# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chunming Cui' _publ_contact_author_email cmcui@nankai.edu.cn _publ_author_name 'Chunming Cui' # Attachment '- shelx.cif' data_shelx _database_code_depnum_ccdc_archive 'CCDC 830375' #TrackingRef '- shelx.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H46 Cl N3 Si2' _chemical_formula_sum 'C26 H46 Cl N3 Si2' _chemical_formula_weight 492.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 10.3126(17) _cell_length_b 17.824(3) _cell_length_c 15.921(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.561(2) _cell_angle_gamma 90.00 _cell_volume 2856.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8581 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.1 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Multilayer _diffrn_measurement_device_type 'Rigaku Saturn 724CCD camera' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24810 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.21 _reflns_number_total 6282 _reflns_number_gt 4762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r2' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6282 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.36894(5) 0.00614(3) 0.80239(3) 0.01977(13) Uani 1 1 d . . . Si2 Si 0.18167(5) 0.03814(3) 0.63904(3) 0.02100(13) Uani 1 1 d . . . Cl1 Cl 0.29544(5) 0.03493(3) 0.92000(3) 0.02752(13) Uani 1 1 d . . . N1 N 0.30196(14) 0.07578(8) 0.72429(9) 0.0178(3) Uani 1 1 d . . . N2 N 0.65987(14) -0.00418(9) 0.83954(9) 0.0216(3) Uani 1 1 d . . . N3 N 0.61265(14) 0.10286(9) 0.88960(9) 0.0216(3) Uani 1 1 d . . . C1 C 0.33281(17) 0.15414(10) 0.71703(10) 0.0197(4) Uani 1 1 d . . . C2 C 0.25864(18) 0.21063(11) 0.74882(11) 0.0228(4) Uani 1 1 d . . . C3 C 0.28166(19) 0.28557(11) 0.73242(12) 0.0273(4) Uani 1 1 d . . . H3 H 0.2321 0.3234 0.7535 0.033 Uiso 1 1 calc R . . C4 C 0.3751(2) 0.30638(11) 0.68616(12) 0.0302(5) Uani 1 1 d . . . H4 H 0.3884 0.3578 0.6749 0.036 Uiso 1 1 calc R . . C5 C 0.44862(19) 0.25164(11) 0.65655(12) 0.0271(4) Uani 1 1 d . . . H5 H 0.5136 0.2660 0.6255 0.032 Uiso 1 1 calc R . . C6 C 0.42978(17) 0.17575(10) 0.67109(11) 0.0217(4) Uani 1 1 d . . . C7 C 0.15203(18) 0.19142(11) 0.79812(12) 0.0267(4) Uani 1 1 d . . . H7 H 0.1510 0.1357 0.8057 0.032 Uiso 1 1 calc R . . C8 C 0.1803(2) 0.22829(12) 0.88817(13) 0.0349(5) Uani 1 1 d . . . H8A H 0.2684 0.2130 0.9204 0.052 Uiso 1 1 calc R . . H8B H 0.1129 0.2122 0.9193 0.052 Uiso 1 1 calc R . . H8C H 0.1774 0.2830 0.8819 0.052 Uiso 1 1 calc R . . C9 C 0.0145(2) 0.21605(14) 0.74865(15) 0.0424(6) Uani 1 1 d . . . H9A H 0.0124 0.2708 0.7428 0.064 Uiso 1 1 calc R . . H9B H -0.0527 0.2001 0.7801 0.064 Uiso 1 1 calc R . . H9C H -0.0045 0.1930 0.6914 0.064 Uiso 1 1 calc R . . C10 C 0.51243(18) 0.11882(11) 0.63390(12) 0.0258(4) Uani 1 1 d . . . H10 H 0.4901 0.0676 0.6522 0.031 Uiso 1 1 calc R . . C11 C 0.66146(19) 0.13132(12) 0.66691(14) 0.0349(5) Uani 1 1 d . . . H11A H 0.6864 0.1801 0.6469 0.052 Uiso 1 1 calc R . . H11B H 0.7108 0.0915 0.6450 0.052 Uiso 1 1 calc R . . H11C H 0.6827 0.1303 0.7300 0.052 Uiso 1 1 calc R . . C12 C 0.4793(2) 0.12119(13) 0.53486(12) 0.0378(5) Uani 1 1 d . . . H12A H 0.3835 0.1141 0.5136 0.057 Uiso 1 1 calc R . . H12B H 0.5275 0.0811 0.5126 0.057 Uiso 1 1 calc R . . H12C H 0.5058 0.1699 0.5154 0.057 Uiso 1 1 calc R . . C13 C 0.1162(2) 