# 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_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Cameron Jones' _publ_contact_author_email cameron.jones@monash.edu _publ_section_title ; Extremely Bulky Amido-Group 14 Element Chloride Complexes: Potential Synthons for Low Oxidation State Main Group Chemistry ; _publ_author_name C.Jones data_Ar*NSiMe3LiOEt2 _database_code_depnum_ccdc_archive 'CCDC 822594' #TrackingRef '- ArNSiMe3LiOEt2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 Li N O Si' _chemical_formula_weight 591.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li 0.0008 0.0003 '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 9.8835(6) _cell_length_b 10.1932(11) _cell_length_c 18.8112(14) _cell_angle_alpha 74.610(8) _cell_angle_beta 88.130(6) _cell_angle_gamma 68.295(8) _cell_volume 1693.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type mirror _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 20449 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.80 _diffrn_reflns_theta_max 67.22 _reflns_number_total 6002 _reflns_number_gt 4815 _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^)+(0.0650P)^2^+0.2242P] 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 6002 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.68469(5) 0.40111(5) 0.26711(2) 0.02141(13) Uani 1 1 d . . . O1 O 0.22651(13) 0.58823(13) 0.30155(6) 0.0276(3) Uani 1 1 d . . . N1 N 0.57897(14) 0.58121(14) 0.24321(7) 0.0186(3) Uani 1 1 d . . . C1 C 0.62834(16) 0.69545(16) 0.21757(8) 0.0169(3) Uani 1 1 d . . . Li1 Li 0.3774(4) 0.6421(4) 0.2560(2) 0.0393(8) Uani 1 1 d . . . C2 C 0.64909(17) 0.77495(17) 0.26502(8) 0.0177(3) Uani 1 1 d . . . C3 C 0.70198(17) 0.88626(17) 0.23897(9) 0.0184(3) Uani 1 1 d . . . H3 H 0.7187 0.9348 0.2725 0.022 Uiso 1 1 calc R . . C4 C 0.73134(17) 0.92900(17) 0.16549(9) 0.0186(3) Uani 1 1 d . . . C5 C 0.69874(17) 0.86047(17) 0.11727(8) 0.0187(3) Uani 1 1 d . . . H5 H 0.7113 0.8924 0.0661 0.022 Uiso 1 1 calc R . . C6 C 0.64837(17) 0.74676(17) 0.14153(8) 0.0172(3) Uani 1 1 d . . . C7 C 0.79355(19) 1.04647(18) 0.13934(9) 0.0233(4) Uani 1 1 d . . . H7A H 0.8040 1.0638 0.0860 0.035 Uiso 1 1 calc R . . H7B H 0.8894 1.0147 0.1653 0.035 Uiso 1 1 calc R . . H7C H 0.7277 1.1374 0.1496 0.035 Uiso 1 1 calc R . . C8 C 0.60078(18) 0.74287(17) 0.34337(8) 0.0188(3) Uani 1 1 d . . . H8 H 0.6301 0.6340 0.3614 0.023 Uiso 1 1 calc R . . C9 C 0.43430(18) 0.80883(18) 0.34483(9) 0.0205(3) Uani 1 1 d . . . C10 C 0.34157(19) 0.89613(18) 0.28194(9) 0.0235(4) Uani 1 1 d . . . H10 H 0.3820 0.9192 0.2360 0.028 Uiso 1 1 calc R . . C11 C 0.1907(2) 0.95011(19) 0.28532(10) 0.0285(4) Uani 1 1 d . . . H11 H 0.1295 1.0082 0.2416 0.034 Uiso 1 1 calc R . . C12 C 0.1288(2) 0.9202(2) 0.35169(10) 0.0306(4) Uani 1 1 d . . . H12 H 0.0258 0.9574 0.3539 0.037 Uiso 1 1 calc R . . C13 C 0.2194(2) 0.8351(2) 0.41485(10) 0.0315(4) Uani 1 1 d . . . H13 H 0.1784 0.8146 0.4609 0.038 Uiso 1 1 calc R . . C14 C 0.3698(2) 0.7796(2) 0.41137(9) 0.0265(4) Uani 1 1 d . . . H14 H 0.4303 0.7205 0.4552 0.032 Uiso 1 1 calc R . . C15 C 0.67976(18) 0.78566(18) 0.39627(8) 0.0204(3) Uani 1 1 d . . . C16 C 0.82005(19) 0.69175(19) 0.42533(9) 0.0249(4) Uani 1 1 d . . . H16 H 0.8639 0.6021 0.4123 0.030 Uiso 1 1 calc R . . C17 C 0.8976(2) 0.7259(2) 0.47300(10) 0.0313(4) Uani 1 1 d . . . H17 H 0.9934 0.6601 0.4923 0.038 Uiso 1 1 calc R . . C18 C 0.8350(2) 0.8564(2) 0.49238(10) 0.0340(4) Uani 1 1 d . . . H18 H 0.8872 0.8804 0.5253 0.041 Uiso 1 1 calc R . . C19 C 0.6961(2) 0.9511(2) 0.46336(10) 0.0327(4) Uani 1 1 d . . . H19 H 0.6529 1.0410 0.4763 0.039 Uiso 1 1 calc R . . C20 C 0.6186(2) 0.91694(19) 0.41560(9) 0.0256(4) Uani 1 1 d . . . H20 H 0.5233 0.9836 0.3960 0.031 Uiso 1 1 calc R . . C21 C 0.60451(17) 0.67839(17) 0.08757(8) 0.0185(3) Uani 1 1 d . . . H21 H 0.6481 0.5698 0.1100 0.022 Uiso 1 1 calc R . . C22 C 0.44023(18) 0.71900(18) 0.08100(8) 0.0199(3) Uani 1 1 d . . . C23 C 0.34171(18) 0.85753(18) 0.08273(9) 0.0223(4) Uani 1 1 d . . . H23 H 0.3774 0.9285 0.0893 0.027 Uiso 1 1 calc R . . C24 C 0.19199(19) 0.8927(2) 0.07495(9) 0.0269(4) Uani 1 1 d . . . H24 H 0.1264 0.9873 0.0765 0.032 Uiso 1 1 calc R . . C25 C 0.1376(2) 0.7912(2) 0.06490(9) 0.0294(4) Uani 1 1 d . . . H25 H 0.0352 0.8156 0.0596 0.035 Uiso 1 1 calc R . . C26 C 0.2344(2) 0.6536(2) 0.06269(10) 0.0292(4) Uani 1 1 d . . . H26 H 0.1983 0.5833 0.0555 0.035 Uiso 1 1 calc R . . C27 C 0.3839(2) 0.61818(19) 0.07100(9) 0.0253(4) Uani 1 1 d . . . H27 H 0.4490 0.5231 0.0698 0.030 Uiso 1 1 calc R . . C28 C 0.66844(18) 0.70705(17) 0.01244(9) 0.0193(3) Uani 1 1 d . . . C29 C 0.81983(18) 0.66251(18) 0.00911(9) 0.0226(4) Uani 1 1 d . . . H29 H 0.8810 0.6165 0.0537 0.027 Uiso 1 1 calc R . . C30 C 0.8823(2) 0.68397(19) -0.05757(9) 0.0255(4) Uani 1 1 d . . . H30 H 0.9852 0.6546 -0.0586 0.031 Uiso 1 1 calc R . . C31 C 0.7940(2) 0.74883(18) -0.12345(9) 0.0259(4) Uani 1 1 d . . . H31 H 0.8365 0.7622 -0.1695 0.031 Uiso 1 1 calc R . . C32 C 0.6443(2) 0.79355(19) -0.12127(9) 0.0257(4) Uani 1 1 d . . . H32 H 0.5835 0.8386 -0.1660 0.031 Uiso 1 1 calc R . . C33 C 0.58194(19) 0.77280(18) -0.05369(9) 0.0218(4) Uani 1 1 d . . . H33 H 0.4788 0.8041 -0.0528 0.026 Uiso 1 1 calc R . . C34 C 0.7797(2) 0.3314(2) 0.36296(10) 0.0371(5) Uani 1 1 d . . . H34A H 0.8491 0.3788 0.3648 0.056 Uiso 1 1 calc R . . H34B H 0.8321 0.2249 0.3747 0.056 Uiso 1 1 calc R . . H34C H 0.7071 0.3545 0.3991 0.056 Uiso 1 1 calc R . . C35 C 0.83782(19) 0.34195(19) 0.20594(10) 0.0283(4) Uani 1 1 d . . . H35A H 0.7981 0.3379 0.1599 0.042 Uiso 1 1 calc R . . H35B H 0.9086 0.2446 0.2315 0.042 Uiso 1 1 calc R . . H35C H 0.8863 0.4126 0.1947 0.042 Uiso 1 1 calc R . . C36 C 0.5658(2) 0.2961(2) 0.26352(12) 0.0358(5) Uani 1 1 d . . . H36A H 0.4832 0.3250 0.2939 0.054 Uiso 1 1 calc R . . H36B H 0.6227 0.1907 0.2825 0.054 Uiso 1 1 calc R . . H36C H 0.5292 0.3175 0.2123 0.054 Uiso 1 1 calc R . . C37 C 0.08478(19) 0.6643(2) 0.26138(10) 0.0283(4) Uani 1 1 d . . . H37A H 0.0883 0.7472 0.2206 0.034 Uiso 1 1 calc R . . H37B H 0.0120 0.7055 0.2950 0.034 Uiso 1 1 calc R . . C38 C 0.0361(2) 0.5668(2) 0.22995(11) 0.0354(4) Uani 1 1 d . . . H38A H 0.1116 0.5189 0.2000 0.053 Uiso 1 1 calc R . . H38B H -0.0550 0.6258 0.1989 0.053 Uiso 1 1 calc R . . H38C H 0.0199 0.4919 0.2704 0.053 Uiso 1 1 calc R . . C39 C 0.2270(2) 0.4771(3) 0.36631(12) 0.0480(6) Uani 1 1 d . . . H39A H 0.2230 0.3918 0.3520 0.058 Uiso 1 1 calc R . . H39B H 0.1393 0.5153 0.3929 0.058 Uiso 1 1 calc R . . C40 C 0.3601(2) 0.4291(2) 0.41605(11) 0.0402(5) Uani 1 1 d . . . H40A H 0.4468 0.4039 0.3879 0.060 Uiso 1 1 calc R . . H40B H 0.3654 0.3429 0.4561 0.060 Uiso 1 1 calc R . . H40C H 0.3559 0.5089 0.4369 0.060 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 0.0214(3) 0.0173(2) 0.0255(2) -0.00601(17) 0.00368(18) -0.00735(18) O1 0.0201(6) 0.0307(7) 0.0299(6) -0.0022(5) -0.0009(5) -0.0113(5) N1 0.0186(7) 0.0195(7) 0.0201(7) -0.0066(5) 0.0027(5) -0.0089(6) C1 0.0111(8) 