc R . . H33 H 1.0744 0.0583 0.9753 0.040 Uiso 1 1 calc R . . C19 C 0.74189(13) 0.06053(6) 0.90337(8) 0.0229(2) Uani 1 1 d . . . H34 H 0.7951 0.0374 0.8578 0.034 Uiso 1 1 calc R . . H35 H 0.6539 0.0805 0.8738 0.034 Uiso 1 1 calc R . . H36 H 0.7137 0.0299 0.9500 0.034 Uiso 1 1 calc R . . C20 C 0.70984(14) 0.05089(6) 1.15146(8) 0.0253(2) Uani 1 1 d . . . H37 H 0.6385 0.0277 1.1860 0.038 Uiso 1 1 calc R . . H38 H 0.7968 0.0609 1.1915 0.038 Uiso 1 1 calc R . . H39 H 0.7378 0.0236 1.1010 0.038 Uiso 1 1 calc R . . C21 C 0.56572(13) 0.17579(6) 1.20468(8) 0.0250(2) Uani 1 1 d . . . H40 H 0.5080 0.1478 1.2423 0.037 Uiso 1 1 calc R . . H41 H 0.5057 0.2126 1.1824 0.037 Uiso 1 1 calc R . . H42 H 0.6516 0.1919 1.2412 0.037 Uiso 1 1 calc R . . C22 C 0.45683(12) 0.10999(6) 1.03183(8) 0.0241(2) Uani 1 1 d . . . H43 H 0.4795 0.0788 0.9846 0.036 Uiso 1 1 calc R . . H44 H 0.4194 0.1501 1.0032 0.036 Uiso 1 1 calc R . . H45 H 0.3827 0.0916 1.0692 0.036 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 0.01157(13) 0.01295(13) 0.01381(14) 0.00119(10) 0.00058(10) -0.00032(10) Si2 0.01463(14) 0.01483(14) 0.01528(14) -0.00067(10) 0.00199(11) 0.00039(10) Si3 0.01266(14) 0.01548(14) 0.01930(15) -0.00068(11) 0.00243(11) -0.00252(10) Si4 0.01591(15) 0.01674(15) 0.01869(15) -0.00391(11) 0.00112(11) 0.00032(10) Si5 0.01585(14) 0.01579(14) 0.01818(15) 0.00214(11) 0.00157(11) -0.00369(10) N1 0.0178(4) 0.0209(5) 0.0176(4) 0.0029(4) -0.0012(3) 0.0010(4) C1 0.0190(5) 0.0169(5) 0.0157(5) -0.0001(4) -0.0042(4) -0.0026(4) C2 0.0241(6) 0.0266(6) 0.0194(5) 0.0010(4) -0.0018(4) 0.0039(5) C3 0.0358(7) 0.0258(6) 0.0274(6) -0.0035(5) -0.0091(5) 0.0104(5) C4 0.0492(8) 0.0170(5) 0.0266(6) 0.0039(5) -0.0162(6) -0.0014(5) C5 0.0372(7) 0.0281(6) 0.0201(6) 0.0064(5) -0.0067(5) -0.0142(5) C6 0.0216(6) 0.0272(6) 0.0203(6) 0.0028(4) -0.0021(4) -0.0054(4) C7 0.0125(4) 0.0125(4) 0.0140(5) 0.0003(4) 0.0005(4) -0.0006(3) C8 0.0154(5) 0.0145(5) 0.0142(5) 0.0020(4) 0.0003(4) -0.0009(4) C9 0.0141(5) 0.0147(5) 0.0161(5) 0.0009(4) -0.0008(4) -0.0007(4) C10 0.0135(5) 0.0127(4) 0.0147(5) 0.0002(4) 0.0006(4) -0.0013(4) C11 0.0159(5) 0.0228(5) 0.0246(6) -0.0013(4) 0.0040(4) 0.0022(4) C12 0.0249(6) 0.0151(5) 0.0258(6) -0.0023(4) 0.0036(4) 0.0009(4) C13 0.0248(6) 0.0296(6) 0.0175(5) -0.0009(5) 0.0024(4) 0.0014(5) C14 0.0259(6) 0.0239(6) 0.0294(6) 0.0059(5) 0.0088(5) -0.0043(5) C15 0.0168(5) 0.0363(7) 0.0274(6) -0.0067(5) -0.0021(4) -0.0047(5) C16 0.0164(5) 0.0236(6) 0.0401(7) -0.0039(5) 0.0065(5) -0.0011(4) C17 0.0266(6) 0.0297(6) 0.0216(6) -0.0061(5) 0.0084(5) -0.0057(5) C18 0.0210(6) 0.0241(6) 0.0347(7) -0.0083(5) -0.0029(5) 0.0059(5) C19 0.0255(6) 0.0199(5) 0.0228(6) -0.0050(4) -0.0016(4) -0.0012(4) C20 0.0298(6) 0.0203(6) 0.0254(6) 0.0064(5) -0.0016(5) -0.0029(5) C21 0.0239(6) 0.0283(6) 0.0236(6) -0.0005(5) 0.0082(5) -0.0053(5) C22 0.0175(5) 0.0256(6) 0.0290(6) 0.0009(5) 0.0000(4) -0.0060(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 Si1 N1 1.5858(9) . ? Si1 C7 1.8477(10) . ? Si1 C10 1.8618(11) . ? Si2 C13 1.8715(12) . ? Si2 C12 1.8740(12) . ? Si2 C11 1.8748(12) . ? Si2 C7 1.9080(10) . ? Si3 C15 1.8622(13) . ? Si3 C14 1.8702(12) . ? Si3 C16 1.8778(12) . ? Si3 C7 1.9110(11) . ? Si4 C18 1.8679(12) . ? Si4 C17 1.8731(12) . ? Si4 C19 1.8750(12) . ? Si4 C10 1.9078(11) . ? Si5 C22 1.8709(12) . ? Si5 C20 1.8717(12) . ? Si5 C21 1.8784(12) . ? Si5 C10 1.9065(10) . ? N1 C1 1.3767(14) . ? C1 C2 1.4042(16) . ? C1 C6 1.4079(16) . ? C2 C3 1.3898(17) . ? C2 H1 0.9500 . ? C3 C4 1.386(2) . ? C3 H2 0.9500 . ? C4 C5 1.387(2) . ? C4 H3 0.9500 . ? C5 C6 1.3895(17) . ? C5 H4 0.9500 . ? C6 H5 0.9500 . ? C7 C8 1.5746(14) . ? C8 C9 1.5523(14) . ? C8 H6 0.9900 . ? C8 H7 0.9900 . ? C9 C10 1.5761(14) . ? C9 H8 0.9900 . ? C9 H9 0.9900 . ? C11 H10 0.9800 . ? C11 H11 0.9800 . ? C11 H12 0.9800 . ? C12 H13 0.9800 . ? C12 H14 0.9800 . ? C12 H15 0.9800 . ? C13 H16 0.9800 . ? C13 H17 0.9800 . ? C13 H18 0.9800 . ? C14 H19 0.9800 . ? C14 H20 0.9800 . ? C14 H21 0.9800 . ? C15 H22 0.9800 . ? C15 H23 0.9800 . ? C15 H24 0.9800 . ? C16 H25 0.9800 . ? C16 H26 0.9800 . ? C16 H27 0.9800 . ? C17 H28 0.9800 . ? C17 H29 0.9800 . ? C17 H30 0.9800 . ? C18 H31 0.9800 . ? C18 H32 0.9800 . ? C18 H33 0.9800 . ? C19 H34 0.9800 . ? C19 H35 0.9800 . ? C19 H36 0.9800 . ? C20 H37 0.9800 . ? C20 H38 0.9800 . ? C20 H39 0.9800 . ? C21 H40 0.9800 . ? C21 H41 0.9800 . ? C21 H42 0.9800 . ? C22 H43 0.9800 . ? C22 H44 0.9800 . ? C22 H45 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C7 123.60(5) . . ? N1 Si1 C10 133.79(5) . . ? C7 Si1 C10 102.61(5) . . ? C13 Si2 C12 110.22(6) . . ? C13 Si2 C11 108.66(5) . . ? C12 Si2 C11 103.19(5) . . ? C13 Si2 C7 112.01(5) . . ? C12 Si2 C7 111.11(5) . . ? C11 Si2 C7 111.28(5) . . ? C15 Si3 C14 111.27(6) . . ? C15 Si3 C16 105.19(6) . . ? C14 Si3 C16 106.54(6) . . ? C15 Si3 C7 111.15(5) . . ? C14 Si3 C7 109.65(5) . . ? C16 Si3 C7 112.91(5) . . ? C18 Si4 C17 107.58(6) . . ? C18 Si4 C19 109.83(6) . . ? C17 Si4 C19 104.78(6) . . ? C18 Si4 C10 110.74(5) . . ? C17 Si4 C10 111.70(5) . . ? C19 Si4 C10 111.96(5) . . ? C22 Si5 C20 109.99(6) . . ? C22 Si5 C21 105.96(6) . . ? C20 Si5 C21 107.28(6) . . ? C22 Si5 C10 110.73(5) . . ? C20 Si5 C10 112.10(5) . . ? C21 Si5 C10 110.55(5) . . ? C1 N1 Si1 144.42(8) . . ? N1 C1 C2 120.79(10) . . ? N1 C1 C6 121.92(10) . . ? C2 C1 C6 117.25(10) . . ? C3 C2 C1 121.35(12) . . ? C3 C2 H1 119.3 . . ? C1 C2 H1 119.3 . . ? C4 C3 C2 