0.11393(11) 0.55957(12) 0.0298(5) Uani 1 1 d . . . H13A H 0.0629 0.1492 0.5852 0.045 Uiso 1 1 calc R . . H13B H 0.0608 0.0916 0.5078 0.045 Uiso 1 1 calc R . . H13C H 0.1907 0.1407 0.5442 0.045 Uiso 1 1 calc R . . C14 C 0.03752(19) -0.00131(11) 0.67771(12) 0.0308(5) Uani 1 1 d . . . H14A H 0.0682 -0.0418 0.7189 0.046 Uiso 1 1 calc R . . H14B H -0.0279 -0.0212 0.6287 0.046 Uiso 1 1 calc R . . H14C H -0.0035 0.0383 0.7058 0.046 Uiso 1 1 calc R . . C15 C 0.2520(2) -0.03756(12) 0.58115(13) 0.0345(5) Uani 1 1 d . . . H15A H 0.3258 -0.0174 0.5584 0.052 Uiso 1 1 calc R . . H15B H 0.1828 -0.0564 0.5336 0.052 Uiso 1 1 calc R . . H15C H 0.2843 -0.0787 0.6211 0.052 Uiso 1 1 calc R . . C16 C 0.91524(18) -0.00175(13) 0.87893(13) 0.0351(5) Uani 1 1 d . . . H16A H 0.9813 0.0386 0.8877 0.053 Uiso 1 1 calc R . . H16B H 0.9158 -0.0276 0.8247 0.053 Uiso 1 1 calc R . . H16C H 0.9370 -0.0376 0.9266 0.053 Uiso 1 1 calc R . . C17 C 0.78007(18) 0.03072(11) 0.87557(11) 0.0252(4) Uani 1 1 d . . . C18 C 0.75033(18) 0.09703(11) 0.90758(11) 0.0248(4) Uani 1 1 d . . . C19 C 0.8450(2) 0.15460(13) 0.95358(13) 0.0370(5) Uani 1 1 d . . . H19A H 0.9348 0.1334 0.9679 0.056 Uiso 1 1 calc R . . H19B H 0.8183 0.1696 1.0065 0.056 Uiso 1 1 calc R . . H19C H 0.8441 0.1985 0.9164 0.056 Uiso 1 1 calc R . . C20 C 0.55576(17) 0.04105(10) 0.84709(11) 0.0209(4) Uani 1 1 d . . . C21 C 0.64388(19) -0.08061(11) 0.80204(12) 0.0265(4) Uani 1 1 d . . . H21 H 0.5483 -0.0945 0.7960 0.032 Uiso 1 1 calc R . . C22 C 0.7248(2) -0.13811(12) 0.86251(13) 0.0346(5) Uani 1 1 d . . . H22A H 0.8181 -0.1353 0.8583 0.052 Uiso 1 1 calc R . . H22B H 0.6904 -0.1885 0.8463 0.052 Uiso 1 1 calc R . . H22C H 0.7180 -0.1274 0.9218 0.052 Uiso 1 1 calc R . . C23 C 0.6715(2) -0.08231(12) 0.71154(13) 0.0370(5) Uani 1 1 d . . . H23A H 0.6116 -0.0473 0.6744 0.056 Uiso 1 1 calc R . . H23B H 0.6568 -0.1332 0.6880 0.056 Uiso 1 1 calc R . . H23C H 0.7638 -0.0675 0.7141 0.056 Uiso 1 1 calc R . . C24 C 0.53515(19) 0.16457(10) 0.91834(11) 0.0240(4) Uani 1 1 d . . . H24 H 0.4396 0.1556 0.8908 0.029 Uiso 1 1 calc R . . C25 C 0.5469(2) 0.16092(12) 1.01574(11) 0.0314(5) Uani 1 1 d . . . H25A H 0.5236 0.1104 1.0318 0.047 Uiso 1 1 calc R . . H25B H 0.4862 0.1975 1.0325 0.047 Uiso 1 1 calc R . . H25C H 0.6383 0.1725 1.0453 0.047 Uiso 1 1 calc R . . C26 C 0.5711(2) 0.24149(11) 0.88847(13) 0.0336(5) Uani 1 1 d . . . H26A H 0.6578 0.2569 0.9227 0.050 Uiso 1 1 calc R . . H26B H 0.5035 0.2781 0.8959 0.050 Uiso 1 1 calc R . . H26C H 0.5750 0.2390 0.8276 0.050 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 0.0192(3) 0.0178(3) 0.0211(2) 0.0014(2) 0.0019(2) -0.0004(2) Si2 0.0217(3) 0.0203(3) 0.0195(2) -0.0013(2) 0.0013(2) -0.0024(2) Cl1 0.0275(3) 0.0321(3) 0.0240(2) 0.0044(2) 0.0079(2) 0.0026(2) N1 0.0191(7) 0.0154(8) 0.0184(7) -0.0001(6) 0.0032(6) -0.0009(6) N2 0.0202(8) 0.0247(9) 0.0195(7) 0.0015(6) 0.0033(6) 0.0023(7) N3 0.0230(8) 0.0228(9) 0.0183(7) 0.0004(6) 0.0034(7) -0.0028(7) C1 0.0225(9) 0.0177(10) 0.0162(8) 0.0015(7) -0.0020(7) -0.0010(7) C2 0.0242(10) 0.0215(10) 0.0202(9) -0.0008(7) -0.0008(8) 0.0018(8) C3 0.0375(12) 0.0179(10) 0.0235(10) -0.0022(8) 0.0003(9) 0.0036(8) C4 0.0437(12) 0.0183(10) 0.0243(10) 0.0020(8) -0.0018(9) -0.0065(9) C5 0.0324(11) 0.0273(11) 0.0199(9) 0.0019(8) 0.0023(8) -0.0072(9) C6 0.0220(10) 0.0230(10) 0.0180(8) 