0.0164(8) 0.0217(8) -0.0055(6) 0.0008(6) -0.0033(6) Li1 0.0248(17) 0.0326(17) 0.056(2) -0.0053(15) 0.0070(15) -0.0104(14) C2 0.0149(8) 0.0178(8) 0.0183(8) -0.0050(6) -0.0004(6) -0.0039(6) C3 0.0154(8) 0.0190(8) 0.0220(8) -0.0089(6) 0.0001(6) -0.0053(6) C4 0.0153(8) 0.0185(8) 0.0222(8) -0.0067(6) 0.0009(6) -0.0055(6) C5 0.0170(8) 0.0201(8) 0.0179(7) -0.0050(6) 0.0023(6) -0.0059(6) C6 0.0129(8) 0.0178(8) 0.0204(8) -0.0074(6) 0.0001(6) -0.0035(6) C7 0.0251(9) 0.0246(9) 0.0245(8) -0.0080(7) 0.0036(7) -0.0136(7) C8 0.0193(9) 0.0188(8) 0.0191(8) -0.0057(6) 0.0012(6) -0.0076(6) C9 0.0223(9) 0.0206(8) 0.0230(8) -0.0097(6) 0.0032(6) -0.0105(7) C10 0.0234(9) 0.0222(8) 0.0243(8) -0.0061(7) 0.0035(7) -0.0083(7) C11 0.0237(10) 0.0246(9) 0.0338(10) -0.0070(7) 0.0004(7) -0.0059(7) C12 0.0198(9) 0.0345(10) 0.0408(10) -0.0165(8) 0.0070(8) -0.0098(8) C13 0.0280(10) 0.0449(11) 0.0293(9) -0.0167(8) 0.0111(8) -0.0187(9) C14 0.0263(10) 0.0361(10) 0.0207(8) -0.0090(7) 0.0027(7) -0.0151(8) C15 0.0225(9) 0.0253(8) 0.0157(7) -0.0048(6) 0.0038(6) -0.0124(7) C16 0.0235(9) 0.0278(9) 0.0232(8) -0.0070(7) 0.0036(7) -0.0095(7) C17 0.0233(10) 0.0424(11) 0.0275(9) -0.0052(8) -0.0030(7) -0.0143(8) C18 0.0372(12) 0.0502(12) 0.0255(9) -0.0145(8) 0.0012(8) -0.0255(10) C19 0.0383(12) 0.0385(11) 0.0313(10) -0.0186(8) 0.0065(8) -0.0196(9) C20 0.0255(10) 0.0273(9) 0.0255(9) -0.0093(7) 0.0027(7) -0.0103(7) C21 0.0196(9) 0.0181(8) 0.0191(8) -0.0070(6) 0.0009(6) -0.0073(7) C22 0.0230(9) 0.0236(8) 0.0160(7) -0.0066(6) 0.0018(6) -0.0111(7) C23 0.0217(9) 0.0243(9) 0.0230(8) -0.0078(7) 0.0016(7) -0.0100(7) C24 0.0217(10) 0.0309(10) 0.0249(9) -0.0067(7) 0.0026(7) -0.0070(8) C25 0.0212(9) 0.0422(11) 0.0262(9) -0.0063(8) 0.0005(7) -0.0155(8) C26 0.0298(10) 0.0364(10) 0.0302(9) -0.0094(8) 0.0011(7) -0.0221(8) C27 0.0292(10) 0.0259(9) 0.0246(8) -0.0088(7) 0.0031(7) -0.0132(7) C28 0.0229(9) 0.0158(8) 0.0215(8) -0.0083(6) 0.0030(6) -0.0079(6) C29 0.0214(9) 0.0229(8) 0.0231(8) -0.0090(7) 0.0001(7) -0.0060(7) C30 0.0217(9) 0.0247(9) 0.0312(9) -0.0115(7) 0.0058(7) -0.0075(7) C31 0.0332(11) 0.0236(9) 0.0238(9) -0.0091(7) 0.0093(7) -0.0126(8) C32 0.0325(10) 0.0234(9) 0.0206(8) -0.0053(7) 0.0000(7) -0.0102(7) C33 0.0215(9) 0.0211(8) 0.0240(8) -0.0072(6) 0.0006(7) -0.0084(7) C34 0.0397(12) 0.0282(10) 0.0321(10) -0.0037(8) -0.0010(8) -0.0032(9) C35 0.0243(10) 0.0216(9) 0.0381(10) -0.0108(7) 0.0058(8) -0.0061(7) C36 0.0358(11) 0.0278(10) 0.0513(12) -0.0162(9) 0.0152(9) -0.0176(9) C37 0.0224(9) 0.0295(9) 0.0300(9) -0.0052(7) -0.0021(7) -0.0081(7) C38 0.0303(11) 0.0378(11) 0.0390(11) -0.0093(9) -0.0036(8) -0.0141(9) C39 0.0332(12) 0.0614(15) 0.0371(11) 0.0121(10) -0.0035(9) -0.0210(11) C40 0.0334(12) 0.0494(13) 0.0307(10) -0.0032(9) -0.0003(8) -0.0127(10) _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 1.6846(14) . ? Si1 C36 1.873(2) . ? Si1 C35 1.8862(17) . ? Si1 C34 1.891(2) . ? O1 C39 1.425(2) . ? O1 C37 1.445(2) . ? O1 Li1 1.880(4) . ? N1 C1 1.391(2) . ? N1 Li1 1.883(4) . ? C1 C2 1.419(2) . ? C1 C6 1.421(2) . ? Li1 C10 2.655(4) . ? C2 C3 1.388(2) . ? C2 C8 1.523(2) . ? C3 C4 1.390(2) . ? C3 H3 0.9500 . ? C4 C5 1.392(2) . ? C4 C7 1.505(2) . ? C5 C6 1.390(2) . ? C5 H5 0.9500 . ? C6 C21 1.527(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C15 1.524(2) . ? C8 C9 1.533(2) . ? C8 H8 1.0000 . ? C9 C10 1.393(2) . ? C9 C14 1.397(2) . ? C10 C11 1.392(2) . ? C10 H10 0.9500 . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 C13 1.383(3) . ? C12 H12 0.9500 . ? C13 C14 1.387(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.388(2) . ? C15 C20 1.391(2) . ? C16 C17 1.386(3) . ? C16 H16 0.9500 . ? C17 C18 1.385(3) . ? C17 H17 0.9500 . ? C18 C19 1.380(3) . ? C18 H18 0.9500 . ? C19 C20 1.387(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.520(2) . ? C21 C28 1.530(2) . ? C21 H21 1.0000 . ? C22 C27 1.391(2) . ? C22 C23 1.396(2) . ? C23 C24 1.390(2) . ? C23 H23 0.9500 . ? C24 C25 1.385(3) . ? C24 H24 0.9500 . ? C25 C26 1.385(3) . ? C25 H25 0.9500 . ? C26 C27 1.389(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.390(2) . ? C28 C29 1.398(2) . ? C29 C30 1.380(2) . ? C29 H29 0.9500 . ? C30 C31 1.394(3) . ? C30 H30 0.9500 . ? C31 C32 1.380(3) . ? C31 H31 0.9500 . ? C32 C33 1.394(2) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.501(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.485(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 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 C36 108.04(8) . . ? N1 Si1 C35 115.78(7) . . ? C36 Si1 C35 106.68(8) . . ? N1 Si1 C34 114.01(8) . . ? C36 Si1 C34 108.08(10) . . ? C35 Si1 C34 103.79(9) . . ? C39 O1 C37 112.72(14) . . ? C39 O1 Li1 131.89(16) . . ? C37 O1 Li1 115.18(15) . . ? C1 N1 Si1 125.53(11) . . ? C1 N1 Li1 114.39(14) . . ? Si1 N1 Li1 119.98(13) . . ? N1 C1 C2 121.49(13) . . ? N1 C1 C6 121.76(14) . . ? C2 C1 C6 116.53(14) . . ? O1 Li1 N1 146.1(2) . . ? O1 Li1 C10 105.67(15) . . ? N1 Li1 C10 97.50(15) . . ? C3 C2 C1 120.74(14) . . ? C3 C2 C8 120.94(14) . . ? C1 C2 C8 118.16(14) . . ? C2 C3 C4 122.20(14) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? C3 C4 C5 117.27(15) . . ? C3 C4 C7 121.05(14) . . ? C5 C4 C7 121.67(14) . . ? C6 C5 C4 122.09(14) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C1 120.73(14) . . ? C5 C6 C21 121.62(14) . . ? C1 C6 C21 117.56(14) . . ? 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 . . ? C2 C8 C15 112.44(13) . . ? C2 C8 C9 111.82(13) . . ? C15 C8 C9 112.85(13) . . ? C2 C8 H8 106.4 . . ? C15 C8 H8 106.4 . . ? C9 C8 H8 106.4 . . ? C10 C9 C14 117.35(16) . . ? C10 C9 C8 122.99(14) . . ? C14 C9 C8 119.65(15) . . ? C11 C10 C9 121.12(16) . . ? C11 C10 Li1 98.94(13) . . ? C9 C10 Li1 84.45(13) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? Li1 C10 H10 86.6 . . ? C12 C11 C10 120.70(17) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 118.90(17) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C12 C13 C14 120.44(16) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C9 121.47(17) . . ? C13 C14 H14 119.3 . . ? C9 C14 H14 119.3 . . ? C16 C15 C20 118.19(16) . . ? C16 C15 C8 118.99(15) . . ? C20 C15 C8 122.80(15) . . ? C17 C16 C15 121.43(17) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C18 C17 C16 119.84(18) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 119.23(17) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 120.90(18) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C15 120.40(17) . . ? C19 C20 H20 119.8 . . ? C15 C20 H20 119.8 . . ? C22 C21 C6 111.73(12) . . ? C22 C21 C28 112.81(13) . . ? C6 C21 C28 113.43(13) . . ? C22 C21 H21 106.1 . . ? C6 C21 H21 106.1 . . ? C28 C21 H21 106.1 . . ? C27 C22 C23 117.95(16) . . ? C27 C22 C21 120.04(14) . . ? C23 C22 C21 121.98(15) . . ? C24 C23 C22 120.75(16) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C23 120.62(17) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.12(17) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C25 C26 C27 