120.68(12) . . ? C4 C3 H2 119.7 . . ? C2 C3 H2 119.7 . . ? C3 C4 C5 118.69(11) . . ? C3 C4 H3 120.7 . . ? C5 C4 H3 120.7 . . ? C4 C5 C6 121.28(12) . . ? C4 C5 H4 119.4 . . ? C6 C5 H4 119.4 . . ? C5 C6 C1 120.67(12) . . ? C5 C6 H5 119.7 . . ? C1 C6 H5 119.7 . . ? C8 C7 Si1 100.70(6) . . ? C8 C7 Si2 111.04(7) . . ? Si1 C7 Si2 114.44(5) . . ? C8 C7 Si3 111.15(7) . . ? Si1 C7 Si3 108.07(5) . . ? Si2 C7 Si3 111.00(5) . . ? C9 C8 C7 110.95(8) . . ? C9 C8 H6 109.4 . . ? C7 C8 H6 109.4 . . ? C9 C8 H7 109.4 . . ? C7 C8 H7 109.4 . . ? H6 C8 H7 108.0 . . ? C8 C9 C10 110.82(8) . . ? C8 C9 H8 109.5 . . ? C10 C9 H8 109.5 . . ? C8 C9 H9 109.5 . . ? C10 C9 H9 109.5 . . ? H8 C9 H9 108.1 . . ? C9 C10 Si1 99.94(6) . . ? C9 C10 Si5 110.87(7) . . ? Si1 C10 Si5 108.71(5) . . ? C9 C10 Si4 111.41(7) . . ? Si1 C10 Si4 113.07(5) . . ? Si5 C10 Si4 112.19(5) . . ? Si2 C11 H10 109.5 . . ? Si2 C11 H11 109.5 . . ? H10 C11 H11 109.5 . . ? Si2 C11 H12 109.5 . . ? H10 C11 H12 109.5 . . ? H11 C11 H12 109.5 . . ? Si2 C12 H13 109.5 . . ? Si2 C12 H14 109.5 . . ? H13 C12 H14 109.5 . . ? Si2 C12 H15 109.5 . . ? H13 C12 H15 109.5 . . ? H14 C12 H15 109.5 . . ? Si2 C13 H16 109.5 . . ? Si2 C13 H17 109.5 . . ? H16 C13 H17 109.5 . . ? Si2 C13 H18 109.5 . . ? H16 C13 H18 109.5 . . ? H17 C13 H18 109.5 . . ? Si3 C14 H19 109.5 . . ? Si3 C14 H20 109.5 . . ? H19 C14 H20 109.5 . . ? Si3 C14 H21 109.5 . . ? H19 C14 H21 109.5 . . ? H20 C14 H21 109.5 . . ? Si3 C15 H22 109.5 . . ? Si3 C15 H23 109.5 . . ? H22 C15 H23 109.5 . . ? Si3 C15 H24 109.5 . . ? H22 C15 H24 109.5 . . ? H23 C15 H24 109.5 . . ? Si3 C16 H25 109.5 . . ? Si3 C16 H26 109.5 . . ? H25 C16 H26 109.5 . . ? Si3 C16 H27 109.5 . . ? H25 C16 H27 109.5 . . ? H26 C16 H27 109.5 . . ? Si4 C17 H28 109.5 . . ? Si4 C17 H29 109.5 . . ? H28 C17 H29 109.5 . . ? Si4 C17 H30 109.5 . . ? H28 C17 H30 109.5 . . ? H29 C17 H30 109.5 . . ? Si4 C18 H31 109.5 . . ? Si4 C18 H32 109.5 . . ? H31 C18 H32 109.5 . . ? Si4 C18 H33 109.5 . . ? H31 C18 H33 109.5 . . ? H32 C18 H33 109.5 . . ? Si4 C19 H34 109.5 . . ? Si4 C19 H35 109.5 . . ? H34 C19 H35 109.5 . . ? Si4 C19 H36 109.5 . . ? H34 C19 H36 109.5 . . ? H35 C19 H36 109.5 . . ? Si5 C20 H37 109.5 . . ? Si5 C20 H38 109.5 . . ? H37 C20 H38 109.5 . . ? Si5 C20 H39 109.5 . . ? H37 C20 H39 109.5 . . ? H38 C20 H39 109.5 . . ? Si5 C21 H40 109.5 . . ? Si5 C21 H41 109.5 . . ? H40 C21 H41 109.5 . . ? Si5 C21 H42 109.5 . . ? H40 C21 H42 109.5 . . ? H41 C21 H42 109.5 . . ? Si5 C22 H43 109.5 . . ? Si5 C22 H44 109.5 . . ? H43 C22 H44 109.5 . . ? Si5 C22 H45 109.5 . . ? H43 C22 H45 109.5 . . ? H44 C22 H45 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 C7 Si1 N1 C1 -175.80(13) . . . . ? C10 Si1 N1 C1 3.84(18) . . . . ? Si1 N1 C1 C2 93.83(16) . . . . ? Si1 N1 C1 C6 -88.30(17) . . . . ? N1 C1 C2 C3 -178.91(11) . . . . ? C6 C1 C2 C3 3.13(17) . . . . ? C1 C2 C3 C4 -1.04(19) . . . . ? C2 C3 C4 C5 -1.05(19) . . . . ? C3 C4 C5 C6 0.94(18) . . . . ? C4 C5 C6 C1 1.24(18) . . . . ? N1 C1 C6 C5 178.85(11) . . . . ? C2 C1 C6 C5 -3.21(17) . . . . ? N1 Si1 C7 C8 170.33(6) . . . . ? C10 Si1 C7 C8 -9.40(7) . . . . ? N1 Si1 C7 Si2 -70.50(7) . . . . ? C10 Si1 C7 Si2 109.77(6) . . . . ? N1 Si1 C7 Si3 53.72(7) . . . . ? C10 Si1 C7 Si3 -126.01(5) . . . . ? C13 Si2 C7 C8 153.47(7) . . . . ? C12 Si2 C7 C8 -82.78(8) . . . . ? C11 Si2 C7 C8 31.61(8) . . . . ? C13 Si2 C7 Si1 40.29(7) . . . . ? C12 Si2 C7 Si1 164.05(6) . . . . ? C11 Si2 C7 Si1 -81.56(7) . . . . ? C13 Si2 C7 Si3 -82.36(6) . . . . ? C12 Si2 C7 Si3 41.40(7) . . . . ? C11 Si2 C7 Si3 155.79(5) . . . . ? C15 Si3 C7 C8 165.77(7) . . . . ? C14 Si3 C7 C8 42.33(8) . . . . ? C16 Si3 C7 C8 -76.29(8) . . . . ? C15 Si3 C7 Si1 -84.61(7) . . . . ? C14 Si3 C7 Si1 151.95(6) . . . . ? C16 Si3 C7 Si1 33.33(7) . . . . ? C15 Si3 C7 Si2 41.66(7) . . . . ? C14 Si3 C7 Si2 -81.78(6) . . . . ? C16 Si3 C7 Si2 159.59(6) . . . . ? Si1 C7 C8 C9 30.22(9) . . . . ? Si2 C7 C8 C9 -91.38(9) . . . . ? Si3 C7 C8 C9 144.53(7) . . . . ? C7 C8 C9 C10 -44.15(11) . . . . ? C8 C9 C10 Si1 32.39(9) . . . . ? C8 C9 C10 Si5 146.93(7) . . . . ? C8 C9 C10 Si4 -87.35(9) . . . . ? N1 Si1 C10 C9 167.65(6) . . . . ? C7 Si1 C10 C9 -12.66(7) . . . . ? N1 Si1 C10 Si5 51.47(8) . . . . ? C7 Si1 C10 Si5 -128.85(5) . . . . ? N1 Si1 C10 Si4 -73.82(8) . . . . ? C7 Si1 C10 Si4 105.87(6) . . . . ? C22 Si5 C10 C9 47.97(8) . . . . ? C20 Si5 C10 C9 171.21(7) . . . . ? C21 Si5 C10 C9 -69.15(8) . . . . ? C22 Si5 C10 Si1 156.89(5) . . . . ? C20 Si5 C10 Si1 -79.87(6) . . . . ? C21 Si5 C10 Si1 39.77(7) . . . . ? C22 Si5 C10 Si4 -77.30(7) . . . . ? C20 Si5 C10 Si4 45.94(7) . . . . ? C21 Si5 C10 Si4 165.58(6) . . . . ? C18 Si4 C10 C9 149.17(7) . . . . ? C17 Si4 C10 C9 29.28(9) . . . . ? C19 Si4 C10 C9 -87.89(8) . . . . ? C18 Si4 C10 Si1 37.53(7) . . . . ? C17 Si4 C10 Si1 -82.36(7) . . . . ? C19 Si4 C10 Si1 160.48(6) . . . . ? C18 Si4 C10 Si5 -85.85(7) . . . . ? C17 Si4 C10 Si5 154.26(6) . . . . ? C19 Si4 C10 Si5 37.09(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.374 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.043 #===END data_N-(1-adamantyl)silanimines _database_code_depnum_ccdc_archive 'CCDC 766387' #TrackingRef '- CIF_silaimines.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H55 N Si5' _chemical_formula_weight 522.16 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' Si Si 0.0817 0.0704 '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 9.445(3) _cell_length_b 10.618(3) _cell_length_c 16.947(5) _cell_angle_alpha 95.035(3) _cell_angle_beta 93.948(3) _cell_angle_gamma 111.147(3) _cell_volume 1569.