0.0000(7) -0.0004(8) -0.0025(8) C7 0.0260(10) 0.0214(11) 0.0325(10) -0.0010(8) 0.0063(9) 0.0034(8) C8 0.0377(12) 0.0349(13) 0.0347(11) -0.0033(10) 0.0132(10) 0.0023(10) C9 0.0345(12) 0.0483(15) 0.0432(13) -0.0028(11) 0.0054(11) 0.0112(11) C10 0.0262(10) 0.0265(11) 0.0261(10) 0.0007(8) 0.0085(8) -0.0041(8) C11 0.0273(11) 0.0401(13) 0.0383(11) 0.0056(10) 0.0089(10) -0.0019(9) C12 0.0393(13) 0.0480(15) 0.0278(11) -0.0061(10) 0.0107(10) 0.0021(10) C13 0.0303(11) 0.0335(12) 0.0218(9) 0.0020(8) -0.0025(8) -0.0013(9) C14 0.0288(11) 0.0321(12) 0.0298(11) 0.0015(9) 0.0028(9) -0.0062(9) C15 0.0412(12) 0.0302(12) 0.0304(11) -0.0101(9) 0.0040(10) -0.0002(10) C16 0.0207(10) 0.0537(15) 0.0300(11) -0.0036(10) 0.0039(9) 0.0008(9) C17 0.0180(9) 0.0378(12) 0.0179(9) 0.0025(8) 0.0000(8) -0.0015(8) C18 0.0217(10) 0.0336(12) 0.0178(9) 0.0017(8) 0.0010(8) -0.0048(8) C19 0.0273(11) 0.0489(15) 0.0331(11) -0.0090(10) 0.0027(9) -0.0127(10) C20 0.0224(9) 0.0219(10) 0.0184(8) 0.0023(7) 0.0047(8) 0.0001(8) C21 0.0244(10) 0.0239(11) 0.0306(10) -0.0023(8) 0.0048(9) 0.0020(8) C22 0.0316(12) 0.0311(12) 0.0420(12) 0.0019(10) 0.0097(10) 0.0078(9) C23 0.0439(13) 0.0356(13) 0.0308(11) -0.0068(9) 0.0066(10) 0.0048(10) C24 0.0271(10) 0.0223(10) 0.0205(9) -0.0019(8) 0.0009(8) -0.0002(8) C25 0.0350(12) 0.0353(12) 0.0227(10) -0.0045(9) 0.0037(9) 0.0017(9) C26 0.0429(13) 0.0268(12) 0.0264(10) -0.0040(8) -0.0027(9) -0.0051(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 N1 1.7861(15) . ? Si1 C20 2.0023(19) . ? Si1 Cl1 2.2274(7) . ? Si2 N1 1.7603(15) . ? Si2 C14 1.8658(19) . ? Si2 C15 1.8673(19) . ? Si2 C13 1.8736(19) . ? N1 C1 1.443(2) . ? N2 C20 1.369(2) . ? N2 C17 1.394(2) . ? N2 C21 1.482(2) . ? N3 C20 1.358(2) . ? N3 C18 1.390(2) . ? N3 C24 1.489(2) . ? C1 C6 1.415(2) . ? C1 C2 1.422(2) . ? C2 C3 1.391(3) . ? C2 C7 1.522(3) . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? C6 C10 1.525(2) . ? C7 C9 1.530(3) . ? C7 C8 1.546(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.529(3) . ? C10 C12 1.540(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.500(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.349(3) . ? C18 C19 1.494(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C22 1.525(3) . ? C21 C23 1.529(3) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.523(3) . ? C24 C25 1.530(2) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 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 C20 103.18(7) . . ? N1 Si1 Cl1 105.92(5) . . ? C20 Si1 Cl1 96.12(5) . . ? N1 Si2 C14 111.57(8) . . ? N1 Si2 C15 111.82(8) . . ? C14 Si2 C15 108.27(10) . . ? N1 Si2 C13 109.63(8) . . ? C14 Si2 C13 107.38(9) . . ? C15 Si2 C13 108.01(9) . . ? C1 N1 Si2 115.96(11) . . ? C1 N1 Si1 132.06(12) . . ? Si2 N1 Si1 111.89(8) . . ? C20 N2 C17 110.21(16) . . ? C20 N2 C21 123.79(15) . . ? C17 N2 C21 125.94(15) . . ? C20 N3 C18 110.70(15) . . ? C20 N3 C24 123.36(15) . . ? C18 N3 C24 125.76(15) . . ? C6 C1 C2 119.11(16) . . ? C6 C1 N1 119.87(15) . . ? C2 C1 N1 120.78(15) . . ? C3 C2 C1 119.07(16) . . ? C3 C2 C7 118.98(16) . . ? C1 C2 C7 121.92(16) . . ? C4 C3 C2 121.59(17) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.34(18) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.52(17) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 119.34(17) . . ? C5 C6 C10 118.14(16) . . ? C1 C6 C10 122.49(16) . . ? C2 C7 C9 111.28(17) . . ? C2 C7 C8 111.77(16) . . ? C9 C7 C8 108.78(16) . . ? C2 C7 H7 108.3 . . ? C9 C7 H7 108.3 . . ? C8 C7 H7 108.