120.22(17) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C22 121.33(16) . . ? C26 C27 H27 119.3 . . ? C22 C27 H27 119.3 . . ? C33 C28 C29 117.97(15) . . ? C33 C28 C21 122.55(15) . . ? C29 C28 C21 119.46(14) . . ? C30 C29 C28 121.37(16) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 119.91(17) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 119.54(15) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 120.21(16) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C28 C33 C32 120.98(16) . . ? C28 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O1 C37 C38 112.86(15) . . ? O1 C37 H37A 109.0 . . ? C38 C37 H37A 109.0 . . ? O1 C37 H37B 109.0 . . ? C38 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O1 C39 C40 111.08(17) . . ? O1 C39 H39A 109.4 . . ? C40 C39 H39A 109.4 . . ? O1 C39 H39B 109.4 . . ? C40 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 67.22 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.295 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.049 # Attachment '- ArNSiMe3LiTHF.CIF' data_Ar*NSiMe3LiTHF _database_code_depnum_ccdc_archive 'CCDC 822595' #TrackingRef '- ArNSiMe3LiTHF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H44 Li N O Si' _chemical_formula_weight 589.79 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' Li Li -0.0003 0.0001 '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' _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 9.7625(4) _cell_length_b 10.1602(4) _cell_length_c 18.8405(7) _cell_angle_alpha 105.507(3) _cell_angle_beta 90.534(3) _cell_angle_gamma 112.600(4) _cell_volume 1649.22(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.979 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 10292 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6437 _reflns_number_gt 5103 _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^)+(0.0351P)^2^+0.4038P] 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 6437 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.80949(5) 0.89956(5) 0.22965(2) 0.01687(12) Uani 1 1 d . . . O1 O 1.26086(15) 1.07461(14) 0.23680(7) 0.0305(3) Uani 1 1 d . . . N1 N 0.91761(15) 1.08373(14) 0.26174(7) 0.0151(3) Uani 1 1 d . . . C1 C 0.86139(17) 1.19320(16) 0.28419(9) 0.0138(3) Uani 1 1 d . . . C2 C 0.83506(18) 1.26801(17) 0.23494(9) 0.0149(3) Uani 1 1 d . . . C3 C 0.77704(18) 1.37541(17) 0.25938(9) 0.0158(3) Uani 1 1 d . . . H3 H 0.7563 1.4208 0.2250 0.019 Uiso 1 1 calc R . . C4 C 0.74825(18) 1.41875(17) 0.33191(9) 0.0156(3) Uani 1 1 d . . . C5 C 0.78380(18) 1.35377(17) 0.38158(9) 0.0156(3) Uani 1 1 d . . . H5 H 0.7705 1.3859 0.4322 0.019 Uiso 1 1 calc R . . C6 C 0.83819(17) 1.24320(16) 0.35924(9) 0.0144(3) Uani 1 1 d . . . C7 C 0.6824(2) 1.53356(19) 0.35614(10) 0.0224(4) Uani 1 1 d . . . H7A H 0.5794 1.4924 0.3320 0.034 Uiso 1 1 calc R . . H7B H 0.7422 1.6229 0.3420 0.034 Uiso 1 1 calc R . . H7C H 0.6831 1.5600 0.4102 0.034 Uiso 1 1 calc R . . C8 C 0.87823(19) 1.23349(17) 0.15644(9) 0.0159(3) Uani 1 1 d . . . H8 H 0.8443 1.1227 0.1377 0.019 Uiso 1 1 calc R . . C9 C 1.04698(19) 1.29975(17) 0.15427(9) 0.0166(4) Uani 1 1 d . . . C10 C 1.14946(19) 1.38626(18) 0.21723(9) 0.0197(4) Uani 1 1 d . . . H10 H 1.1145 1.4066 0.2641 0.024 Uiso 1 1 calc R . . C11 C 1.3024(2) 1.44380(19) 0.21291(10) 0.0248(4) Uani 1 1 d . . . H11 H 1.3706 1.5016 0.2568 0.030 Uiso 1 1 calc R . . C12 C 1.3557(2) 1.41746(19) 0.14520(10) 0.0252(4) Uani 1 1 d . . . H12 H 1.4601 1.4577 0.1422 0.030 Uiso 1 1 calc R . . C13 C 1.2555(2) 1.3319(2) 0.08191(10) 0.0251(4) Uani 1 1 d . . . H13 H 1.2911 1.3137 0.0350 0.030 Uiso 1 1 calc R . . C14 C 1.1033(2) 1.27242(19) 0.08634(9) 0.0213(4) Uani 1 1 d . . . H14 H 1.0359 1.2119 0.0424 0.026 Uiso 1 1 calc R . . C15 C 0.79490(19) 1.27678(17) 0.10361(9) 0.0166(4) Uani 1 1 d . . . C16 C 0.8608(2) 1.40698(18) 0.08319(9) 0.0213(4) Uani 1 1 d . . . H16 H 0.9625 1.4711 0.1011 0.026 Uiso 1 1 calc R . . C17 C 0.7794(2) 1.4443(2) 0.03684(10) 0.0263(4) Uani 1 1 d . . . H17 H 0.8261 1.5331 0.0230 0.032 Uiso 1 1 calc R . . C18 C 0.6310(2) 1.3531(2) 0.01083(10) 0.0261(4) Uani 1 1 d . . . H18 H 0.5756 1.3788 -0.0208 0.031 Uiso 1 1 calc R . . C19 C 0.5639(2) 1.2240(2) 0.03124(9) 0.0248(4) Uani 1 1 d . . . H19 H 0.4618 1.1609 0.0138 0.030 Uiso 1 1 calc R . . C20 C 0.6454(2) 1.18640(19) 0.07723(9) 0.0208(4) Uani 1 1 d . . . H20 H 0.5983 1.0974 0.0909 0.025 Uiso 1 1 calc R . . C21 C 0.88192(18) 1.17529(17) 0.41457(8) 0.0143(3) Uani 1 1 d . . . H21 H 0.8319 1.0647 0.3921 0.017 Uiso 1 1 calc R . . C22 C 0.82495(18) 1.20907(17) 0.48956(9) 0.0147(3) Uani 1 1 d . . . C23 C 0.67155(19) 1.16510(17) 0.49235(9) 0.0178(4) Uani 1 1 d . . . H23 H 0.6048 1.1161 0.4475 0.021 Uiso 1 1 calc R . . C24 C 0.6146(2) 1.19153(18) 0.55942(9) 0.0210(4) Uani 1 1 d . . . H24 H 0.5098 1.1616 0.5601 0.025 Uiso 1 1 calc R . . C25 C 0.7103(2) 1.26152(18) 0.62554(9) 0.0211(4) Uani 1 1 d . . . H25 H 0.6716 1.2787 0.6716 0.025 Uiso 1 1 calc R . . C26 C 0.8626(2) 1.30593(18) 0.62364(9) 0.0202(4) Uani 1 1 d . . . H26 H 0.9289 1.3543 0.6687 0.024 Uiso 1 1 calc R . . C27 C 0.91958(19) 1.28047(17) 0.55637(9) 0.0174(4) Uani 1 1 d . . . H27 H 1.0246 1.3122 0.5560 0.021 Uiso 1 1 calc R . . C28 C 1.04929(19) 1.21341(17) 0.42168(8) 0.0151(3) Uani 1 1 d . . . C29 C 1.1029(2) 1.10814(18) 0.43020(9) 0.0190(4) Uani 1 1 d . . . H29 H 1.0343 1.0135 0.4324 0.023 Uiso 1 1 calc R . . C30 C 1.2550(2) 1.14027(19) 0.43541(10) 0.0240(4) Uani 1 1 d . . . H30 H 1.2893 1.0678 0.4415 0.029 Uiso 1 1 calc R . . C31 C 1.3566(2) 1.2769(2) 0.43185(10) 0.0253(4) Uani 1 1 d . . . H31 H 1.4604 1.2979 0.4344 0.030 Uiso 1 1 calc R . . C32 C 1.3053(2) 1.38331(19) 0.42448(10) 0.0230(4) Uani 1 1 d . . . H32 H 1.3745 1.4781 0.4227 0.028 Uiso 1 1 calc R . . C33 C 1.15355(19) 1.35160(18) 0.41978(9) 0.0181(4) Uani 1 1 d . . . H33 H 1.1201 1.4256 0.4152 0.022 Uiso 1 1 calc R . . C34 C 0.6365(2) 0.83949(19) 0.27730(10) 0.0249(4) Uani 1 1 d . . . H34A H 0.6618 0.8237 0.3239 0.037 Uiso 1 1 calc R . . H34B H 0.5606 0.7464 0.2449 0.037 Uiso 1 1 calc R . . H34C H 0.5971 0.9172 0.2878 0.037 Uiso 1 1 calc R . . C35 C 0.7412(2) 0.8274(2) 0.12741(10) 0.0298(4) Uani 1 1 d . . . H35A H 0.6728 0.8712 0.1166 0.045 Uiso 1 1 calc R . . H35B H 0.6886 0.7186 0.1130 0.045 Uiso 1 1 calc R . . H35C H 0.8267 0.8549 0.0994 0.045 Uiso 1 1 calc R . . C36 C 0.9215(2) 0.79310(19) 0.24478(11) 0.0275(4) Uani 1 1 d . . . H36A H 1.0126 0.8226 0.2208 0.041 Uiso 1 1 calc R . . H36B H 0.8619 0.6860 0.2233 0.041 Uiso 1 1 calc R . . H36C H 0.9485 0.8150 0.2981 0.041 Uiso 1 1 calc R . . C37 C 1.3633(2) 1.0097(2) 0.24920(12) 0.0408(5) Uani 1 1 d . . . H37A H 1.3450 0.9754 0.2941 0.049 Uiso 1 1 calc R . . H37B H 1.4680 1.0836 0.2560 0.049 Uiso 1 1 calc R . . C38 C 1.3352(3) 0.8796(3) 0.18106(12) 0.0458(6) Uani 1 1 d . . . H38A H 1.2832 0.7840 0.1924 0.055 Uiso 1 1 calc R . . H38B H 1.4306 0.8822 0.1626 0.055 Uiso 1 1 calc R . . C39 C 1.2376(3) 0.8967(3) 0.12375(11) 0.0460(6) Uani 1 1 d . . . H39A H 1.2790 0.8896 0.0758 