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 5390 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.35 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9531 _exptl_absorpt_correction_T_max 0.9762 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17268 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.37 _reflns_number_total 6926 _reflns_number_gt 6076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.0519P)^2^+0.6663P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6926 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.66700(5) 0.40858(4) 0.26087(2) 0.01854(10) Uani 1 1 d . . . N1 N 0.72062(17) 0.32959(17) 0.19569(9) 0.0316(3) Uani 1 1 d . . . C1 C 0.77551(18) 0.27116(16) 0.13138(9) 0.0213(3) Uani 1 1 d . . . C2 C 0.65216(19) 0.21946(18) 0.05942(9) 0.0249(3) Uani 1 1 d . . . H1 H 0.5580 0.1522 0.0752 0.030 Uiso 1 1 calc R . . H2 H 0.6275 0.2965 0.0421 0.030 Uiso 1 1 calc R . . C3 C 0.70785(19) 0.15309(18) -0.01009(9) 0.0256(3) Uani 1 1 d . . . H3 H 0.6263 0.1201 -0.0561 0.031 Uiso 1 1 calc R . . C4 C 0.7447(2) 0.03304(17) 0.01603(10) 0.0278(4) Uani 1 1 d . . . H4 H 0.7794 -0.0103 -0.0288 0.033 Uiso 1 1 calc R . . H5 H 0.6519 -0.0357 0.0321 0.033 Uiso 1 1 calc R . . C5 C 0.8702(2) 0.08426(17) 0.08634(10) 0.0255(3) Uani 1 1 d . . . H6 H 0.8946 0.0060 0.1036 0.031 Uiso 1 1 calc R . . C6 C 0.81267(19) 0.14895(17) 0.15559(9) 0.0246(3) Uani 1 1 d . . . H7 H 0.8917 0.1796 0.2020 0.030 Uiso 1 1 calc R . . H8 H 0.7199 0.0802 0.1716 0.030 Uiso 1 1 calc R . . C7 C 0.92081(19) 0.37447(16) 0.10515(10) 0.0249(3) Uani 1 1 d . . . H9 H 0.8992 0.4536 0.0889 0.030 Uiso 1 1 calc R . . H10 H 1.0019 0.4075 0.1506 0.030 Uiso 1 1 calc R . . C8 C 0.9769(2) 0.30962(18) 0.03523(10) 0.0277(4) Uani 1 1 d . . . H11 H 1.0708 0.3785 0.0189 0.033 Uiso 1 1 calc R . . C9 C 0.8516(2) 0.2587(2) -0.03518(10) 0.0312(4) Uani 1 1 d . . . H12 H 0.8279 0.3360 -0.0527 0.037 Uiso 1 1 calc R . . H13 H 0.8875 0.2173 -0.0804 0.037 Uiso 1 1 calc R . . C10 C 1.0132(2) 0.18931(18) 0.06114(10) 0.0286(4) Uani 1 1 d . . . H14 H 1.0499 0.1473 0.0165 0.034 Uiso 1 1 calc R . . H15 H 1.0950 0.2214 0.1062 0.034 Uiso 1 1 calc R . . C11 C 0.57586(18) 0.34355(16) 0.35150(9) 0.0210(3) Uani 1 1 d . . . C12 C 0.57444(19) 0.47751(17) 0.39807(9) 0.0236(3) Uani 1 1 d . . . H16 H 0.4858 0.4549 0.4295 0.028 Uiso 1 1 calc R . . H17 H 0.6684 0.5195 0.4357 0.028 Uiso 1 1 calc R . . C13 C 0.56507(19) 0.58056(17) 0.34063(9) 0.0239(3) Uani 1 1 d . . . H18 H 0.5943 0.6718 0.3711 0.029 Uiso 1 1 calc R . . H19 H 0.4586 0.5531 0.3160 0.029 Uiso 1 1 calc R . . C14 C 0.67324(18) 0.58794(16) 0.27343(9) 0.0203(3) Uani 1 1 d . . . Si2 Si 0.37528(5) 0.21008(5) 0.32906(3) 0.02728(12) Uani 1 1 d . . . C15 C 0.3139(2) 0.1205(2) 0.41903(13) 0.0452(5) Uani 1 1 d . . . H20 H 0.2056 0.0621 0.4091 0.068 Uiso 1 1 calc R . . H21 H 0.3296 0.1880 0.4653 0.068 Uiso 1 1 calc R . . H22 H 0.3747 0.0648 0.4295 0.068 Uiso 1 1 calc R . . C16 C 0.2307(2) 0.2894(2) 0.30938(14) 0.0417(5) Uani 1 1 d . . . H23 H 0.2486 0.3329 0.2604 0.063 Uiso 1 1 calc R . . H24 H 0.2398 0.3578 0.3542 0.063 Uiso 1 1 calc R . . H25 H 0.1279 0.2190 0.3032 0.063 Uiso 1 1 calc R . . C17 C 0.3582(2) 0.0839(2) 0.24138(12) 0.0418(5) Uani 1 1 d . . . H26 H 0.2551 0.0139 0.2341 0.063 Uiso 1 1 calc R . . H27 H 0.4331 0.0412 0.2506 0.063 Uiso 1 1 calc R . . H28 H 0.3773 0.1303 0.1935 0.063 Uiso 1 1 calc R . . Si3 Si 0.70713(5) 0.27656(5) 0.41031(3) 0.02584(12) Uani 1 1 d . . . C18 C 0.6756(3) 0.0956(2) 0.37621(12) 0.0410(5) Uani 1 1 d . . . H29 H 0.6874 0.0856 0.3193 0.061 Uiso 1 1 calc R . . H30 H 0.5723 0.0372 0.3852 0.061 Uiso 1 1 calc R . . H31 H 0.7506 0.0689 0.4062 0.061 Uiso 1 1 calc R . . C19 C 0.6833(2) 0.2948(2) 0.51944(10) 0.0375(4) Uani 1 1 d . . . H32 H 0.5759 0.2474 0.5272 0.056 Uiso 1 1 calc R . . H33 H 0.7148 0.3914 0.5394 0.056 Uiso 1 1 calc R . . H34 H 0.7467 0.2550 0.5487 0.056 Uiso 1 1 calc R . . C20 C 0.9118(2) 0.3750(2) 0.39915(11) 0.0353(4) Uani 1 1 d . . . H35 H 0.9772 0.3418 0.4320 0.053 Uiso 1 1 calc R . . H36 H 0.9359 0.4717 0.4164 0.053 Uiso 1 1 calc R . . H37 H 0.9296 0.3632 0.3432 0.053 Uiso 1 1 calc R . . Si4 Si 0.58191(5) 0.62207(5) 0.17802(3) 0.02373(11) Uani 1 1 d . . . C21 C 0.4084(2) 0.4722(2) 0.13478(11) 0.0373(4) Uani 1 1 d . . . H38 H 0.3265 0.4616 0.1691 0.056 Uiso 1 1 calc R . . H39 H 0.4330 0.3899 0.1311 0.056 Uiso 1 1 calc R . . H40 H 0.3748 0.4868 0.0815 0.056 Uiso 1 1 calc R . . C22 C 0.5125(2) 0.7647(2) 0.20044(12) 0.0367(4) Uani 1 1 d . . . H41 H 0.6001 0.8496 0.2165 0.055 Uiso 1 1 calc R . . H42 H 0.4472 0.7449 0.2438 0.055 Uiso 1 1 calc R . . H43 H 0.4539 0.7739 0.1528 0.055 Uiso 1 1 calc R . . C23 C 0.7136(2) 0.6584(2) 0.09864(10) 0.0345(4) Uani 1 1 d . . . H44 H 0.6674 0.6875 0.0537 0.052 Uiso 1 1 calc R . . H45 H 0.7320 0.5759 0.0805 0.052 Uiso 1 1 calc R . . H46 H 0.8108 0.7308 0.1200 0.052 Uiso 1 1 calc R . . Si5 Si 0.87301(5) 0.72066(5) 0.30436(3) 0.02256(11) Uani 1 1 d . . . C24 C 0.9182(2) 0.7514(2) 0.41545(10) 0.0350(4) Uani 1 1 d . . . H47 H 0.9159 0.6670 0.4356 0.053 Uiso 1 1 calc R . . H48 H 0.8423 0.7813 0.4393 0.053 Uiso 1 1 calc R . . H49 H 1.0200 0.8220 0.4295 0.053 Uiso 1 1 calc R . . C25 C 0.8936(2) 0.89290(19) 0.27678(12) 0.0379(4) Uani 1 1 d . . . H50 H 0.9974 0.9574 0.2949 0.057 Uiso 1 