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C11 111.99(16) . . ? C6 C10 C12 111.17(16) . . ? C11 C10 C12 109.32(15) . . ? C6 C10 H10 108.1 . . ? C11 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N2 106.95(16) . . ? C18 C17 C16 127.65(18) . . ? N2 C17 C16 125.38(18) . . ? C17 C18 N3 107.08(16) . . ? C17 C18 C19 127.52(18) . . ? N3 C18 C19 125.40(18) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 N2 105.04(15) . . ? N3 C20 Si1 135.03(13) . . ? N2 C20 Si1 119.88(13) . . ? N2 C21 C22 111.46(16) . . ? N2 C21 C23 111.75(16) . . ? C22 C21 C23 113.16(16) . . ? N2 C21 H21 106.7 . . ? C22 C21 H21 106.7 . . ? C23 C21 H21 106.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N3 C24 C26 112.69(15) . . ? N3 C24 C25 110.52(15) . . ? C26 C24 C25 112.57(16) . . ? N3 C24 H24 106.9 . . ? C26 C24 H24 106.9 . . ? C25 C24 H24 106.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 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 C14 Si2 N1 C1 -121.41(13) . . . . ? C15 Si2 N1 C1 117.17(13) . . . . ? C13 Si2 N1 C1 -2.59(14) . . . . ? C14 Si2 N1 Si1 61.37(10) . . . . ? C15 Si2 N1 Si1 -60.05(11) . . . . ? C13 Si2 N1 Si1 -179.81(8) . . . . ? C20 Si1 N1 C1 -28.20(16) . . . . ? Cl1 Si1 N1 C1 72.21(15) . . . . ? C20 Si1 N1 Si2 148.43(8) . . . . ? Cl1 Si1 N1 Si2 -111.16(7) . . . . ? Si2 N1 C1 C6 -86.03(17) . . . . ? Si1 N1 C1 C6 90.50(19) . . . . ? Si2 N1 C1 C2 88.28(17) . . . . ? Si1 N1 C1 C2 -95.20(19) . . . . ? C6 C1 C2 C3 1.2(3) . . . . ? N1 C1 C2 C3 -173.10(16) . . . . ? C6 C1 C2 C7 179.49(16) . . . . ? N1 C1 C2 C7 5.1(3) . . . . ? C1 C2 C3 C4 -0.2(3) . . . . ? C7 C2 C3 C4 -178.45(17) . . . . ? C2 C3 C4 C5 -0.9(3) . . . . ? C3 C4 C5 C6 0.9(3) . . . . ? C4 C5 C6 C1 0.2(3) . . . . ? C4 C5 C6 C10 178.25(17) . . . . ? C2 C1 C6 C5 -1.3(3) . . . . ? N1 C1 C6 C5 173.13(16) . . . . ? C2 C1 C6 C10 -179.23(16) . . . . ? N1 C1 C6 C10 -4.8(3) . . . . ? C3 C2 C7 C9 62.9(2) . . . . ? C1 C2 C7 C9 -115.3(2) . . . . ? C3 C2 C7 C8 -58.9(2) . . . . ? C1 C2 C7 C8 122.82(19) . . . . ? C5 C6 C10 C11 58.5(2) . . . . ? C1 C6 C10 C11 -123.51(18) . . . . ? C5 C6 C10 C12 -64.1(2) . . . . ? C1 C6 C10 C12 113.89(19) . . . . ? C20 N2 C17 C18 1.6(2) . . . . ? C21 N2 C17 C18 -175.55(16) . . . . ? C20 N2 C17 C16 -179.78(17) . . . . ? C21 N2 C17 C16 3.1(3) . . . . ? N2 C17 C18 N3 -1.1(2) . . . . ? C16 C17 C18 N3 -179.68(17) . . . . ? N2 C17 C18 C19 179.18(17) . . . . ? C16 C17 C18 C19 0.6(3) . . . . ? C20 N3 C18 C17 0.2(2) . . . . ? C24 N3 C18 C17 175.51(16) . . . . ? C20 N3 C18 C19 180.00(17) . . . . ? C24 N3 C18 C19 -4.7(3) . . . . ? C18 N3 C20 N2 0.71(18) . . . . ? C24 N3 C20 N2 -174.70(15) . . . . ? C18 N3 C20 Si1 178.21(14) . . . . ? C24 N3 C20 Si1 2.8(3) . . . . ? C17 N2 C20 N3 -1.38(19) . . . . ? C21 N2 C20 N3 175.81(15) . . . . ? C17 N2 C20 Si1 -179.35(11) . . . . ? C21 N2 C20 Si1 -2.2(2) . . . . ? N1 Si1 C20 N3 62.43(18) . . . . ? Cl1 Si1 C20 N3 -45.54(18) . . . . ? N1 Si1 C20 N2 -120.35(14) . . . . ? Cl1 Si1 C20 N2 131.68(13) . . . . ? C20 N2 C21 C22 -127.34(18) . . . . ? C17 N2 C21 C22 49.4(2) . . . . ? C20 N2 C21 C23 104.93(19) . . . . ? C17 N2 C21 C23 -78.3(2) . . . . ? C20 N3 C24 C26 -127.65(18) . . . . ? C18 N3 C24 C26 57.6(2) . . . . ? C20 N3 C24 C25 105.43(19) . . . . ? C18 N3 C24 C25 -69.