0.055 Uiso 1 1 calc R . . H39B H 1.1342 0.8197 0.1156 0.055 Uiso 1 1 calc R . . C40 C 1.2413(3) 1.0496(3) 0.15789(12) 0.0496(7) Uani 1 1 d . . . H40A H 1.3253 1.1254 0.1429 0.059 Uiso 1 1 calc R . . H40B H 1.1467 1.0544 0.1423 0.059 Uiso 1 1 calc R . . Li1 Li 1.1242(4) 1.1375(3) 0.29185(18) 0.0313(7) Uani 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 Si1 0.0194(3) 0.0159(2) 0.0164(3) 0.00435(18) 0.0022(2) 0.0086(2) O1 0.0320(8) 0.0378(7) 0.0355(8) 0.0158(6) 0.0145(6) 0.0250(6) N1 0.0172(7) 0.0162(7) 0.0148(7) 0.0054(5) 0.0037(6) 0.0091(6) C1 0.0102(8) 0.0147(8) 0.0156(9) 0.0040(6) 0.0019(7) 0.0042(7) C2 0.0134(8) 0.0156(8) 0.0148(9) 0.0052(6) 0.0009(7) 0.0043(7) C3 0.0160(9) 0.0174(8) 0.0174(9) 0.0086(7) 0.0023(7) 0.0080(7) C4 0.0136(8) 0.0156(8) 0.0181(9) 0.0051(6) 0.0028(7) 0.0061(7) C5 0.0136(8) 0.0184(8) 0.0138(8) 0.0045(6) 0.0032(7) 0.0057(7) C6 0.0117(8) 0.0150(8) 0.0155(9) 0.0048(6) 0.0009(7) 0.0041(7) C7 0.0258(10) 0.0272(9) 0.0224(10) 0.0104(7) 0.0070(8) 0.0170(8) C8 0.0198(9) 0.0163(8) 0.0135(8) 0.0053(6) 0.0020(7) 0.0088(7) C9 0.0207(9) 0.0179(8) 0.0169(9) 0.0090(7) 0.0050(7) 0.0112(7) C10 0.0217(9) 0.0193(8) 0.0185(9) 0.0047(7) 0.0058(8) 0.0092(7) C11 0.0217(10) 0.0232(9) 0.0248(10) 0.0021(7) 0.0017(8) 0.0073(8) C12 0.0197(10) 0.0252(9) 0.0343(11) 0.0129(8) 0.0104(9) 0.0099(8) C13 0.0301(11) 0.0347(10) 0.0220(10) 0.0147(8) 0.0125(9) 0.0206(9) C14 0.0258(10) 0.0286(9) 0.0150(9) 0.0079(7) 0.0033(8) 0.0158(8) C15 0.0214(9) 0.0196(8) 0.0119(8) 0.0041(6) 0.0039(7) 0.0117(7) C16 0.0220(10) 0.0227(9) 0.0217(10) 0.0080(7) 0.0031(8) 0.0106(8) C17 0.0353(11) 0.0287(10) 0.0257(10) 0.0154(8) 0.0075(9) 0.0191(9) C18 0.0337(11) 0.0381(11) 0.0181(10) 0.0098(8) 0.0028(8) 0.0258(9) C19 0.0225(10) 0.0333(10) 0.0184(10) 0.0009(7) -0.0008(8) 0.0156(8) C20 0.0233(10) 0.0239(9) 0.0169(9) 0.0057(7) 0.0046(8) 0.0115(8) C21 0.0154(9) 0.0138(8) 0.0140(8) 0.0042(6) 0.0019(7) 0.0060(7) C22 0.0182(9) 0.0143(8) 0.0162(9) 0.0079(6) 0.0051(7) 0.0089(7) C23 0.0180(9) 0.0190(8) 0.0169(9) 0.0066(7) 0.0007(7) 0.0068(7) C24 0.0185(9) 0.0232(9) 0.0250(10) 0.0105(7) 0.0080(8) 0.0098(8) C25 0.0289(10) 0.0207(9) 0.0180(9) 0.0079(7) 0.0098(8) 0.0127(8) C26 0.0260(10) 0.0201(9) 0.0151(9) 0.0044(7) -0.0001(8) 0.0105(8) C27 0.0186(9) 0.0176(8) 0.0174(9) 0.0053(7) 0.0013(7) 0.0086(7) C28 0.0193(9) 0.0194(8) 0.0075(8) 0.0030(6) 0.0018(7) 0.0094(7) C29 0.0227(9) 0.0212(9) 0.0164(9) 0.0074(7) 0.0032(7) 0.0110(8) C30 0.0270(10) 0.0290(10) 0.0237(10) 0.0084(8) 0.0029(8) 0.0189(9) C31 0.0176(9) 0.0341(10) 0.0252(10) 0.0057(8) 0.0013(8) 0.0135(8) C32 0.0196(9) 0.0233(9) 0.0235(10) 0.0064(7) 0.0033(8) 0.0061(8) C33 0.0208(9) 0.0206(9) 0.0157(9) 0.0056(7) 0.0034(7) 0.0111(7) C34 0.0218(10) 0.0221(9) 0.0283(11) 0.0068(7) 0.0038(8) 0.0067(8) C35 0.0382(12) 0.0218(9) 0.0234(10) 0.0027(7) -0.0002(9) 0.0084(9) C36 0.0283(11) 0.0219(9) 0.0370(11) 0.0105(8) 0.0076(9) 0.0136(8) C37 0.0362(12) 0.0519(13) 0.0482(14) 0.0126(11) 0.0057(11) 0.0335(11) C38 0.0638(16) 0.0579(14) 0.0398(13) 0.0163(11) 0.0145(12) 0.0486(13) C39 0.0640(16) 0.0713(16) 0.0278(12) 0.0192(11) 0.0188(11) 0.0501(14) C40 0.0756(18) 0.0725(16) 0.0420(14) 0.0384(12) 0.0332(13) 0.0582(15) Li1 0.0220(17) 0.0354(17) 0.0330(19) 0.0018(14) 0.0023(14) 0.0136(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 Si1 N1 1.6871(13) . ? Si1 C36 1.8746(17) . ? Si1 C35 1.8809(18) . ? Si1 C34 1.8869(18) . ? O1 C40 1.438(2) . ? O1 C37 1.441(2) . ? O1 Li1 1.895(3) . ? N1 C1 1.3925(19) . ? N1 Li1 1.912(3) . ? C1 C6 1.421(2) . ? C1 C2 1.424(2) . ? C2 C3 1.391(2) . ? C2 C8 1.528(2) . ? C3 C4 1.386(2) . ? C4 C5 1.390(2) . ? C4 C7 1.509(2) . ? C5 C6 1.390(2) . ? C6 C21 1.532(2) . ? C8 C9 1.527(2) . ? C8 C15 1.530(2) . ? C9 C10 1.387(2) . ? C9 C14 1.399(2) . ? C10 C11 1.391(2) . ? C11 C12 1.381(2) . ? C12 C13 1.380(3) . ? C13 C14 1.385(2) . ? C15 C20 1.390(2) . ? C15 C16 1.391(2) . ? C16 C17 1.391(2) . ? C17 C18 1.382(3) . ? C18 C19 1.382(2) . ? C19 C20 1.389(2) . ? C21 C28 1.523(2) . ? C21 C22 1.525(2) . ? C22 C27 1.392(2) . ? C22 C23 1.395(2) . ? C23 C24 1.387(2) . ? C24 C25 1.387(2) . ? C25 C26 1.382(2) . ? C26 C27 1.389(2) . ? C28 C33 1.392(2) . ? C28 C29 1.402(2) . ? C28 Li1 2.564(3) . ? C29 C30 1.388(2) . ? C29 Li1 2.703(4) . ? C30 C31 1.381(3) . ? C31 C32 1.391(2) . ? C32 C33 1.386(2) . ? C33 Li1 2.707(4) . ? C37 C38 1.509(3) . ? C38 C39 1.521(3) . ? C39 C40 1.500(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C36 108.85(8) . . ? N1 Si1 C35 115.34(7) . . ? C36 Si1 C35 105.36(8) . . ? N1 Si1 C34 113.51(7) . . ? C36 Si1 C34 107.70(8) . . ? C35 Si1 C34 105.54(9) . . ? C40 O1 C37 105.51(14) . . ? C40 O1 Li1 116.72(15) . . ? C37 O1 Li1 135.92(16) . . ? C1 N1 Si1 123.85(11) . . ? C1 N1 Li1 117.82(14) . . ? Si1 N1 Li1 116.37(11) . . ? N1 C1 C6 121.08(13) . . ? N1 C1 C2 122.00(14) . . ? C6 C1 C2 116.76(13) . . ? C3 C2 C1 120.14(14) . . ? C3 C2 C8 120.86(13) . . ? C1 C2 C8 118.94(13) . . ? C4 C3 C2 122.59(14) . . ? C3 C4 C5 117.50(13) . . ? C3 C4 C7 121.15(13) . . ? C5 C4 C7 121.35(14) . . ? C6 C5 C4 121.88(15) . . ? C5 C6 C1 120.89(13) . . ? C5 C6 C21 121.74(14) . . ? C1 C6 C21 117.32(13) . . ? C9 C8 C2 113.13(13) . . ? C9 C8 C15 111.93(13) . . ? C2 C8 C15 111.78(12) . . ? C10 C9 C14 117.49(16) . . ? C10 C9 C8 123.01(14) . . ? C14 C9 C8 119.50(15) . . ? C9 C10 C11 121.21(15) . . ? C12 C11 C10 120.43(17) . . ? C13 C12 C11 119.22(17) . . ? C12 C13 C14 120.37(16) . . ? C13 C14 C9 121.26(17) . . ? C20 C15 C16 118.24(15) . . ? C20 C15 C8 119.10(14) . . ? C16 C15 C8 122.60(15) . . ? C17 C16 C15 120.66(17) . . ? C18 C17 C16 120.44(17) . . ? C17 C18 C19 119.43(16) . . ? C18 C19 C20 120.13(17) . . ? C19 C20 C15 121.10(16) . . ? C28 C21 C22 112.76(13) . . ? C28 C21 C6 111.11(12) . . ? C22 C21 C6 114.25(12) . . ? C27 C22 C23 117.89(14) . . ? C27 C22 C21 122.84(15) . . ? C23 C22 C21 119.26(14) . . ? C24 C23 C22 121.22(16) . . ? C25 C24 C23 120.19(16) . . ? C26 C25 C24 119.24(15) . . ? C25 C26 C27 120.52(16) . . ? C26 C27 C22 120.95(16) . . ? C33 C28 C29 117.81(15) . . ? C33 C28 C21 121.94(13) . . ? C29 C28 C21 120.25(14) . . ? C33 C28 Li1 80.48(12) . . ? C29 C28 Li1 80.12(11) . . ? C21 C28 Li1 108.85(12) . . ? C30 C29 C28 120.92(15) . . ? C30 C29 Li1 86.80(12) . . ? C28 C29 Li1 69.15(11) . . ? C31 C30 C29 120.48(15) . . ? C30 C31 C32 119.28(17) . . ? C33 C32 C31 120.24(16) . . ? C32 C33 C28 121.25(14) . . ? C32 C33 Li1 86.52(12) . . ? C28 C33 Li1 69.05(11) . . ? O1 C37 C38 106.14(16) . . ? C37 C38 C39 105.56(16) . . ? C40 C39 C38 103.49(19) . . ? O1 C40 C39 105.53(14) . . ? O1 Li1 N1 127.99(18) . . ? O1 Li1 C28 145.16(17) . . ? N1 Li1 C28 82.65(12) . . ? O1 Li1 C29 117.45(15) . . ? N1 Li1 C29 98.78(14) . . ? C28 Li1 C29 30.73(6) . . ? O1 Li1 C33 134.02(16) . . ? N1 Li1 C33 97.30(13) . . ? C28 Li1 C33 30.47(6) . . ? C29 Li1 C33 52.49(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.308 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.046 # Attachment '- ArNSiMe3NaTHF3.CIF' data_Ar*NSiMe3NaTHF3 _database_code_depnum_ccdc_archive 'CCDC 822596' #TrackingRef '- ArNSiMe3NaTHF3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H60 N Na O3 Si' _chemical_formula_weight 750.05 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' Na Na 0.0362 0.0249 '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 10.8967(7) _cell_length_b 11.1647(7) _cell_length_c 18.3301(12) _cell_angle_alpha 78.746(4) _cell_angle_beta 89.505(4) _cell_angle_gamma 75.339(4) _cell_volume 2114.