1 calc R . . H51 H 0.8198 0.9236 0.3022 0.057 Uiso 1 1 calc R . . H52 H 0.8746 0.8879 0.2188 0.057 Uiso 1 1 calc R . . C26 C 1.0249(2) 0.67248(19) 0.26055(11) 0.0312(4) Uani 1 1 d . . . H53 H 1.0052 0.6595 0.2023 0.047 Uiso 1 1 calc R . . H54 H 1.0245 0.5877 0.2793 0.047 Uiso 1 1 calc R . . H55 H 1.1246 0.7450 0.2770 0.047 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 0.0177(2) 0.0199(2) 0.0175(2) 0.00023(16) 0.00199(15) 0.00676(17) N1 0.0237(7) 0.0406(9) 0.0282(7) -0.0105(6) 0.0010(6) 0.0129(7) C1 0.0208(8) 0.0216(7) 0.0206(7) -0.0017(6) 0.0023(6) 0.0077(6) C2 0.0218(8) 0.0291(8) 0.0239(8) -0.0021(6) -0.0005(6) 0.0111(7) C3 0.0273(8) 0.0297(9) 0.0197(7) -0.0012(6) -0.0009(6) 0.0122(7) C4 0.0311(9) 0.0227(8) 0.0270(8) -0.0043(6) 0.0010(7) 0.0088(7) C5 0.0313(9) 0.0210(8) 0.0263(8) 0.0006(6) 0.0008(7) 0.0129(7) C6 0.0271(8) 0.0245(8) 0.0213(7) 0.0035(6) 0.0023(6) 0.0083(7) C7 0.0248(8) 0.0196(8) 0.0292(8) 0.0002(6) 0.0055(6) 0.0070(6) C8 0.0251(8) 0.0259(8) 0.0301(9) 0.0023(7) 0.0101(7) 0.0063(7) C9 0.0395(10) 0.0372(10) 0.0213(8) 0.0072(7) 0.0086(7) 0.0175(8) C10 0.0246(8) 0.0328(9) 0.0295(8) -0.0033(7) 0.0027(7) 0.0137(7) C11 0.0198(7) 0.0234(8) 0.0196(7) 0.0018(6) 0.0031(6) 0.0077(6) C12 0.0243(8) 0.0278(8) 0.0192(7) -0.0003(6) 0.0047(6) 0.0107(7) C13 0.0238(8) 0.0259(8) 0.0228(7) -0.0018(6) 0.0029(6) 0.0114(7) C14 0.0216(8) 0.0200(7) 0.0190(7) 0.0005(6) 0.0010(6) 0.0082(6) Si2 0.0225(2) 0.0280(2) 0.0274(2) 0.00192(19) 0.00540(18) 0.00448(19) C15 0.0350(11) 0.0508(13) 0.0408(11) 0.0136(10) 0.0123(9) 0.0017(10) C16 0.0202(9) 0.0416(11) 0.0577(13) 0.0043(10) 0.0025(8) 0.0054(8) C17 0.0348(11) 0.0350(10) 0.0423(11) -0.0076(9) 0.0059(8) -0.0006(8) Si3 0.0286(2) 0.0324(3) 0.0213(2) 0.00646(18) 0.00503(17) 0.0158(2) C18 0.0544(13) 0.0367(11) 0.0410(11) 0.0098(9) 0.0091(9) 0.0260(10) C19 0.0400(11) 0.0546(12) 0.0242(9) 0.0080(8) 0.0052(7) 0.0238(10) C20 0.0283(9) 0.0522(12) 0.0307(9) 0.0091(8) 0.0013(7) 0.0206(9) Si4 0.0247(2) 0.0253(2) 0.0212(2) 0.00173(17) -0.00161(17) 0.01010(19) C21 0.0311(10) 0.0402(11) 0.0332(10) -0.0005(8) -0.0084(7) 0.0077(8) C22 0.0420(11) 0.0372(10) 0.0382(10) 0.0055(8) -0.0021(8) 0.0241(9) C23 0.0406(11) 0.0401(10) 0.0245(8) 0.0082(8) 0.0049(7) 0.0158(9) Si5 0.0220(2) 0.0208(2) 0.0226(2) -0.00038(17) -0.00073(16) 0.00649(18) C24 0.0312(10) 0.0399(10) 0.0261(9) -0.0046(8) -0.0050(7) 0.0071(8) C25 0.0386(11) 0.0239(9) 0.0460(11) 0.0028(8) -0.0040(8) 0.0073(8) C26 0.0240(9) 0.0299(9) 0.0364(9) 0.0007(7) 0.0049(7) 0.0064(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.5496(14) . ? Si1 C11 1.8751(16) . ? Si1 C14 1.8766(16) . ? N1 C1 1.426(2) . ? C1 C7 1.539(2) . ? C1 C2 1.540(2) . ? C1 C6 1.542(2) . ? C2 C3 1.539(2) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 C4 1.529(2) . ? C3 C9 1.532(3) . ? C3 H3 1.0000 . ? C4 C5 1.532(2) . ? C4 H4 0.9900 . ? C4 H5 0.9900 . ? C5 C10 1.525(2) . ? C5 C6 1.536(2) . ? C5 H6 1.0000 . ? C6 H7 0.9900 . ? C6 H8 0.9900 . ? C7 C8 1.538(2) . ? C7 H9 0.9900 . ? C7 H10 0.9900 . ? C8 C10 1.529(2) . ? C8 C9 1.532(2) . ? C8 H11 1.0000 . ? C9 H12 0.9900 . ? C9 H13 0.9900 . ? C10 H14 0.9900 . ? C10 H15 0.9900 . ? C11 C12 1.570(2) . ? C11 Si2 1.9004(17) . ? C11 Si3 1.9045(16) . ? C12 C13 1.548(2) . ? C12 H16 0.9900 . ? C12 H17 0.9900 . ? C13 C14 1.570(2) . ? C13 H18 0.9900 . ? C13 H19 0.9900 . ? C14 Si4 1.9041(16) . ? C14 Si5 1.9070(17) . ? Si2 C17 1.868(2) . ? Si2 C16 1.871(2) . ? Si2 C15 1.883(2) . ? C15 H20 0.9800 . ? C15 H21 0.9800 . ? C15 H22 0.9800 . ? C16 H23 0.9800 . ? C16 H24 0.9800 . ? C16 H25 0.9800 . ? C17 H26 0.9800 . ? C17 H27 0.9800 . ? C17 H28 0.9800 . ? Si3 C18 1.866(2) . ? Si3 C20 1.869(2) . ? Si3 C19 1.8801(19) . ? C18 H29 0.9800 . ? C18 H30 0.9800 . ? C18 H31 0.9800 . ? C19 H32 0.9800 . ? C19 H33 0.9800 . ? C19 H34 0.9800 . ? C20 H35 0.9800 . ? C20 H36 0.9800 . ? C20 H37 0.9800 . ? Si4 C23 1.8661(19) . ? Si4 C21 1.872(2) . ? Si4 C22 1.8750(19) . ? C21 H38 0.9800 . ? C21 H39 0.9800 . ? C21 H40 0.9800 . ? C22 H41 0.9800 . ? C22 H42 0.9800 . ? C22 H43 0.9800 . ? C23 H44 0.9800 . ? C23 H45 0.9800 . ? C23 H46 0.9800 . ? Si5 C26 1.8653(18) . ? Si5 C25 1.873(2) . ? Si5 C24 1.8745(19) . ? C24 H47 0.9800 . ? C24 H48 0.9800 . ? C24 H49 0.9800 . ? C25 H50 0.9800 . ? C25 H51 0.9800 . ? C25 H52 0.9800 . ? C26 H53 0.9800 . ? C26 H54 0.9800 . ? C26 H55 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C11 127.30(8) . . ? N1 Si1 C14 131.72(8) . . ? C11 Si1 C14 100.98(7) . . ? C1 N1 Si1 173.30(15) . . ? N1 C1 C7 111.87(13) . . ? N1 C1 C2 109.83(13) . . ? C7 C1 C2 108.47(13) . . ? N1 C1 C6 110.54(14) . . ? C7 C1 C6 108.14(13) . . ? C2 C1 C6 107.89(13) . . ? C3 C2 C1 110.66(13) . . ? C3 C2 H1 109.5 . . ? C1 C2 H1 109.5 . . ? C3 C2 H2 109.5 . . ? C1 C2 H2 109.5 . . ? H1 C2 H2 108.1 . . ? C4 C3 C9 109.54(14) . . ? C4 C3 C2 109.81(14) . . ? C9 C3 C2 109.14(14) . . ? C4 C3 H3 109.4 . . ? C9 C3 H3 109.4 . . ? C2 C3 H3 109.4 . . ? C3 C4 C5 109.21(13) . . ? C3 C4 H4 109.8 . . ? C5 C4 H4 109.8 . . ? C3 C4 H5 109.8 . . ? C5 C4 H5 109.8 . . ? H4 C4 H5 108.3 . . ? C10 C5 C4 109.64(14) . . ? C10 C5 C6 109.95(13) . . ? C4 C5 C6 108.84(14) . . ? C10 C5 H6 109.5 . . ? C4 C5 H6 109.5 . . ? C6 C5 H6 109.5 . . ? C5 C6 C1 110.93(13) . . ? C5 C6 H7 109.5 . . ? C1 C6 H7 109.5 . . ? C5 C6 H8 109.5 . . ? C1 C6 H8 109.5 . . ? H7 C6 H8 108.0 . . ? C8 C7 C1 110.93(13) . . ? C8 C7 H9 109.5 . . ? C1 C7 H9 109.5 . . ? C8 C7 H10 109.5 . . ? C1 C7 