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.21 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.403 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.059 data_r100712c1 _database_code_depnum_ccdc_archive 'CCDC 830376' #TrackingRef '- r100712c1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H47 Cl N3 Si2' _chemical_formula_weight 493.30 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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' '-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 10.129(2) _cell_length_b 17.177(3) _cell_length_c 34.277(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5964(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 0.226 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 35933 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5244 _reflns_number_gt 4625 _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^)+(0.0550P)^2^+4.7364P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0074(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5244 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1363 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.82478(6) 0.20262(4) 0.178288(18) 0.0340(2) Uani 1 1 d . . . Si1 Si 0.68152(6) 0.11759(4) 0.169030(17) 0.02166(19) Uani 1 1 d . . . Si2 Si 0.83088(7) -0.03523(5) 0.173050(19) 0.0280(2) Uani 1 1 d . . . N1 N 0.74626(18) 0.03738(12) 0.14631(5) 0.0208(4) Uani 1 1 d . . . N2 N 0.42451(19) 0.19806(13) 0.15072(5) 0.0263(5) Uani 1 1 d . . . N3 N 0.45203(18) 0.22283(12) 0.09022(5) 0.0217(4) Uani 1 1 d . . . C1 C 0.5486(2) 0.16530(14) 0.14075(6) 0.0216(5) Uani 1 1 d . . . C2 C 0.5618(2) 0.18209(14) 0.10227(6) 0.0218(5) Uani 1 1 d . . . H2 H 0.6331 0.1684 0.0866 0.026 Uiso 1 1 calc R . . C3 C 0.3634(2) 0.23298(16) 0.11976(7) 0.0273(6) Uani 1 1 d . . . C4 C 0.3647(3) 0.19629(19) 0.19049(7) 0.0380(7) Uani 1 1 d . . . C5 C 0.3405(3) 0.1117(2) 0.20200(9) 0.0484(9) Uani 1 1 d . . . H5A H 0.2836 0.0876 0.1831 0.073 Uiso 1 1 calc R . . H5B H 0.2994 0.1099 0.2272 0.073 Uiso 1 1 calc R . . H5C H 0.4231 0.0844 0.2029 0.073 Uiso 1 1 calc R . . C6 C 0.4565(3) 0.2384(2) 0.21904(7) 0.0447(8) Uani 1 1 d . . . H6A H 0.5412 0.2133 0.2192 0.067 Uiso 1 1 calc R . . H6B H 0.4192 0.2367 0.2448 0.067 Uiso 1 1 calc R . . H6C H 0.4668 0.2916 0.2110 0.067 Uiso 1 1 calc R . . C7 C 0.2322(3) 0.2398(3) 0.18952(9) 0.0676(12) Uani 1 1 d . . . H7A H 0.2463 0.2922 0.1807 0.101 Uiso 1 1 calc R . . H7B H 0.1947 0.2407 0.2152 0.101 Uiso 1 1 calc R . . H7C H 0.1729 0.2138 0.1720 0.101 Uiso 1 1 calc R . . C8 C 0.4328(2) 0.24991(16) 0.04935(6) 0.0252(5) Uani 1 1 d . . . C9 C 0.5549(3) 0.2952(2) 0.03685(7) 0.0421(8) Uani 1 1 d . . . H9A H 0.5690 0.3378 0.0545 0.063 Uiso 1 1 calc R . . H9B H 0.5424 0.3150 0.0109 0.063 Uiso 1 1 calc R . . H9C H 0.6304 0.2614 0.0373 0.063 Uiso 1 1 calc R . . C10 C 0.4118(3) 0.17853(18) 0.02368(8) 0.0457(8) Uani 1 1 d . . . H10A H 0.4863 0.1443 0.0261 0.068 Uiso 1 1 calc R . . H10B H 0.4024 0.1945 -0.0030 0.068 Uiso 1 1 calc R . . H10C H 0.3333 0.1518 0.0318 0.068 Uiso 1 1 calc R . . C11 C 0.3131(3) 0.30264(19) 0.04744(8) 0.0415(7) Uani 1 1 d . . . H11A H 0.2361 0.2741 0.0554 0.062 Uiso 1 1 calc R . . H11B H 0.3016 0.3209 0.0212 0.062 Uiso 1 1 calc R . . H11C H 