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.959 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 40150 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9058 _reflns_number_gt 6151 _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. 3 CH2 fragments of one THF ligand (containing O3) were found to be disordered over two sites. This disorder was successfully modelled and the C atoms of both disordered sets refined aniosotropically. ; _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^)+(0.0607P)^2^+0.4876P] 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 9058 _refine_ls_number_parameters 519 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.83511(5) 0.67449(5) 0.35667(3) 0.02345(15) Uani 1 1 d . . . Na1 Na 1.09371(7) 0.74627(8) 0.26707(5) 0.0323(2) Uani 1 1 d . B . O1 O 1.20123(15) 0.71203(15) 0.38074(9) 0.0368(4) Uani 1 1 d . . . N1 N 0.87624(15) 0.76873(15) 0.28312(9) 0.0214(4) Uani 1 1 d . . . C1 C 0.80153(17) 0.86320(18) 0.23021(10) 0.0181(4) Uani 1 1 d . . . O2 O 1.19888(16) 0.57412(17) 0.21463(10) 0.0455(4) Uani 1 1 d . . . C2 C 0.78944(17) 0.84801(18) 0.15495(10) 0.0194(4) Uani 1 1 d . . . O3 O 1.23077(14) 0.86431(17) 0.20689(9) 0.0422(4) Uani 1 1 d D . . C3 C 0.72014(18) 0.94603(19) 0.10051(11) 0.0217(4) Uani 1 1 d . . . H3 H 0.7155 0.9325 0.0511 0.026 Uiso 1 1 calc R . . C4 C 0.65770(18) 1.06229(19) 0.11533(11) 0.0214(4) Uani 1 1 d . . . C5 C 0.66826(18) 1.07876(19) 0.18811(11) 0.0214(4) Uani 1 1 d . . . H5 H 0.6257 1.1575 0.2000 0.026 Uiso 1 1 calc R . . C6 C 0.73860(18) 0.98461(19) 0.24410(10) 0.0200(4) Uani 1 1 d . . . C7 C 0.5841(2) 1.1669(2) 0.05519(12) 0.0294(5) Uani 1 1 d . . . H7A H 0.5028 1.2073 0.0740 0.044 Uiso 1 1 calc R . . H7B H 0.5685 1.1320 0.0121 0.044 Uiso 1 1 calc R . . H7C H 0.6330 1.2296 0.0402 0.044 Uiso 1 1 calc R . . C8 C 0.85718(18) 0.72259(19) 0.13504(11) 0.0211(4) Uani 1 1 d . . . H8 H 0.9235 0.6802 0.1757 0.025 Uiso 1 1 calc R . . C9 C 0.77287(18) 0.63398(19) 0.13559(11) 0.0214(4) Uani 1 1 d . . . C10 C 0.6612(2) 0.6670(2) 0.09160(13) 0.0311(5) Uani 1 1 d . . . H10 H 0.6342 0.7496 0.0619 0.037 Uiso 1 1 calc R . . C11 C 0.5893(2) 0.5819(2) 0.09045(14) 0.0370(6) Uani 1 1 d . . . H11 H 0.5136 0.6062 0.0599 0.044 Uiso 1 1 calc R . . C12 C 0.6267(2) 0.4614(2) 0.13342(13) 0.0347(5) Uani 1 1 d . . . H12 H 0.5773 0.4027 0.1325 0.042 Uiso 1 1 calc R . . C13 C 0.7359(2) 0.4274(2) 0.17743(12) 0.0335(5) Uani 1 1 d . . . H13 H 0.7621 0.3449 0.2073 0.040 Uiso 1 1 calc R . . C14 C 0.8081(2) 0.51275(19) 0.17844(11) 0.0266(5) Uani 1 1 d . . . H14 H 0.8836 0.4878 0.2092 0.032 Uiso 1 1 calc R . . C15 C 0.92932(18) 0.73924(19) 0.06342(11) 0.0215(4) Uani 1 1 d . . . C16 C 1.0036(2) 0.8249(2) 0.05306(12) 0.0324(5) Uani 1 1 d . . . H16 H 1.0036 0.8761 0.0888 0.039 Uiso 1 1 calc R . . C17 C 1.0781(2) 0.8373(2) -0.00844(13) 0.0355(6) Uani 1 1 d . . . H17 H 1.1279 0.8969 -0.0144 0.043 Uiso 1 1 calc R . . C18 C 1.0802(2) 0.7640(2) -0.06060(12) 0.0340(5) Uani 1 1 d . . . H18 H 1.1325 0.7712 -0.1021 0.041 Uiso 1 1 calc R . . C19 C 1.0056(2) 0.6801(2) -0.05199(12) 0.0364(6) Uani 1 1 d . . . H19 H 1.0053 0.6300 -0.0884 0.044 Uiso 1 1 calc R . . C20 C 0.9307(2) 0.6676(2) 0.00931(12) 0.0296(5) Uani 1 1 d . . . H20 H 0.8796 0.6092 0.0143 0.036 Uiso 1 1 calc R . . C21 C 0.75699(18) 1.01270(19) 0.32091(11) 0.0226(4) Uani 1 1 d . . . H21 H 0.7759 0.9295 0.3565 0.027 Uiso 1 1 calc R . . C22 C 0.87121(19) 1.06572(19) 0.32652(12) 0.0249(5) Uani 1 1 d . . . C23 C 0.9068(2) 1.0857(2) 0.39512(13) 0.0386(6) Uani 1 1 d . . . H23 H 0.8607 1.0636 0.4377 0.046 Uiso 1 1 calc R . . C24 C 1.0077(2) 1.1371(3) 0.40250(16) 0.0487(7) Uani 1 1 d . . . H24 H 1.0294 1.1510 0.4497 0.058 Uiso 1 1 calc R . . C25 C 1.0766(2) 1.1682(2) 0.34199(17) 0.0464(7) Uani 1 1 d . . . H25 H 1.1455 1.2042 0.3470 0.056 Uiso 1 1 calc R . . C26 C 1.0451(2) 1.1468(2) 0.27383(15) 0.0445(6) Uani 1 1 d . . . H26 H 1.0928 1.1673 0.2318 0.053 Uiso 1 1 calc R . . C27 C 0.9438(2) 1.0953(2) 0.26680(13) 0.0334(5) Uani 1 1 d . . . H27 H 0.9237 1.0800 0.2197 0.040 Uiso 1 1 calc R . . C28 C 0.63707(19) 1.0938(2) 0.34685(11) 0.0243(5) Uani 1 1 d . . . C29 C 0.6125(2) 1.2244(2) 0.33645(12) 0.0320(5) Uani 1 1 d . . . H29 H 0.6734 1.2655 0.3133 0.038 Uiso 1 1 calc R . . C30 C 0.5008(2) 1.2961(2) 0.35920(13) 0.0383(6) Uani 1 1 d . . . H30 H 0.4846 1.3855 0.3503 0.046 Uiso 1 1 calc R . . C31 C 0.4132(2) 1.2374(2) 0.39470(13) 0.0408(6) Uani 1 1 d . . . H31 H 0.3376 1.2860 0.4114 0.049 Uiso 1 1 calc R . . C32 C 0.4361(2) 1.1089(2) 0.40566(14) 0.0410(6) Uani 1 1 d . . . H32 H 0.3757 1.0683 0.4298 0.049 Uiso 1 1 calc R . . C33 C 0.5468(2) 1.0376(2) 0.38182(12) 0.0326(5) Uani 1 1 d . . . H33 H 0.5610 0.9484 0.3896 0.039 Uiso 1 1 calc R . . C34 C 0.6701(2) 0.6571(2) 0.34568(14) 0.0386(6) Uani 1 1 d . . . H34A H 0.6097 0.7405 0.3376 0.058 Uiso 1 1 calc R . . H34B H 0.6495 0.6038 0.3908 0.058 Uiso 1 1 calc R . . H34C H 0.6646 0.6177 0.3029 0.058 Uiso 1 1 calc R . . C35 C 0.8449(2) 0.7206(2) 0.44994(12) 0.0377(6) Uani 1 1 d . . . H35A H 0.9235 0.7465 0.4544 0.056 Uiso 1 1 calc R . . H35B H 0.8444 0.6482 0.4899 0.056 Uiso 1 1 calc R . . H35C H 0.7718 0.7909 0.4539 0.056 Uiso 1 1 calc R . . C36 C 0.9487(2) 0.5142(2) 0.37285(12) 0.0352(5) Uani 1 1 d . . . H36A H 0.9395 0.4727 0.3315 0.053 Uiso 1 1 calc R . . H36B H 0.9302 0.4634 0.4196 0.053 Uiso 1 1 calc R . . H36C H 1.0357 0.5226 0.3760 0.053 Uiso 1 1 calc R . . C37 C 1.2023(3) 0.8201(2) 0.41155(15) 0.0472(7) Uani 1 1 d . . . H37A H 1.1297 0.8388 0.4440 0.057 Uiso 1 1 calc R . . H37B H 1.1969 0.8951 0.3715 0.057 Uiso 1 1 calc R . . C38 C 1.3254(2) 0.7864(2) 0.45572(14) 0.0403(6) Uani 1 1 d . . . H38A H 1.3959 0.8002 0.4235 0.048 Uiso 1 1 calc R . . H38B H 1.3200 0.8355 0.4957 0.048 Uiso 1 1 calc R . . C39 C 1.3407(3) 0.6498(3) 0.48690(18) 0.0624(9) Uani 1 1 d . . . H39A H 1.2939 0.6374 0.5331 0.075 Uiso 1 1 calc R . . H39B H 1.4314 0.6047 0.4976 0.075 Uiso 1 1 calc R . . C40 C 1.2847(3) 0.6053(2) 0.42549(18) 0.0678(10) Uani 1 1 d . . . H40A H 1.3530 0.5655 0.3952 0.081 Uiso 1 1 calc R . . H40B H 1.2379 0.5422 0.4468 0.081 Uiso 1 1 calc R . . C41 C 1.1903(3) 0.4475(3) 0.2307(2) 0.0670(9) Uani 1 1 d . . . H41A H 1.1009 0.4440 0.2260 0.080 Uiso 1 1 calc R . . H41B H 1.2235 0.4064 0.2820 0.080 Uiso 1 1 calc R . . C42 C 1.2695(3) 0.3817(3) 0.1747(2) 0.0669(9) Uani 1 1 d . . . H42A H 1.3560 0.3367 0.1957 0.080 Uiso 1 1 calc R . . H42B H 1.2291 0.3208 0.1583 0.080 Uiso 1 1 calc R . . C43 C 