H10 109.5 . . ? H9 C7 H10 108.0 . . ? C10 C8 C9 109.10(14) . . ? C10 C8 C7 109.28(14) . . ? C9 C8 C7 109.53(14) . . ? C10 C8 H11 109.6 . . ? C9 C8 H11 109.6 . . ? C7 C8 H11 109.6 . . ? C3 C9 C8 109.63(14) . . ? C3 C9 H12 109.7 . . ? C8 C9 H12 109.7 . . ? C3 C9 H13 109.7 . . ? C8 C9 H13 109.7 . . ? H12 C9 H13 108.2 . . ? C5 C10 C8 109.71(13) . . ? C5 C10 H14 109.7 . . ? C8 C10 H14 109.7 . . ? C5 C10 H15 109.7 . . ? C8 C10 H15 109.7 . . ? H14 C10 H15 108.2 . . ? C12 C11 Si1 101.45(10) . . ? C12 C11 Si2 111.16(10) . . ? Si1 C11 Si2 114.17(8) . . ? C12 C11 Si3 110.01(10) . . ? Si1 C11 Si3 108.39(8) . . ? Si2 C11 Si3 111.21(8) . . ? C13 C12 C11 111.47(12) . . ? C13 C12 H16 109.3 . . ? C11 C12 H16 109.3 . . ? C13 C12 H17 109.3 . . ? C11 C12 H17 109.3 . . ? H16 C12 H17 108.0 . . ? C12 C13 C14 111.24(12) . . ? C12 C13 H18 109.4 . . ? C14 C13 H18 109.4 . . ? C12 C13 H19 109.4 . . ? C14 C13 H19 109.4 . . ? H18 C13 H19 108.0 . . ? C13 C14 Si1 100.91(10) . . ? C13 C14 Si4 108.99(10) . . ? Si1 C14 Si4 108.99(8) . . ? C13 C14 Si5 111.90(10) . . ? Si1 C14 Si5 113.67(8) . . ? Si4 C14 Si5 111.80(8) . . ? C17 Si2 C16 108.27(10) . . ? C17 Si2 C15 110.30(11) . . ? C16 Si2 C15 103.48(10) . . ? C17 Si2 C11 112.25(8) . . ? C16 Si2 C11 111.55(9) . . ? C15 Si2 C11 110.64(9) . . ? Si2 C15 H20 109.5 . . ? Si2 C15 H21 109.5 . . ? H20 C15 H21 109.5 . . ? Si2 C15 H22 109.5 . . ? H20 C15 H22 109.5 . . ? H21 C15 H22 109.5 . . ? Si2 C16 H23 109.5 . . ? Si2 C16 H24 109.5 . . ? H23 C16 H24 109.5 . . ? Si2 C16 H25 109.5 . . ? H23 C16 H25 109.5 . . ? H24 C16 H25 109.5 . . ? Si2 C17 H26 109.5 . . ? Si2 C17 H27 109.5 . . ? H26 C17 H27 109.5 . . ? Si2 C17 H28 109.5 . . ? H26 C17 H28 109.5 . . ? H27 C17 H28 109.5 . . ? C18 Si3 C20 105.44(10) . . ? C18 Si3 C19 109.28(10) . . ? C20 Si3 C19 107.36(9) . . ? C18 Si3 C11 113.31(9) . . ? C20 Si3 C11 110.96(8) . . ? C19 Si3 C11 110.23(8) . . ? Si3 C18 H29 109.5 . . ? Si3 C18 H30 109.5 . . ? H29 C18 H30 109.5 . . ? Si3 C18 H31 109.5 . . ? H29 C18 H31 109.5 . . ? H30 C18 H31 109.5 . . ? Si3 C19 H32 109.5 . . ? Si3 C19 H33 109.5 . . ? H32 C19 H33 109.5 . . ? Si3 C19 H34 109.5 . . ? H32 C19 H34 109.5 . . ? H33 C19 H34 109.5 . . ? Si3 C20 H35 109.5 . . ? Si3 C20 H36 109.5 . . ? H35 C20 H36 109.5 . . ? Si3 C20 H37 109.5 . . ? H35 C20 H37 109.5 . . ? H36 C20 H37 109.5 . . ? C23 Si4 C21 106.25(9) . . ? C23 Si4 C22 111.09(9) . . ? C21 Si4 C22 105.41(9) . . ? C23 Si4 C14 112.42(8) . . ? C21 Si4 C14 111.62(8) . . ? C22 Si4 C14 109.80(8) . . ? Si4 C21 H38 109.5 . . ? Si4 C21 H39 109.5 . . ? H38 C21 H39 109.5 . . ? Si4 C21 H40 109.5 . . ? H38 C21 H40 109.5 . . ? H39 C21 H40 109.5 . . ? Si4 C22 H41 109.5 . . ? Si4 C22 H42 109.5 . . ? H41 C22 H42 109.5 . . ? Si4 C22 H43 109.5 . . ? H41 C22 H43 109.5 . . ? H42 C22 H43 109.5 . . ? Si4 C23 H44 109.5 . . ? Si4 C23 H45 109.5 . . ? H44 C23 H45 109.5 . . ? Si4 C23 H46 109.5 . . ? H44 C23 H46 109.5 . . ? H45 C23 H46 109.5 . . ? C26 Si5 C25 107.75(9) . . ? C26 Si5 C24 108.36(9) . . ? C25 Si5 C24 103.26(9) . . ? C26 Si5 C14 112.74(8) . . ? C25 Si5 C14 112.79(8) . . ? C24 Si5 C14 111.41(8) . . ? Si5 C24 H47 109.5 . . ? Si5 C24 H48 109.5 . . ? H47 C24 H48 109.5 . . ? Si5 C24 H49 109.5 . . ? H47 C24 H49 109.5 . . ? H48 C24 H49 109.5 . . ? Si5 C25 H50 109.5 . . ? Si5 C25 H51 109.5 . . ? H50 C25 H51 109.5 . . ? Si5 C25 H52 109.5 . . ? H50 C25 H52 109.5 . . ? H51 C25 H52 109.5 . . ? Si5 C26 H53 109.5 . . ? Si5 C26 H54 109.5 . . ? H53 C26 H54 109.5 . . ? Si5 C26 H55 109.5 . . ? H53 C26 H55 109.5 . . ? H54 C26 H55 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 C11 Si1 N1 C1 -180(100) . . . . ? C14 Si1 N1 C1 0.1(11) . . . . ? Si1 N1 C1 C7 36.5(11) . . . . ? Si1 N1 C1 C2 -84.0(11) . . . . ? Si1 N1 C1 C6 157.1(10) . . . . ? N1 C1 C2 C3 -178.75(14) . . . . ? C7 C1 C2 C3 58.71(17) . . . . ? C6 C1 C2 C3 -58.20(17) . . . . ? C1 C2 C3 C4 59.76(18) . . . . ? C1 C2 C3 C9 -60.32(17) . . . . ? C9 C3 C4 C5 59.75(18) . . . . ? C2 C3 C4 C5 -60.09(18) . . . . ? C3 C4 C5 C10 -59.92(17) . . . . ? C3 C4 C5 C6 60.38(18) . . . . ? C10 C5 C6 C1 59.09(17) . . . . ? C4 C5 C6 C1 -61.01(18) . . . . ? N1 C1 C6 C5 179.36(13) . . . . ? C7 C1 C6 C5 -57.87(17) . . . . ? C2 C1 C6 C5 59.26(17) . . . . ? N1 C1 C7 C8 -179.42(14) . . . . ? C2 C1 C7 C8 -58.12(17) . . . . ? C6 C1 C7 C8 58.63(17) . . . . ? C1 C7 C8 C10 -60.25(18) . . . . ? C1 C7 C8 C9 59.22(18) . . . . ? C4 C3 C9 C8 -60.08(17) . . . . ? C2 C3 C9 C8 60.17(17) . . . . ? C10 C8 C9 C3 59.90(18) . . . . ? C7 C8 C9 C3 -59.67(18) . . . . ? C4 C5 C10 C8 60.31(17) . . . . ? C6 C5 C10 C8 -59.31(17) . . . . ? C9 C8 C10 C5 -60.06(17) . . . . ? C7 C8 C10 C5 59.67(18) . . . . ? N1 Si1 C11 C12 171.46(10) . . . . ? C14 Si1 C11 C12 -8.31(11) . . . . ? N1 Si1 C11 Si2 -68.90(12) . . . . ? C14 Si1 C11 Si2 111.34(9) . . . . ? N1 Si1 C11 Si3 55.65(12) . . . . ? C14 Si1 C11 Si3 -124.11(8) . . . . ? Si1 C11 C12 C13 28.73(14) . . . . ? Si2 C11 C12 C13 -93.03(13) . . . . ? Si3 C11 C12 C13 143.33(11) . . . . ? C11 C12 C13 C14 -42.69(17) . . . . ? C12 C13 C14 Si1 31.98(14) . . . . ? C12 C13 C14 Si4 146.61(11) . . . . ? C12 C13 C14 Si5 -89.23(14) . . . . ? N1 Si1 C14 C13 167.26(10) . . . . ? C11 Si1 C14 C13 -12.99(11) . . . . ? N1 Si1 C14 Si4 52.63(13) . . . . ? C11 Si1 C14 Si4 -127.62(8) . . . . ? N1 Si1 C14 Si5 -72.79(12) . . . . ? C11 Si1 C14 Si5 106.96(9) . . . . ? C12 C11 Si2 C17 156.04(12) . . . . ? Si1 C11 Si2 C17 42.02(12) . . . . ? Si3 C11 Si2 