0.3258 0.3463 0.0645 0.062 Uiso 1 1 calc R . . C12 C 0.7201(3) -0.07953(19) 0.21015(9) 0.0486(8) Uani 1 1 d . . . H12A H 0.6934 -0.0405 0.2285 0.073 Uiso 1 1 calc R . . H12B H 0.7662 -0.1204 0.2236 0.073 Uiso 1 1 calc R . . H12C H 0.6435 -0.1007 0.1975 0.073 Uiso 1 1 calc R . . C13 C 0.9743(3) 0.0085(2) 0.19903(9) 0.0485(8) Uani 1 1 d . . . H13A H 1.0369 0.0277 0.1803 0.073 Uiso 1 1 calc R . . H13B H 1.0156 -0.0303 0.2151 0.073 Uiso 1 1 calc R . . H13C H 0.9445 0.0507 0.2151 0.073 Uiso 1 1 calc R . . C14 C 0.8888(3) -0.11039(18) 0.13828(8) 0.0410(7) Uani 1 1 d . . . H14A H 0.8153 -0.1295 0.1234 0.061 Uiso 1 1 calc R . . H14B H 0.9283 -0.1526 0.1524 0.061 Uiso 1 1 calc R . . H14C H 0.9529 -0.0880 0.1209 0.061 Uiso 1 1 calc R . . C15 C 0.7301(2) 0.02589(14) 0.10442(6) 0.0212(5) Uani 1 1 d . . . C16 C 0.6164(2) -0.01243(15) 0.09051(7) 0.0266(5) Uani 1 1 d . . . C17 C 0.6045(3) -0.02393(17) 0.05023(7) 0.0350(6) Uani 1 1 d . . . H17 H 0.5305 -0.0496 0.0406 0.042 Uiso 1 1 calc R . . C18 C 0.6991(3) 0.00161(17) 0.02466(7) 0.0383(7) Uani 1 1 d . . . H18 H 0.6889 -0.0065 -0.0020 0.046 Uiso 1 1 calc R . . C19 C 0.8092(3) 0.03931(17) 0.03861(7) 0.0321(6) Uani 1 1 d . . . H19 H 0.8727 0.0568 0.0211 0.039 Uiso 1 1 calc R . . C20 C 0.8278(2) 0.05192(15) 0.07855(7) 0.0244(6) Uani 1 1 d . . . C21 C 0.9509(2) 0.09443(16) 0.09173(7) 0.0301(6) Uani 1 1 d . . . H21 H 0.9548 0.0913 0.1202 0.036 Uiso 1 1 calc R . . C22 C 0.9462(3) 0.18048(17) 0.08058(8) 0.0382(7) Uani 1 1 d . . . H22A H 0.9392 0.1852 0.0528 0.057 Uiso 1 1 calc R . . H22B H 1.0254 0.2057 0.0893 0.057 Uiso 1 1 calc R . . H22C H 0.8711 0.2045 0.0927 0.057 Uiso 1 1 calc R . . C23 C 1.0772(3) 0.0579(2) 0.07562(11) 0.0539(9) Uani 1 1 d . . . H23A H 1.0818 0.0043 0.0834 0.081 Uiso 1 1 calc R . . H23B H 1.1524 0.0854 0.0856 0.081 Uiso 1 1 calc R . . H23C H 1.0767 0.0611 0.0477 0.081 Uiso 1 1 calc R . . C24 C 0.5086(2) -0.04231(17) 0.11721(8) 0.0348(6) Uani 1 1 d . . . H24 H 0.5297 -0.0262 0.1439 0.042 Uiso 1 1 calc R . . C25 C 0.3732(3) -0.00807(19) 0.10641(9) 0.0433(7) Uani 1 1 d . . . H25A H 0.3788 0.0477 0.1060 0.065 Uiso 1 1 calc R . . H25B H 0.3089 -0.0240 0.1254 0.065 Uiso 1 1 calc R . . H25C H 0.3475 -0.0266 0.0811 0.065 Uiso 1 1 calc R . . C26 C 0.5021(3) -0.13114(19) 0.11619(11) 0.0516(8) Uani 1 1 d . . . H26A H 0.4833 -0.1481 0.0901 0.077 Uiso 1 1 calc R . . H26B H 0.4337 -0.1488 0.1334 0.077 Uiso 1 1 calc R . . H26C H 0.5853 -0.1523 0.1244 0.077 Uiso 1 1 calc R . . H1 H 0.651(2) 0.0979(15) 0.2075(7) 0.024(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0368(4) 0.0330(4) 0.0323(3) -0.0079(3) -0.0088(3) -0.0040(3) Si1 0.0248(4) 0.0254(4) 0.0148(3) 0.0005(3) -0.0016(2) 0.0025(3) Si2 0.0341(4) 0.0294(4) 0.0206(3) 0.0039(3) -0.0020(3) 0.0091(3) N1 0.0226(9) 0.0235(11) 0.0162(9) 0.0008(8) -0.0019(7) 0.0009(8) N2 0.0246(10) 0.0368(13) 0.0174(9) 0.0045(9) 0.0035(8) 0.0056(9) N3 0.0224(9) 0.0259(12) 0.0169(9) 0.0025(8) -0.0015(7) 0.0024(8) C1 0.0231(11) 0.0222(13) 0.0195(11) 0.0016(10) 0.0008(9) 0.0026(10) C2 0.0206(11) 0.0255(14) 0.0193(11) -0.0005(10) 0.0012(9) 0.0017(10) C3 0.0279(12) 0.0317(15) 0.0222(11) 0.0048(11) 0.0031(10) 0.0031(11) C4 0.0353(14) 0.057(2) 0.0217(12) 0.0106(13) 0.0123(11) 0.0126(14) C5 0.0409(16) 0.069(2) 0.0355(15) 0.0200(16) 0.0111(12) -0.0037(15) C6 0.0632(19) 0.050(2) 