1.2729(3) 0.4892(3) 0.11174(16) 0.0566(8) Uani 1 1 d . . . H43A H 1.3486 0.4681 0.0818 0.068 Uiso 1 1 calc R . . H43B H 1.1954 0.5137 0.0788 0.068 Uiso 1 1 calc R . . C44 C 1.2792(3) 0.5896(3) 0.15264(15) 0.0551(8) Uani 1 1 d . . . H44A H 1.3675 0.5797 0.1703 0.066 Uiso 1 1 calc R . . H44B H 1.2481 0.6741 0.1203 0.066 Uiso 1 1 calc R . . C45 C 1.2231(2) 0.9601(3) 0.14064(16) 0.0485(7) Uani 1 1 d D B . H45A H 1.1463 1.0302 0.1402 0.058 Uiso 1 1 calc R A 1 H45B H 1.2189 0.9242 0.0957 0.058 Uiso 1 1 calc R A 1 C46 C 1.3415(12) 1.0074(13) 0.1418(8) 0.035(4) Uani 0.515(12) 1 d PD B 1 H46A H 1.3194 1.0997 0.1397 0.042 Uiso 0.515(12) 1 calc PR B 1 H46B H 1.3946 0.9884 0.0993 0.042 Uiso 0.515(12) 1 calc PR B 1 C48 C 1.3666(12) 0.8144(15) 0.2292(10) 0.053(4) Uani 0.515(12) 1 d PD B 1 H48A H 1.4110 0.7560 0.1975 0.063 Uiso 0.515(12) 1 calc PR B 1 H48B H 1.3790 0.7705 0.2820 0.063 Uiso 0.515(12) 1 calc PR B 1 C47A C 1.4332(5) 0.8894(7) 0.1840(4) 0.0365(18) Uani 0.485(12) 1 d PD B 2 H47A H 1.4599 0.8324 0.1484 0.044 Uiso 0.485(12) 1 calc PR B 2 H47B H 1.5090 0.9055 0.2056 0.044 Uiso 0.485(12) 1 calc PR B 2 C47 C 1.4110(7) 0.9344(8) 0.2167(4) 0.049(2) Uani 0.515(12) 1 d PD B 1 H47C H 1.5044 0.9163 0.2129 0.059 Uiso 0.515(12) 1 calc PR B 1 H47D H 1.3853 0.9817 0.2571 0.059 Uiso 0.515(12) 1 calc PR B 1 C48A C 1.3547(12) 0.8394(17) 0.2420(9) 0.045(3) Uani 0.485(12) 1 d PD B 2 H48C H 1.3901 0.7475 0.2601 0.054 Uiso 0.485(12) 1 calc PR B 2 H48D H 1.3505 0.8824 0.2847 0.054 Uiso 0.485(12) 1 calc PR B 2 C46A C 1.3379(14) 1.0116(16) 0.1481(12) 0.065(7) Uani 0.485(12) 1 d PD B 2 H46C H 1.3649 1.0492 0.0991 0.078 Uiso 0.485(12) 1 calc PR B 2 H46D H 1.3223 1.0745 0.1807 0.078 Uiso 0.485(12) 1 calc PR B 2 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 0.0257(3) 0.0241(3) 0.0179(3) 0.0003(2) 0.0015(2) -0.0048(2) Na1 0.0245(4) 0.0438(5) 0.0303(5) -0.0062(4) 0.0036(4) -0.0128(4) O1 0.0408(9) 0.0340(9) 0.0348(9) -0.0062(8) -0.0046(7) -0.0085(7) N1 0.0220(9) 0.0234(9) 0.0182(8) -0.0029(8) 0.0016(7) -0.0056(7) C1 0.0164(9) 0.0199(10) 0.0186(9) -0.0018(9) 0.0021(7) -0.0071(8) O2 0.0431(10) 0.0459(11) 0.0433(10) -0.0068(9) 0.0167(8) -0.0059(8) C2 0.0193(10) 0.0218(10) 0.0180(9) -0.0032(9) 0.0026(8) -0.0076(8) O3 0.0303(9) 0.0559(11) 0.0408(10) 0.0035(9) -0.0005(7) -0.0219(8) C3 0.0232(10) 0.0258(11) 0.0167(9) -0.0025(9) 0.0007(8) -0.0089(9) C4 0.0209(10) 0.0218(10) 0.0204(10) 0.0013(9) 0.0005(8) -0.0079(8) C5 0.0208(10) 0.0193(10) 0.0240(10) -0.0043(9) 0.0033(8) -0.0051(8) C6 0.0195(10) 0.0245(11) 0.0173(9) -0.0042(9) 0.0034(8) -0.0081(8) C7 0.0337(12) 0.0281(12) 0.0237(11) -0.0010(10) -0.0019(9) -0.0063(10) C8 0.0214(10) 0.0239(11) 0.0175(10) -0.0038(9) 0.0007(8) -0.0047(8) C9 0.0234(10) 0.0214(10) 0.0187(10) -0.0054(9) 0.0041(8) -0.0039(8) C10 0.0339(12) 0.0228(11) 0.0339(12) 0.0033(10) -0.0045(10) -0.0090(10) C11 0.0328(13) 0.0316(13) 0.0477(15) -0.0029(12) -0.0043(11) -0.0137(10) C12 0.0381(13) 0.0271(12) 0.0435(14) -0.0084(11) 0.0104(11) -0.0161(10) C13 0.0434(14) 0.0243(12) 0.0296(12) 0.0006(10) 0.0109(10) -0.0076(10) C14 0.0312(12) 0.0241(11) 0.0215(10) -0.0015(9) 0.0013(9) -0.0039(9) C15 0.0208(10) 0.0223(10) 0.0199(10) -0.0032(9) 0.0014(8) -0.0036(8) C16 0.0349(13) 0.0388(13) 0.0310(12) -0.0166(11) 0.0093(10) -0.0159(11) C17 0.0347(13) 0.0368(13) 0.0378(13) -0.0074(12) 0.0103(10) -0.0146(11) C18 0.0338(13) 0.0368(13) 0.0264(12) -0.0015(11) 0.0075(10) -0.0039(11) C19 0.0479(15) 0.0396(14) 0.0235(11) -0.0121(11) 0.0075(10) -0.0105(12) C20 0.0364(13) 0.0300(12) 0.0254(11) -0.0090(10) 0.0058(9) -0.0112(10) C21 0.0297(11) 0.0200(10) 0.0171(10) -0.0025(9) 0.0021(8) -0.0057(9) C22 0.0258(11) 0.0196(10) 0.0283(11) -0.0071(10) -0.0014(9) -0.0023(9) C23 0.0376(13) 0.0491(15) 0.0335(13) -0.0229(12) 0.0004(10) -0.0079(12) C24 0.0435(16) 0.0503(17) 0.0575(18) -0.0309(15) -0.0126(13) -0.0058(13) C25 0.0409(15) 0.0318(14) 0.0686(19) -0.0084(14) -0.0148(14) -0.0138(12) C26 0.0411(14) 0.0469(16) 0.0466(15) 0.0054(13) -0.0065(12) -0.0240(12) C27 0.0342(13) 0.0368(13) 0.0299(12) -0.0005(11) -0.0044(10) -0.0145(10) C28 0.0277(11) 0.0278(11) 0.0169(10) -0.0046(9) 0.0020(8) -0.0062(9) C29 0.0372(13) 0.0268(12) 0.0307(12) -0.0052(11) 0.0091(10) -0.0066(10) C30 0.0401(14) 0.0323(13) 0.0399(14) -0.0118(12) 0.0092(11) -0.0011(11) C31 0.0361(14) 0.0472(16) 0.0359(13) -0.0135(13) 0.0107(11) -0.0015(12) C32 0.0325(13) 0.0489(16) 0.0404(14) -0.0057(13) 0.0138(11) -0.0113(12) C33 0.0351(13) 0.0311(12) 0.0314(12) -0.0047(11) 0.0067(10) -0.0093(10) C34 0.0338(13) 0.0432(15) 0.0368(13) 0.0031(12) 0.0059(10) -0.0150(11) C35 0.0501(15) 0.0375(14) 0.0204(11) -0.0010(11) 0.0033(10) -0.0059(11) C36 0.0453(14) 0.0292(12) 0.0253(12) 0.0023(10) -0.0005(10) -0.0047(11) C37 0.0536(17) 0.0345(14) 0.0489(16) -0.0149(13) -0.0048(13) 0.0024(12) C38 0.0467(15) 0.0411(14) 0.0365(13) -0.0132(12) 0.0047(11) -0.0131(12) C39 0.074(2) 0.0438(17) 0.065(2) 0.0017(16) -0.0281(17) -0.0148(15) C40 0.097(3) 0.0277(14) 0.071(2) -0.0002(15) -0.0383(19) -0.0076(15) C41 0.0566(19) 0.0514(19) 0.083(2) 0.0004(18) 0.0258(17) -0.0081(15) C42 0.0555(19) 0.0472(18) 0.105(3) -0.028(2) 0.0277(18) -0.0179(15) C43 0.0441(16) 0.081(2) 0.0462(17) -0.0216(17) -0.0007(13) -0.0128(15) C44 0.0636(19) 0.0453(16) 0.0468(16) -0.0052(14) 0.0234(14) -0.0002(14) C45 0.0463(16) 0.0523(17) 0.0464(16) 0.0068(14) -0.0048(12) -0.0238(13) C46 0.045(9) 0.035(8) 0.031(5) -0.002(6) -0.001(5) -0.023(6) C48 0.029(4) 0.079(8) 0.051(7) -0.006(4) -0.003(4) -0.019(4) C47A 0.031(3) 0.046(4) 0.036(4) -0.004(3) 0.003(2) -0.019(3) C47 0.047(4) 0.068(5) 0.044(4) -0.009(4) 0.003(3) -0.038(3) C48A 0.040(5) 0.060(7) 0.033(5) 0.016(5) -0.004(4) -0.025(5) C46A 0.056(12) 0.061(13) 0.080(13) 0.010(10) 0.000(9) -0.035(10) _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 1.6733(18) . ? Si1 C36 1.871(2) . ? Si1 C34 1.874(2) . ? Si1 C35 1.890(2) . ? Na1 O1 2.3162(17) . ? Na1 N1 2.3411(18) . ? Na1 O2 2.3491(18) . ? Na1 O3 2.3632(18) . ? O1 C40 1.415(3) . ? O1 C37 1.431(3) . ? N1 C1 1.377(2) . ? C1 C6 1.426(3) . ? C1 C2 1.433(3) . ? O2 C41 1.414(3) . ? O2 C44 1.439(3) . ? C2 C3 1.390(3) . ? C2 C8 1.520(3) . ? O3 C45 1.440(3) . ? O3 C48A 1.438(13) . ? O3 C48 1.474(13) . ? C3 C4 1.382(3) . ? C3 H3 0.9500 . ? C4 C5 1.391(3) . ? C4 C7 1.504(3) . ? C5 C6 1.389(3) . ? C5 H5 0.9500 . ? C6 C21 1.526(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.510(3) . ? C8 C15 1.529(3) . ? C8 H8 1.0000 . ? C9 C14 1.387(3) . ? C9 C10 1.393(3) . ? C10 C11 1.380(3) . ? C10 H10 0.9500 . ? C11 C12 1.382(3) . ? C11 H11 0.9500 . ? C12 C13 1.371(3) . ? C12 H12 0.9500 . ? C13 C14 1.383(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.388(3) . ? C15 C16 1.387(3) . ? C16 C17 1.389(3) . ? C16 H16 0.9500 . ? C17 C18 1.371(3) . ? C17 H17 0.9500 . ? C18 C19 1.375(3) . ? C18 H18 0.9500 . ? C19 C20 1.389(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.520(3) . ? C21 C28 1.521(3) . ? C21 H21 1.0000 . ? C22 C27 1.382(3) . ? C22 C23 