C17 -81.01(11) . . . . ? C12 C11 Si2 C16 34.33(14) . . . . ? Si1 C11 Si2 C16 -79.69(11) . . . . ? Si3 C11 Si2 C16 157.28(9) . . . . ? C12 C11 Si2 C15 -80.27(13) . . . . ? Si1 C11 Si2 C15 165.71(10) . . . . ? Si3 C11 Si2 C15 42.67(12) . . . . ? C12 C11 Si3 C18 163.49(12) . . . . ? Si1 C11 Si3 C18 -86.41(11) . . . . ? Si2 C11 Si3 C18 39.88(11) . . . . ? C12 C11 Si3 C20 -78.12(13) . . . . ? Si1 C11 Si3 C20 31.98(11) . . . . ? Si2 C11 Si3 C20 158.27(9) . . . . ? C12 C11 Si3 C19 40.68(14) . . . . ? Si1 C11 Si3 C19 150.78(9) . . . . ? Si2 C11 Si3 C19 -82.93(11) . . . . ? C13 C14 Si4 C23 171.48(11) . . . . ? Si1 C14 Si4 C23 -79.24(10) . . . . ? Si5 C14 Si4 C23 47.26(11) . . . . ? C13 C14 Si4 C21 -69.25(13) . . . . ? Si1 C14 Si4 C21 40.03(11) . . . . ? Si5 C14 Si4 C21 166.54(9) . . . . ? C13 C14 Si4 C22 47.28(13) . . . . ? Si1 C14 Si4 C22 156.56(9) . . . . ? Si5 C14 Si4 C22 -76.94(11) . . . . ? C13 C14 Si5 C26 147.57(11) . . . . ? Si1 C14 Si5 C26 34.06(11) . . . . ? Si4 C14 Si5 C26 -89.86(10) . . . . ? C13 C14 Si5 C25 -90.11(13) . . . . ? Si1 C14 Si5 C25 156.38(9) . . . . ? Si4 C14 Si5 C25 32.47(11) . . . . ? C13 C14 Si5 C24 25.48(13) . . . . ? Si1 C14 Si5 C24 -88.03(10) . . . . ? Si4 C14 Si5 C24 148.06(9) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.37 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.526 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.054 #===END data_N-(trimethylsilyl)silanimines _database_code_depnum_ccdc_archive 'CCDC 766388' #TrackingRef '- CIF_silaimines.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H49 N Si6' _chemical_formula_weight 460.13 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.673(5) _cell_length_b 9.188(3) _cell_length_c 21.868(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.864(4) _cell_angle_gamma 90.00 _cell_volume 2927.0(19) _cell_formula_units_Z 4 _cell_measurement_temperature 120 _cell_measurement_reflns_used 8870 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.43 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.291 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9178 _exptl_absorpt_correction_T_max 0.9715 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25067 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6344 _reflns_number_gt 5605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.0440P)^2^+2.3627P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6344 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1145 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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 0.24611(4) 0.69655(5) 0.41499(2) 0.01940(12) Uani 1 1 d . . . N1 N 0.16138(12) 0.79203(19) 0.38950(8) 0.0294(4) Uani 1 1 d . . . Si2 Si 0.06750(4) 0.88712(7) 0.36280(3) 0.02964(14) Uani 1 1 d . . . C1 C 0.29683(13) 0.6639(2) 0.49567(8) 0.0210(4) Uani 1 1 d . . . C2 C 0.38606(14) 0.5769(2) 0.48560(8) 0.0258(4) Uani 1 1 d . . . H1 H 0.4378 0.6457 0.4846 0.031 Uiso 1 1 calc R . . H2 H 0.4018 0.5094 0.5206 0.031 Uiso 1 1 calc R . . C3 C 0.37250(14) 0.4891(2) 0.42462(8) 0.0248(4) Uani 1 1 d . . . H3 H 0.3361 0.4005 0.4303 0.030 Uiso 1 1 calc R . . H4 H 0.4330 0.4585 0.4134 0.030 Uiso 1 1 calc R . . C4 C 0.32164(13) 0.5842(2) 0.37151(8) 0.0212(4) Uani 1 1 d . . . C5 C 0.0467(2) 1.0400(3) 0.41500(14) 0.0579(8) Uani 1 1 d . . . H5 H 0.0329 1.0011 0.4546 0.087 Uiso 1 1 calc R . . H6 H -0.0054 1.0981 0.3964 0.087 Uiso 1 1 calc R . . H7 H 0.1016 1.1014 0.4216 0.087 Uiso 1 1 calc R . . C6 C 0.07816(19) 0.9693(3) 0.28585(12) 0.0497(7) Uani 1 1 d . . . H8 H 0.1345 1.0274 0.2882 0.075 Uiso 1 1 calc R . . H9 H 0.0250 1.0318 0.2736 0.075 Uiso 1 1 calc R . . H10 H 0.0806 0.8917 0.2553 0.075 Uiso 1 1 calc R . . C7 C -0.03514(19) 0.7649(3) 0.35652(16) 0.0567(8) Uani 1 1 d . . . H11 H -0.0285 0.6889 0.3259 0.085 Uiso 1 1 calc R . . H12 H -0.0906 0.8220 0.3438 0.085 Uiso 1 1 calc R . . H13 H -0.0401 0.7198 0.3966 0.085 Uiso 1 1 calc R . . Si3 Si 0.32729(4) 0.84880(6) 0.53312(2) 0.02538(13) Uani 1 1 d . . . C8 C 0.36013(17) 0.9858(2) 0.47593(10) 0.0336(5) Uani 1 1 d . . . H14 H 0.3073 1.0052 0.4452 0.050 Uiso 1 1 calc R . . H15 H 0.4109 0.9474 0.4554 0.050 Uiso 1 1 calc R . . H16 H 0.3794 1.0764 0.4974 0.050 Uiso 1 1 calc R . . C9 C 0.42896(18) 0.8250(3) 0.59281(11) 0.0411(6) Uani 1 1 d . . . H17 H 0.4423 0.9172 0.6146 0.062 Uiso 1 1 calc R . . H18 H 0.4823 0.7954 0.5728 0.062 Uiso 1 1 calc R . . H19 H 0.4155 0.7499 0.6223 0.062 Uiso 1 1 calc R . . C10 C 0.23069(18) 0.9357(2) 0.56789(10) 0.0370(5) Uani 1 1 d . . . H20 H 0.2513 1.0287 0.5867 0.055 Uiso 1 1 calc R . . H21 H 0.2108 0.8713 0.5994 0.055 Uiso 1 1 calc R . . H22 H 0.1793 0.9528 0.5358 0.055 Uiso 1 1 calc R . . Si4 Si 0.22020(4) 0.55455(6) 0.54337(2) 0.02631(14) Uani 1 1 d . . . C11 C 0.2634(2) 0.5614(3) 0.62746(10) 0.0422(6) Uani 1 1 d . . . H23 H 0.2609 0.6618 0.6422 0.063 Uiso 1 1 calc R . . H24 H 0.3269 0.5265 0.6338 0.063 Uiso 1 1 calc R . . H25 H 0.2250 0.4993 0.6503 0.063 Uiso 1 1 calc R . . C12 C 0.09937(17) 0.6198(3) 0.53064(12) 0.0411(5) Uani 1 1 d . . . H26 H 0.0735 0.5991 0.4881 0.062 Uiso 1 1 calc R . . H27 H 0.0978 0.7249 0.5380 0.062 Uiso 1 1 calc R . . H28 H 0.0631 0.5698 0.5591 0.062 Uiso 1 1 calc R . . C13 C 0.2221(2) 0.3562(2) 0.52403(11) 0.0422(6) Uani 1 1 d . . . H29 H 0.1894 0.3013 0.5530 0.063 Uiso 1 1 calc R . . H30 H 0.2859 0.3225 0.5269 0.063 Uiso 1 1 calc R . . H31 H 0.1921 0.3410 0.4820 0.063 Uiso 1 1 