0.0208(12) -0.0017(13) 0.0128(13) 0.0134(16) C7 0.0500(19) 0.116(4) 0.0368(16) 0.022(2) 0.0228(15) 0.041(2) C8 0.0281(12) 0.0319(15) 0.0157(10) 0.0033(10) -0.0030(9) 0.0018(11) C9 0.0411(15) 0.061(2) 0.0240(13) 0.0157(14) -0.0030(11) -0.0100(15) C10 0.076(2) 0.0356(18) 0.0257(13) -0.0031(12) -0.0167(14) 0.0059(16) C11 0.0467(17) 0.047(2) 0.0305(14) 0.0139(13) -0.0003(12) 0.0173(14) C12 0.064(2) 0.0430(19) 0.0385(16) 0.0182(14) 0.0112(15) 0.0148(16) C13 0.0492(18) 0.056(2) 0.0404(16) -0.0020(15) -0.0207(14) 0.0143(16) C14 0.0544(18) 0.0358(17) 0.0328(14) 0.0026(12) -0.0018(13) 0.0186(15) C15 0.0245(12) 0.0204(13) 0.0188(11) -0.0007(9) -0.0044(9) 0.0059(10) C16 0.0264(12) 0.0237(14) 0.0297(12) -0.0009(10) -0.0063(10) 0.0030(11) C17 0.0391(15) 0.0324(16) 0.0335(14) -0.0082(12) -0.0153(12) 0.0026(13) C18 0.0524(17) 0.0403(18) 0.0223(12) -0.0077(12) -0.0082(12) 0.0100(14) C19 0.0414(15) 0.0347(16) 0.0202(12) 0.0032(11) 0.0020(10) 0.0079(12) C20 0.0275(13) 0.0247(14) 0.0211(12) 0.0035(10) -0.0016(9) 0.0059(10) C21 0.0271(13) 0.0367(16) 0.0266(12) 0.0063(11) 0.0027(10) -0.0011(11) C22 0.0418(15) 0.0371(17) 0.0357(14) 0.0020(13) 0.0068(12) -0.0075(13) C23 0.0295(15) 0.055(2) 0.078(2) 0.0020(19) 0.0091(15) 0.0045(14) C24 0.0283(13) 0.0343(16) 0.0417(15) 0.0014(13) -0.0064(11) -0.0055(12) C25 0.0291(14) 0.0421(19) 0.0586(18) -0.0023(15) -0.0059(13) -0.0031(13) C26 0.0441(17) 0.0342(18) 0.076(2) 0.0091(16) -0.0029(16) -0.0093(14) _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 Si1 2.0833(10) . ? Si1 N1 1.713(2) . ? Si1 C1 1.851(2) . ? Si1 H1 1.40(2) . ? Si2 N1 1.769(2) . ? Si2 C14 1.852(3) . ? Si2 C12 1.859(3) . ? Si2 C13 1.863(3) . ? N1 C15 1.459(3) . ? N2 C3 1.367(3) . ? N2 C1 1.419(3) . ? N2 C4 1.492(3) . ? N3 C3 1.365(3) . ? N3 C2 1.377(3) . ? N3 C8 1.489(3) . ? C1 C2 1.357(3) . ? C2 H2 0.9300 . ? C4 C5 1.525(5) . ? C4 C6 1.531(4) . ? C4 C7 1.537(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C11 1.515(4) . ? C8 C9 1.523(4) . ? C8 C10 1.524(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.402(3) . ? C15 C16 1.410(3) . ? C16 C17 1.400(3) . ? C16 C24 1.514(4) . ? C17 C18 1.371(4) . ? C17 H17 0.9300 . ? C18 C19 1.375(4) . ? C18 H18 0.9300 . ? C19 C20 1.399(3) . ? C19 H19 0.9300 . ? C20 C21 1.514(3) . ? C21 C22 1.527(4) . ? C21 C23 1.528(4) . ? C21 H21 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C26 1.528(4) . ? C24 C25 1.537(4) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C1 113.37(10) . . ? N1 Si1 Cl1 111.50(7) . . ? C1 Si1 Cl1 106.03(9) . . ? N1 Si1 H1 108.7(10) . . ? C1 Si1 H1 116.0(10) . . ? Cl1 Si1 H1 100.5(10) . . ? N1 Si2 C14 108.15(11) . . ? N1 Si2 C12 110.51(12) . . ? C14 Si2 C12 110.25(15) . . ? N1 Si2 C13 109.95(13) . . ? C14 Si2 C13 109.98(14) . . ? C12 Si2 C13 108.00(15) . . ? C15 N1 Si1 120.89(15) . . ? C15 N1 Si2 117.96(15) . . ? Si1 N1 Si2 121.13(11) . . ? C3 N2 C1 112.86(18) . . ? C3 N2 C4 122.3(2) . . ? C1 N2 C4 124.85(19) . . ? C3 N3 C2 111.95(19) . . ? C3 N3 C8 124.91(19) . . ? C2 N3 C8 123.11(18) . . ? C2 C1 N2 103.72(19) . . ? C2 C1 Si1 122.12(17) . . ? N2 C1 Si1 133.95(16) . . ? C1 C2 N3 108.66(19) . . ? C1 C2 H2 125.7 . . ? N3 C2 H2 125.7 . . ? N3 C3 N2 102.80(19) . . ? N2 C4 C5 108.7(2) . . ? N2 C4 C6 109.1(2) . . ? C5 C4 C6 112.5(2) . . ? N2 C4 C7 109.0(2) . . ? C5 C4 C7 109.2(3) . . ? C6 C4 C7 