1.394(3) . ? C23 C24 1.381(3) . ? C23 H23 0.9500 . ? C24 C25 1.372(4) . ? C24 H24 0.9500 . ? C25 C26 1.379(4) . ? C25 H25 0.9500 . ? C26 C27 1.385(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.385(3) . ? C28 C29 1.389(3) . ? C29 C30 1.387(3) . ? C29 H29 0.9500 . ? C30 C31 1.379(3) . ? C30 H30 0.9500 . ? C31 C32 1.367(3) . ? C31 H31 0.9500 . ? C32 C33 1.386(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.497(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.488(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.506(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.515(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.502(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.480(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.515(12) . ? C45 C46A 1.521(14) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.547(13) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C48 C47 1.513(15) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C47A C48A 1.473(14) . ? C47A C46A 1.522(15) . ? C47A H47A 0.9900 . ? C47A H47B 0.9900 . ? C47 H47C 0.9900 . ? C47 H47D 0.9900 . ? C48A H48C 0.9900 . ? C48A H48D 0.9900 . ? C46A H46C 0.9900 . ? C46A H46D 0.9900 . ? 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 C36 110.24(10) . . ? N1 Si1 C34 112.71(10) . . ? C36 Si1 C34 108.82(11) . . ? N1 Si1 C35 116.42(10) . . ? C36 Si1 C35 101.71(10) . . ? C34 Si1 C35 106.19(11) . . ? O1 Na1 N1 110.68(7) . . ? O1 Na1 O2 103.88(7) . . ? N1 Na1 O2 115.76(7) . . ? O1 Na1 O3 91.80(6) . . ? N1 Na1 O3 139.08(7) . . ? O2 Na1 O3 89.61(7) . . ? C40 O1 C37 107.92(18) . . ? C40 O1 Na1 133.78(15) . . ? C37 O1 Na1 117.68(14) . . ? C1 N1 Si1 130.11(14) . . ? C1 N1 Na1 112.91(12) . . ? Si1 N1 Na1 116.93(9) . . ? N1 C1 C6 123.31(17) . . ? N1 C1 C2 121.29(16) . . ? C6 C1 C2 115.26(17) . . ? C41 O2 C44 108.7(2) . . ? C41 O2 Na1 129.71(16) . . ? C44 O2 Na1 121.44(16) . . ? C3 C2 C1 121.29(17) . . ? C3 C2 C8 120.20(17) . . ? C1 C2 C8 118.49(17) . . ? C45 O3 C48A 107.8(6) . . ? C45 O3 C48 106.5(6) . . ? C48A O3 C48 15.5(13) . . ? C45 O3 Na1 135.87(14) . . ? C48A O3 Na1 116.3(6) . . ? C48 O3 Na1 115.9(6) . . ? C4 C3 C2 122.64(18) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 116.88(18) . . ? C3 C4 C7 121.48(18) . . ? C5 C4 C7 121.63(18) . . ? C6 C5 C4 122.63(18) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C1 121.27(17) . . ? C5 C6 C21 120.04(17) . . ? C1 C6 C21 118.56(17) . . ? 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 . . ? C9 C8 C2 113.50(16) . . ? C9 C8 C15 112.82(16) . . ? C2 C8 C15 112.52(16) . . ? C9 C8 H8 105.7 . . ? C2 C8 H8 105.7 . . ? C15 C8 H8 105.7 . . ? C14 C9 C10 117.4(2) . . ? C14 C9 C8 120.17(18) . . ? C10 C9 C8 122.38(19) . . ? C11 C10 C9 121.1(2) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 120.4(2) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 119.3(2) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 120.2(2) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C9 121.5(2) . . ? C13 C14 H14 119.2 . . ? C9 C14 H14 119.2 . . ? C20 C15 C16 117.44(19) . . ? C20 C15 C8 123.41(19) . . ? C16 C15 C8 119.05(17) . . ? C15 C16 C17 121.4(2) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C18 C17 C16 120.4(2) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 119.1(2) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C18 C19 C20 120.7(2) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C15 C20 C19 121.0(2) . . ? C15 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C28 112.25(16) . . ? C22 C21 C6 112.64(16) . . ? C28 C21 C6 112.73(16) . . ? C22 C21 H21 106.2 . . ? C28 C21 H21 106.2 . . ? C6 C21 H21 106.2 . . ? C27 C22 C23 117.2(2) . . ? C27 C22 C21 123.50(18) . . ? C23 C22 C21 119.3(2) . . ? C24 C23 C22 121.3(2) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C25 C24 C23 120.3(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 119.5(2) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 119.9(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C22 C27 C26 121.7(2) . . ? C22 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C33 C28 C29 117.54(19) . . ? C33 C28 C21 119.84(19) . . ? C29 C28 C21 122.62(19) . . ? C28 C29 C30 121.2(2) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C31 C30 C29 120.0(2) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 119.5(2) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 120.5(2) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C28 C33 C32 121.2(2) . . ? C28 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O1 C37 C38 105.79(19) . . ? O1 C37 H37A 110.6 . . ? C38 C37 H37A 110.6 . . ? O1 C37 H37B 110.6 . . ? C38 C37 H37B 110.6 . . ? H37A C37 H37B 108.7 . . ? C39 C38 C37 101.7(2) . . ? C39 C38 H38A 111.4 . . ? C37 C38 H38A 111.4 . . ? C39 C38 H38B 111.4 . . ? C37 C38 H38B 111.4 . . ? H38A C38 H38B 109.3 . . ? C38 C39 C40 102.9(2) . . ? C38 C39 H39A 111.2 . . ? C40 C39 H39A 111.2 . . ? C38 C39 H39B 111.2 . . ? C40 C39 H39B 111.2 . . ? H39A C39 H39B 109.1 . . ? O1 C40 C39 107.7(2) . . ? O1 C40 H40A 110.2 . . ? C39 C40 H40A 110.2 . . ? O1 C40 H40B 110.2 . . ? C39 C40 H40B 110.2 . . ? H40A C40 H40B 108.5 . . ? O2 C41 C42 106.5(2) . . ? O2 C41 H41A 110.4 . . ? C42 C41 H41A 110.4 . . ? O2 C41 H41B 110.4 . . ? C42 C41 H41B 110.4 . . ? H41A C41 H41B 108.6 . . ? C43 C42 C41 102.9(2) . . ? C43 C42 H42A 111.2 . . ? C41 C42 H42A 111.2 . . ? C43 C42 H42B 111.2 . . ? C41 C42 H42B 111.2 . . ? H42A C42 H42B 109.1 . . ? C44 C43 C42 101.3(2) . . ? C44 C43 H43A 111.5 . . ? C42 C43 H43A 111.5 . . ? C44 C43 H43B 111.5 . . ? C42 C43 H43B 111.5 . . ? H43A C43 H43B 109.3 . . ? O2 C44 C43 105.4(2) . . ? O2 C44 H44A 110.7 . . ? C43 C44 H44A 110.7 . . ? O2 C44 H44B 110.7 . . ? C43 C44 H44B 110.7 . . ? H44A C44 H44B 108.8 . . ? O3 C45 C46 106.9(5) . . ? O3 C45 C46A 104.5(7) . . ? C46 C45 C46A 5.1(14) . . ? O3 C45 H45A 110.3 . . ? C46 C45 H45A 110.3 . . ? C46A C45 H45A 107.5 . . ? O3 C45 H45B 110.3 . . ? C46 C45 H45B 110.3 . . ? C46A C45 H45B 115.4 . . ? H45A C45 H45B 108.6 . . ? C45 C46 C47 103.9(9) . . ? C45 C46 H46A 111.0 . . ? C47 C46 H46A 111.0 . . ? C45 C46 H46B 111.0 . . ? C47 C46 H46B 111.0 . . ? H46A C46 H46B 109.0 . . ? O3 C48 C47 101.4(10) . . ? O3 C48 H48A 111.5 . . ? C47 C48 H48A 111.5 . . ? O3 C48 H48B 111.5 . . ? C47 C48 H48B 111.5 . . ? H48A C48 H48B 109.3 . . ? C48A C47A C46A 99.5(11) . . ? C48A C47A H47A 111.9 . . ? C46A C47A H47A 111.9 . . ? C48A C47A H47B 111.9 . . ? C46A C47A H47B 111.9 . . ? H47A C47A H47B 109.6 . . ? C48 C47 C46 101.9(9) . . ? C48 C47 H47C 111.4 . . ? C46 C47 H47C 111.4 . . ? C48 C47 H47D 111.4 . . ? C46 C47 H47D 111.4 . . ? H47C C47 H47D 109.2 . . ? O3 C48A C47A 105.5(10) . . ? O3 C48A H48C 110.6 . . ? C47A C48A H48C 110.6 . . ? O3 C48A H48D 110.6 . . ? C47A C48A H48D 110.6 . . ? H48C C48A H48D 108.8 . . ? C47A C46A C45 99.2(10) . . ? C47A C46A H46C 111.9 . . ? C45 C46A H46C 111.9 . . ? C47A C46A H46D 111.9 . . ? C45 C46A H46D 111.9 . . ? H46C C46A H46D 109.6 