calc R . . Si5 Si 0.40516(4) 0.69526(6) 0.33010(2) 0.02591(13) Uani 1 1 d . . . C14 C 0.35136(17) 0.8683(3) 0.29852(10) 0.0363(5) Uani 1 1 d . . . H32 H 0.3401 0.9325 0.3326 0.055 Uiso 1 1 calc R . . H33 H 0.2930 0.8464 0.2735 0.055 Uiso 1 1 calc R . . H34 H 0.3927 0.9167 0.2729 0.055 Uiso 1 1 calc R . . C15 C 0.51274(15) 0.7419(3) 0.38145(10) 0.0355(5) Uani 1 1 d . . . H35 H 0.5549 0.7942 0.3577 0.053 Uiso 1 1 calc R . . H36 H 0.5421 0.6523 0.3982 0.053 Uiso 1 1 calc R . . H37 H 0.4975 0.8037 0.4153 0.053 Uiso 1 1 calc R . . C16 C 0.4506(2) 0.5876(3) 0.26764(12) 0.0486(7) Uani 1 1 d . . . H38 H 0.4961 0.6458 0.2491 0.073 Uiso 1 1 calc R . . H39 H 0.4000 0.5622 0.2360 0.073 Uiso 1 1 calc R . . H40 H 0.4796 0.4983 0.2851 0.073 Uiso 1 1 calc R . . Si6 Si 0.24385(5) 0.46780(6) 0.31456(3) 0.03025(14) Uani 1 1 d . . . C17 C 0.19903(19) 0.5757(3) 0.24514(10) 0.0449(6) Uani 1 1 d . . . H41 H 0.1575 0.5151 0.2174 0.067 Uiso 1 1 calc R . . H42 H 0.2504 0.6080 0.2237 0.067 Uiso 1 1 calc R . . H43 H 0.1656 0.6608 0.2578 0.067 Uiso 1 1 calc R . . C18 C 0.3067(2) 0.3015(3) 0.29287(15) 0.0590(8) Uani 1 1 d . . . H44 H 0.3339 0.2517 0.3303 0.089 Uiso 1 1 calc R . . H45 H 0.3553 0.3301 0.2682 0.089 Uiso 1 1 calc R . . H46 H 0.2636 0.2358 0.2688 0.089 Uiso 1 1 calc R . . C19 C 0.14144(19) 0.4011(3) 0.34925(12) 0.0461(6) Uani 1 1 d . . . H47 H 0.1011 0.3471 0.3182 0.069 Uiso 1 1 calc R . . H48 H 0.1080 0.4842 0.3637 0.069 Uiso 1 1 calc R . . H49 H 0.1614 0.3369 0.3841 0.069 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 0.0201(3) 0.0201(2) 0.0186(2) 0.00055(17) 0.00458(18) 0.00023(19) N1 0.0239(10) 0.0321(9) 0.0324(9) 0.0055(7) 0.0041(7) 0.0034(7) Si2 0.0233(3) 0.0319(3) 0.0344(3) 0.0088(2) 0.0061(2) 0.0053(2) C1 0.0221(10) 0.0230(8) 0.0185(8) 0.0003(7) 0.0050(7) 0.0002(7) C2 0.0283(11) 0.0282(9) 0.0209(8) 0.0022(7) 0.0024(7) 0.0046(8) C3 0.0259(11) 0.0243(9) 0.0252(9) 0.0013(7) 0.0069(8) 0.0068(8) C4 0.0219(10) 0.0222(8) 0.0202(8) -0.0011(7) 0.0052(7) 0.0017(7) C5 0.069(2) 0.0464(15) 0.0614(17) 0.0025(13) 0.0209(15) 0.0236(14) C6 0.0383(15) 0.0665(17) 0.0443(13) 0.0227(12) 0.0052(11) 0.0131(13) C7 0.0298(14) 0.0543(16) 0.084(2) 0.0229(15) -0.0026(13) -0.0024(12) Si3 0.0308(3) 0.0244(3) 0.0211(2) -0.00265(19) 0.0040(2) -0.0025(2) C8 0.0415(14) 0.0279(10) 0.0327(10) -0.0021(8) 0.0096(9) -0.0081(9) C9 0.0455(15) 0.0400(12) 0.0345(11) -0.0031(10) -0.0083(10) -0.0067(11) C10 0.0495(15) 0.0294(10) 0.0350(11) -0.0054(9) 0.0174(10) 0.0013(10) Si4 0.0329(3) 0.0251(3) 0.0226(3) 0.0018(2) 0.0101(2) -0.0016(2) C11 0.0598(17) 0.0444(13) 0.0238(10) 0.0062(9) 0.0107(10) -0.0042(12) C12 0.0321(13) 0.0435(13) 0.0508(13) 0.0048(11) 0.0177(11) -0.0037(10) C13 0.0626(18) 0.0270(10) 0.0406(12) 0.0028(9) 0.0209(11) -0.0068(11) Si5 0.0253(3) 0.0313(3) 0.0227(3) 0.0004(2) 0.0093(2) -0.0001(2) C14 0.0359(13) 0.0402(12) 0.0339(11) 0.0139(9) 0.0082(9) -0.0024(10) C15 0.0244(11) 0.0434(12) 0.0397(11) 0.0049(10) 0.0077(9) -0.0033(10) C16 0.0486(17) 0.0606(16) 0.0419(13) -0.0111(12) 0.0271(12) -0.0050(13) Si6 0.0371(4) 0.0274(3) 0.0263(3) -0.0059(2) 0.0040(2) -0.0050(2) C17 0.0517(17) 0.0557(15) 0.0249(10) -0.0017(10) -0.0049(10) -0.0140(13) C18 0.072(2) 0.0388(14) 0.0663(18) -0.0251(13) 0.0095(15) 0.0010(14) C19 0.0491(16) 0.0449(14) 0.0438(13) -0.0001(11) 0.0036(11) -0.0199(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.5685(18) . ? Si1 C1 1.8554(19) . ? Si1 C4 1.8573(19) . ? N1 Si2 1.6762(19) . ? Si2 C5 1.858(3) . ? Si2 C6 1.868(3) . ? Si2 C7 1.870(3) . ? C1 C2 1.572(3) . ? C1 Si4 1.9088(19) . ? C1 Si3 1.915(2) . ? C2 C3 1.551(3) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 C4 1.569(3) . ? C3 H3 0.9900 . ? C3 H4 0.9900 . ? C4 Si5 1.905(2) . ? C4 Si6 1.912(2) . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C5 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C6 H10 0.9800 . ? C7 H11 0.9800 . ? C7 H12 0.9800 . ? C7 H13 0.9800 . ? Si3 C10 1.866(2) . ? Si3 C9 1.874(2) . ? Si3 C8 1.878(2) . ? C8 H14 0.9800 . ? C8 H15 0.9800 . ? C8 H16 0.9800 . ? C9 H17 0.9800 . ? C9 H18 0.9800 . ? C9 H19 0.9800 . ? C10 H20 0.9800 . ? C10 H21 0.9800 . ? C10 H22 0.9800 . ? Si4 C12 1.861(3) . ? Si4 C13 1.871(2) . ? Si4 C11 1.873(2) . ? C11 H23 0.9800 . ? C11 H24 0.9800 . ? C11 H25 0.9800 . ? C12 H26 0.9800 . ? C12 H27 0.9800 . ? C12 H28 0.9800 . ? C13 H29 0.9800 . ? C13 H30 0.9800 . ? C13 H31 0.9800 . ? Si5 C14 1.870(2) . ? Si5 C16 1.873(2) . ? Si5 C15 1.874(2) . ? C14 H32 0.9800 . ? C14 H33 0.9800 . ? C14 H34 0.9800 . ? C15 H35 0.9800 . ? C15 H36 0.9800 . ? C15 H37 0.9800 . ? C16 H38 0.9800 . ? C16 H39 0.9800 . ? C16 H40 0.9800 . ? Si6 C19 1.866(3) . ? Si6 C17 1.866(3) . ? Si6 C18 1.874(3) . ? C17 H41 0.9800 . ? C17 H42 0.9800 . ? C17 H43 0.9800 . ? C18 H44 0.9800 . ? C18 H45 0.9800 . ? C18 H46 0.9800 . ? C19 H47 0.9800 . ? C19 H48 0.9800 . ? C19 H49 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C1 129.72(9) . . ? N1 Si1 C4 128.69(9) . . ? C1 Si1 C4 101.59(9) . . ? Si1 N1 Si2 177.19(13) . . ? N1 Si2 C5 111.62(13) . . ? N1 Si2 C6 111.76(11) . . ? C5 Si2 C6 106.59(14) . . ? N1 Si2 C7 109.49(11) . . ? C5 Si2 C7 107.99(16) . . ? C6 Si2 C7 109.26(14) . . ? C2 C1 Si1 101.25(11) . . ? C2 C1 Si4 111.32(13) . . ? Si1 C1 Si4 114.15(10) . . ? C2 C1 Si3 110.82(13) . . ? Si1 C1 Si3 108.06(9) . . ? Si4 C1 Si3 110.84(9) . . ? C3 C2 C1 111.20(16) . . ? C3 C2 H1 109.4 . . ? C1 C2 H1 109.4 . . ? C3 C2 H2 109.4 . . ? C1 C2 H2 109.4 . . ? H1 C2 H2 108.0 . . ? C2 C3 C4 110.34(15) . . ? C2 C3 H3 109.6 . . ? C4 C3 H3 109.6 . . ? C2 C3 H4 109.6 . . ? C4 C3 H4 109.6 . . ? H3 C3 H4 108.1 . . ? C3 C4 Si1 101.00(12) . . ? C3 C4 Si5 111.97(13) . . ? Si1 C4 Si5 113.74(10) . . ? C3 C4 Si6 111.39(13) . . ? Si1 C4 Si6 107.34(10) . . ? Si5 C4 Si6 110.96(9) . . ? Si2 C5 H5 109.5 . . ? Si2 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? Si2 C5 H7 109.5 . . ? H5 C5 H7 109.5 . . ? H6 C5 H7 109.5 . . ? Si2 C6 H8 109.5 . . ? Si2 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? Si2 C6 H10 109.5 . . ? H8 C6 H10 109.5 . . ? H9 C6 H10 109.5 . . ? Si2 C7 H11 109.5 . . ? Si2 C7 H12 109.5 . . ? H11 C7 H12 109.5 . . ? Si2 C7 H13 109.5 . . ? H11 C7 H13 109.5 . . ? H12 C7 H13 109.5 . . ? C10 Si3 C9 110.27(12) . . ? C10 Si3 C8 104.61(11) . . ? C9 Si3 C8 107.21(11) . . ? C10 Si3 C1 113.83(10) . . ? C9 Si3 C1 108.67(10) . . ? C8 Si3 C1 112.03(9) . . ? Si3 C8 H14 109.5 . . ? Si3 C8 H15 109.5 . . ? H14 C8 H15 109.5 . . ? Si3 C8 H16 109.5 . . ? H14 C8 H16 109.5 . . ? H15 C8 H16 109.5 . . ? Si3 C9 H17 109.5 . . ? Si3 C9 H18 109.5 . . ? H17 C9 H18 109.5 . . ? Si3 C9 H19 109.5 . . ? H17 C9 H19 109.5 . . ? H18 C9 H19 109.5 . . ? Si3 C10 H20 109.5 . . ? Si3 C10 H21 109.5 . . ? H20 C10 H21 109.5 . . ? Si3 C10 H22 109.5 . . ? H20 C10 H22 109.5 . . ? H21 C10 H22 109.5 . . ? C12 Si4 C13 108.65(13) . . ? C12 Si4 C11 109.92(12) . . ? C13 Si4 C11 104.00(11) . . ? C12 Si4 C1 111.20(10) . . ? C13 Si4 C1 111.30(10) . . ? C11 Si4 C1 111.51(10) . . ? Si4 C11 H23 109.5 . . ? Si4 C11 H24 109.5 . . ? H23 C11 H24 109.5 . . ? Si4 C11 H25 109.5 . . ? H23 C11 H25 109.5 . . ? H24 C11 H25 109.5 . . ? Si4 C12 H26 109.5 . . ? Si4 C12 H27 109.5 . . ? H26 C12 H27 109.5 . . ? Si4 C12 H28 109.5 . . ? H26 C12 H28 109.5 . . ? H27 C12 H28 109.5 . . ? Si4 C13 H29 109.5 . . ? Si4 C13 H30 109.5 . . ? H29 C13 H30 109.5 . . ? Si4 C13 H31 109.5 . . ? H29 C13 H31 109.5 . . ? H30 C13 H31 109.5 . . ? C14 Si5 C16 110.57(12) . . ? C14 Si5 C15 108.35(11) . . ? C16 Si5 C15 102.11(12) . . ? C14 Si5 C4 111.34(10) . . ? C16 Si5 C4 111.67(11) . . ? C15 Si5 C4 112.41(9) . . ? Si5 C14 H32 109.5 . . ? Si5 C14 H33 109.5 . . ? H32 C14 H33 109.5 . . ? Si5 C14 H34 109.5 . . ? H32 C14 H34 109.5 . . ? H33 C14 H34 109.5 . . ? Si5 C15 H35 109.5 . . ? Si5 C15 H36 109.5 . . ? H35 C15 H36 109.5 . . ? Si5 C15 H37 109.5 . . ? H35 C15 H37 109.5 . . ? H36 C15 H37 109.5 . . ? Si5 C16 H38 109.5 . . ? Si5 C16 H39 109.5 . . ? H38 C16 H39 109.5 . . ? Si5 C16 H40 109.5 . . ? H38 C16 H40 109.5 . . ? H39 C16 H40 109.5 . . ? C19 Si6 C17 106.43(13) . . ? C19 Si6 C18 106.21(14) . . ? C17 Si6 C18 111.31(14) . . ? C19 Si6 C4 111.46(10) . . ? C17 Si6 C4 110.95(10) . . ? C18 Si6 C4 110.33(12) . . ? Si6 C17 H41 109.5 . . ? Si6 C17 H42 109.5 . . ? H41 C17 H42 109.5 . . ? Si6 C17 H43 109.5 . . ? H41 C17 H43 109.5 . . ? H42 C17 H43 109.5 . . ? Si6 C18 H44 109.5 . . ? Si6 C18 H45 109.5 . . ? H44 C18 H45 109.5 . . ? Si6 C18 H46 109.5 . . ? H44 C18 H46 109.5 . . ? H45 C18 H46 109.5 . . ? Si6 C19 H47 109.5 . . ? Si6 C19 H48 109.5 . . ? H47 C19 H48 109.5 . . ? Si6 C19 H49 109.5 . . ? H47 C19 H49 109.5 . . ? H48 C19 H49 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 C1 Si1 N1 Si2 -85(3) . . . . ? C4 Si1 N1 Si2 94(3) . . . . ? Si1 N1 Si2 C5 113(3) . . . . ? Si1 N1 Si2 C6 -128(3) . . . . ? Si1 N1 Si2 C7 -6(3) . . . . ? N1 Si1 C1 C2 -172.61(13) . . . . ? C4 Si1 C1 C2 7.94(14) . . . . ? N1 Si1 C1 Si4 67.69(15) . . . . ? C4 Si1 C1 Si4 -111.76(11) . . . . ? N1 Si1 C1 Si3 -56.12(15) . . . . ? C4 Si1 C1 Si3 124.43(10) . . . . ? Si1 C1 C2 C3 -28.99(17) . . . . ? Si4 C1 C2 C3 92.72(16) . . . . ? Si3 C1 C2 C3 -143.43(13) . . . . ? C1 C2 C3 C4 43.3(2) . . . . ? C2 C3 C4 Si1 -32.93(18) . . . . ? C2 C3 C4 Si5 88.44(17) . . . . ? C2 C3 C4 Si6 -146.65(14) . . . . ? N1 Si1 C4 C3 -165.52(13) . . . . ? C1 Si1 C4 C3 13.93(14) . . . . ? N1 Si1 C4 Si5 74.36(15) . . . . ? C1 Si1 C4 Si5 -106.19(10) . . . . ? N1 Si1 C4 Si6 -48.78(15) . . . . ? C1 Si1 C4 Si6 130.67(9) . . . . ? C2 C1 Si3 C10 -162.86(13) . . . . ? Si1 C1 Si3 C10 87.04(12) . . . . ? Si4 C1 Si3 C10 -38.74(13) . . . . ? C2 C1 Si3 C9 -39.57(15) . . . . ? Si1 C1 Si3 C9 -149.67(11) . . . . ? Si4 C1 Si3 C9 84.55(13) . . . . ? C2 C1 Si3 C8 78.70(15) . . . . ? Si1 C1 Si3 C8 -31.40(14) . . . . ? Si4 C1 Si3 C8 -157.18(11) . . . . ? C2 C1 Si4 C12 -158.15(14) . . . . ? Si1 C1 Si4 C12 -44.29(14) . . . . ? Si3 C1 Si4 C12 78.01(13) . . . . ? C2 C1 Si4 C13 -36.86(17) . . . . ? Si1 C1 Si4 C13 77.00(14) . . . . ? Si3 C1 Si4 C13 -160.70(12) . . . . ? C2 C1 Si4 C11 78.78(15) . . . . ? Si1 C1 Si4 C11 -167.36(11) . . . . ? Si3 C1 Si4 C11 -45.06(14) . . . . ? C3 C4 Si5 C14 -150.66(13) . . . . ? Si1 C4 Si5 C14 -36.95(14) . . . . ? Si6 C4 Si5 C14 84.20(12) . . . . ? C3 C4 Si5 C16 85.21(16) . . . . ? Si1 C4 Si5 C16 -161.08(12) . . . . ? Si6 C4 Si5 C16 -39.94(15) . . . . ? C3 C4 Si5 C15 -28.87(16) . . . . ? Si1 C4 Si5 C15 84.84(13) . . . . ? Si6 C4 Si5 C15 -154.02(11) . . . . ? C3 C4 Si6 C19 70.98(16) . . . . ? Si1 C4 Si6 C19 -38.71(14) . . . . ? Si5 C4 Si6 C19 -163.55(12) . . . . ? C3 C4 Si6 C17 -170.61(14) . . . . ? Si1 C4 Si6 C17 79.70(13) . . . . ? Si5 C4 Si6 C17 -45.13(14) . . . . ? C3 C4 Si6 C18 -46.77(18) . . . . ? Si1 C4 Si6 C18 -156.46(13) . . . . ? Si5 C4 Si6 C18 78.70(15) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.440 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.064 #===END