108.3(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C11 109.38(19) . . ? N3 C8 C9 108.57(18) . . ? C11 C8 C9 109.4(2) . . ? N3 C8 C10 108.1(2) . . ? C11 C8 C10 110.1(2) . . ? C9 C8 C10 111.3(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 120.8(2) . . ? C20 C15 N1 120.0(2) . . ? C16 C15 N1 119.2(2) . . ? C17 C16 C15 118.0(2) . . ? C17 C16 C24 119.1(2) . . ? C15 C16 C24 122.9(2) . . ? C18 C17 C16 121.7(2) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 119.7(2) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 121.5(2) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C15 118.3(2) . . ? C19 C20 C21 118.5(2) . . ? C15 C20 C21 123.1(2) . . ? C20 C21 C22 111.5(2) . . ? C20 C21 C23 112.6(2) . . ? C22 C21 C23 109.4(2) . . ? C20 C21 H21 107.7 . . ? C22 C21 H21 107.7 . . ? C23 C21 H21 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C16 C24 C26 110.8(2) . . ? C16 C24 C25 111.6(2) . . ? C26 C24 C25 109.8(2) . . ? C16 C24 H24 108.2 . . ? C26 C24 H24 108.2 . . ? C25 C24 H24 108.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 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 C15 19.8(2) . . . . ? Cl1 Si1 N1 C15 -99.72(17) . . . . ? C1 Si1 N1 Si2 -158.48(12) . . . . ? Cl1 Si1 N1 Si2 81.95(12) . . . . ? C14 Si2 N1 C15 3.0(2) . . . . ? C12 Si2 N1 C15 -117.82(19) . . . . ? C13 Si2 N1 C15 123.05(19) . . . . ? C14 Si2 N1 Si1 -178.67(14) . . . . ? C12 Si2 N1 Si1 60.56(18) . . . . ? C13 Si2 N1 Si1 -58.57(17) . . . . ? C3 N2 C1 C2 0.4(3) . . . . ? C4 N2 C1 C2 -179.0(2) . . . . ? C3 N2 C1 Si1 175.0(2) . . . . ? C4 N2 C1 Si1 -4.4(4) . . . . ? N1 Si1 C1 C2 -48.1(2) . . . . ? Cl1 Si1 C1 C2 74.6(2) . . . . ? N1 Si1 C1 N2 138.1(2) . . . . ? Cl1 Si1 C1 N2 -99.2(2) . . . . ? N2 C1 C2 N3 0.3(3) . . . . ? Si1 C1 C2 N3 -175.10(17) . . . . ? C3 N3 C2 C1 -1.0(3) . . . . ? C8 N3 C2 C1 -179.3(2) . . . . ? C2 N3 C3 N2 1.2(3) . . . . ? C8 N3 C3 N2 179.4(2) . . . . ? C1 N2 C3 N3 -1.0(3) . . . . ? C4 N2 C3 N3 178.5(2) . . . . ? C3 N2 C4 C5 117.8(3) . . . . ? C1 N2 C4 C5 -62.7(3) . . . . ? C3 N2 C4 C6 -119.1(3) . . . . ? C1 N2 C4 C6 60.3(3) . . . . ? C3 N2 C4 C7 -1.0(4) . . . . ? C1 N2 C4 C7 178.4(3) . . . . ? C3 N3 C8 C11 10.3(3) . . . . ? C2 N3 C8 C11 -171.6(2) . . . . ? C3 N3 C8 C9 129.6(3) . . . . ? C2 N3 C8 C9 -52.3(3) . . . . ? C3 N3 C8 C10 -109.6(3) . . . . ? C2 N3 C8 C10 68.5(3) . . . . ? Si1 N1 C15 C20 93.4(2) . . . . ? Si2 N1 C15 C20 -88.2(2) . . . . ? Si1 N1 C15 C16 -87.4(3) . . . . ? Si2 N1 C15 C16 91.0(2) . . . . ? C20 C15 C16 C17 0.3(4) . . . . ? N1 C15 C16 C17 -178.9(2) . . . . ? C20 C15 C16 C24 179.4(2) . . . . ? N1 C15 C16 C24 0.3(4) . . . . ? C15 C16 C17 C18 -0.6(4) . . . . ? C24 C16 C17 C18 -179.8(3) . . . . ? C16 C17 C18 C19 0.3(4) . . . . ? C17 C18 C19 C20 0.5(4) . . . . ? C18 C19 C20 C15 -0.8(4) . . . . ? C18 C19 C20 C21 -179.5(2) . . . . ? C16 C15 C20 C19 0.4(4) . . . . ? N1 C15 C20 C19 179.5(2) . . . . ? C16 C15 C20 C21 179.1(2) . . . . ? N1 C15 C20 C21 -1.8(4) . . . . ? C19 C20 C21 C22 70.4(3) . . . . ? C15 C20 C21 C22 -108.3(3) . . . . ? C19 C20 C21 C23 -53.0(3) . . . . ? C15 C20 C21 C23 128.3(3) . . . . ? C17 C16 C24 C26 65.4(3) . . . . ? C15 C16 C24 C26 -113.8(3) . . . . ? C17 C16 C24 C25 -57.3(3) . . . . ? C15 C16 C24 C25 123.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.362 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.064