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.341 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.047 # Attachment '- ArNSiPh3KOEt2.CIF' data_Ar*NSiPh3KOEt2 _database_code_depnum_ccdc_archive 'CCDC 822597' #TrackingRef '- ArNSiPh3KOEt2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H52 K N O Si' _chemical_formula_weight 810.17 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.6752(4) _cell_length_b 12.6029(4) _cell_length_c 18.4402(7) _cell_angle_alpha 91.644(3) _cell_angle_beta 97.180(3) _cell_angle_gamma 114.573(3) _cell_volume 2229.57(14) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 0.186 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 15243 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10800 _reflns_number_gt 9994 _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. Two crystallofraphically independent molecules were located and refined in the asymmetric unit of the structure. There are no significant geometric differences between them. The crystal was found to be a racemic twin and the structure was refined with the TWIN and BASF commands of SHELXL. Attempts to solve the crystal structure in the centrosymmetric space group P-1 were not successful. ; _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^)+(0.0861P)^2^+0.2659P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.54(4) _refine_ls_number_reflns 10800 _refine_ls_number_parameters 1070 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.046 _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 K1 K 0.29725(9) 0.13587(7) 0.36136(5) 0.0320(2) Uani 1 1 d . . . Si1 Si 0.60045(10) 0.40896(8) 0.31950(5) 0.0224(2) Uani 1 1 d . . . O1 O 0.3044(3) -0.0726(2) 0.31415(18) 0.0395(7) Uani 1 1 d . . . N1 N 0.4583(3) 0.3622(2) 0.36099(16) 0.0211(6) Uani 1 1 d . . . C1 C 0.4254(4) 0.4445(3) 0.3957(2) 0.0219(8) Uani 1 1 d . . . K2 K 0.98928(9) 0.32446(7) 0.83080(5) 0.0353(2) Uani 1 1 d . . . Si2 Si 1.03744(10) 0.05592(8) 0.87727(5) 0.0230(2) Uani 1 1 d . . . O2 O 1.2246(3) 0.5340(2) 0.86404(17) 0.0396(7) Uani 1 1 d . . . N2 N 0.9202(3) 0.0973(3) 0.83391(16) 0.0239(7) Uani 1 1 d . . . C2 C 0.3363(4) 0.4901(3) 0.3579(2) 0.0224(8) Uani 1 1 d . . . C3 C 0.3237(4) 0.5847(3) 0.3890(2) 0.0233(8) Uani 1 1 d . . . H3 H 0.2665 0.6152 0.3616 0.028 Uiso 1 1 calc R . . C4 C 0.3904(4) 0.6380(3) 0.4584(2) 0.0255(8) Uani 1 1 d . . . C5 C 0.4624(4) 0.5837(3) 0.4990(2) 0.0252(8) Uani 1 1 d . . . H5 H 0.5027 0.6138 0.5483 0.030 Uiso 1 1 calc R . . C6 C 0.4776(4) 0.4878(3) 0.4706(2) 0.0220(8) Uani 1 1 d . . . C7 C 0.3840(5) 0.7479(4) 0.4885(2) 0.0341(9) Uani 1 1 d . . . H7A H 0.3476 0.7819 0.4487 0.051 Uiso 1 1 calc R . . H7B H 0.4777 0.8044 0.5103 0.051 Uiso 1 1 calc R . . H7C H 0.3226 0.7286 0.5261 0.051 Uiso 1 1 calc R . . C8 C 0.2611(4) 0.4302(3) 0.28181(19) 0.0208(7) Uani 1 1 d . . . H8 H 0.3329 0.4238 0.2543 0.025 Uiso 1 1 calc R . . C9 C 0.1521(4) 0.3050(3) 0.2859(2) 0.0245(8) Uani 1 1 d . . . C10 C 0.1089(4) 0.2240(3) 0.2260(2) 0.0305(9) Uani 1 1 d . . . H10 H 0.1491 0.2458 0.1825 0.037 Uiso 1 1 calc R . . C11 C 0.0074(4) 0.1108(4) 0.2276(3) 0.0393(11) Uani 1 1 d . . . H11 H -0.0212 0.0560 0.1857 0.047 Uiso 1 1 calc R . . C12 C -0.0514(5) 0.0785(4) 0.2905(3) 0.0417(11) Uani 1 1 d . . . H12 H -0.1203 0.0011 0.2921 0.050 Uiso 1 1 calc R . . C13 C -0.0107(5) 0.1574(4) 0.3500(3) 0.0391(11) Uani 1 1 d . . . H13 H -0.0518 0.1345 0.3931 0.047 Uiso 1 1 calc R . . C14 C 0.0901(4) 0.2710(3) 0.3491(2) 0.0289(9) Uani 1 1 d . . . H14 H 0.1169 0.3253 0.3912 0.035 Uiso 1 1 calc R . . C15 C 0.1927(4) 0.4941(3) 0.2360(2) 0.0262(8) Uani 1 1 d . . . C16 C 0.2556(5) 0.5560(4) 0.1797(2) 0.0374(10) Uani 1 1 d . . . H16 H 0.3467 0.5654 0.1739 0.045 Uiso 1 1 calc R . . C17 C 0.1878(6) 0.6040(4) 0.1320(3) 0.0496(13) Uani 1 1 d . . . H17 H 0.2316 0.6437 0.0928 0.059 Uiso 1 1 calc R . . C18 C 0.0583(6) 0.5954(4) 0.1402(3) 0.0518(13) Uani 1 1 d . . . H18 H 0.0118 0.6280 0.1068 0.062 Uiso 1 1 calc R . . C19 C -0.0035(5) 0.5385(4) 0.1980(3) 0.0475(12) Uani 1 1 d . . . H19 H -0.0922 0.5337 0.2052 0.057 Uiso 1 1 calc R . . C20 C 0.0621(4) 0.4893(3) 0.2447(3) 0.0341(9) Uani 1 1 d . . . H20 H 0.0180 0.4508 0.2841 0.041 Uiso 1 1 calc R . . C21 C 0.5524(4) 0.4259(3) 0.5156(2) 0.0238(8) Uani 1 1 d . . . H21 H 0.6249 0.4239 0.4868 0.029 Uiso 1 1 calc R . . C22 C 0.4557(4) 0.2973(3) 0.52252(19) 0.0245(8) Uani 1 1 d . . . C23 C 0.3136(4) 0.2600(4) 0.5228(2) 0.0305(9) Uani 1 1 d . . . H23 H 0.2735 0.3146 0.5191 0.037 Uiso 1 1 calc R . . C24 C 0.2294(5) 0.1413(4) 0.5286(2) 0.0361(10) Uani 1 1 d . . . H24 H 0.1322 0.1162 0.5284 0.043 Uiso 1 1 calc R . . C25 C 0.2853(5) 0.0613(4) 0.5345(2) 0.0394(10) Uani 1 1 d . . . H25 H 0.2272 -0.0189 0.5380 0.047 Uiso 1 1 calc R . . C26 C 0.4274(5) 0.0982(4) 0.5353(2) 0.0374(10) Uani 1 1 d . . . H26 H 0.4674 0.0436 0.5397 0.045 Uiso 1 1 calc R . . C27 C 0.5112(5) 0.2163(4) 0.5297(2) 0.0326(9) Uani 1 1 d . . . H27 H 0.6086 0.2414 0.5309 0.039 Uiso 1 1 calc R . . C28 C 0.6302(4) 0.4904(3) 0.5892(2) 0.0263(8) Uani 1 1 d . . . C29 C 0.5667(5) 0.4810(4) 0.6515(2) 0.0376(10) Uani 1 1 d . . . H29 H 0.4705 0.4310 0.6488 0.045 Uiso 1 1 calc R . . C30 C 0.6424(5) 0.5439(4) 0.7180(2) 0.0453(12) Uani 1 1 d . . . H30 H 0.5975 0.5379 0.7600 0.054 Uiso 1 1 calc R . . C31 C 0.7842(5) 0.6155(4) 0.7224(3) 0.0431(11) Uani 1 1 d . . . H31 H 0.8366 0.6579 0.7677 0.052 Uiso 1 1 calc R . . C32 C 0.8479(5) 0.6247(4) 0.6613(3) 0.0402(10) Uani 1 1 d . . . H32 H 0.9444 0.6740 0.6641 0.048 Uiso 1 1 calc R . . C33 C 0.7717(4) 0.5620(3) 0.5955(2) 0.0319(9) Uani 1 1 d . . . H33 H 0.8174 0.5682 0.5537 0.038 Uiso 1 1 calc R . . C34 C 0.5824(4) 0.2928(3) 0.2482(2) 0.0252(8) Uani 1 1 d . . . C35 C 0.4547(4) 0.2229(3) 0.2059(2) 0.0303(9) Uani 1 1 d . . . H35 H 0.3743 0.2320 0.2158 0.036 Uiso 1 1 calc R . . C36 C 0.4399(5) 0.1408(4) 0.1502(2) 0.0400(10) Uani 1 1 d . . . H36 H 0.3509 0.0943 0.1227 0.048 Uiso 1 1 calc R . . C37 C 0.5577(5) 0.1273(4) 0.1350(3) 0.0436(11) Uani 1 1 d . . . H37 H 0.5497 0.0722 0.0964 0.052 Uiso 1 1 calc R . . C38 C 0.6839(5) 0.1935(4) 0.1757(3) 0.0414(11) Uani 1 1 d . . . H38 H 0.7638 0.1838 0.1656 0.050 Uiso 1 1 calc R . . C39 C 0.6972(4) 0.2743(4) 0.2313(2) 0.0322(9) Uani 1 1 d . . . H39 H 0.7864 0.3189 0.2592 0.039 Uiso 1 1 calc R . . C40 C 0.7727(4) 0.4449(3) 0.3807(2) 0.0267(8) Uani 1 1 d . . . C41 C 0.7931(4) 0.3571(4) 0.4180(2) 0.0321(9) Uani 1 1 d . . . H41 H 0.7216 0.2795 0.4103 0.039 Uiso 1 1 calc R . . C42 C 0.9147(5) 0.3795(4) 0.4660(2) 0.0353(10) Uani 1 1 d . . . H42 H 0.9251 0.3182 0.4911 0.042 Uiso 1 1 calc R . . C43 C 1.0204(4) 0.4924(4) 0.4766(2) 0.0356(10) Uani 1 1 d . . . H43 H 1.1040 0.5089 0.5091 0.043 Uiso 1 1 calc R . . C44 C 1.0037(4) 0.5794(4) 0.4403(2) 0.0372(10) Uani 1 1 d . . . H44 H 1.0765 0.6564 0.4472 0.045 Uiso 1 1 calc R . . C45 C 0.8812(4) 0.5570(4) 0.3934(2) 0.0315(9) Uani 1 1 d . . . H45 H 0.8713 0.6194 0.3694 0.038 Uiso 1 1 calc R . . C46 C 0.6290(4) 0.5478(3) 0.2722(2) 0.0254(8) Uani 1 1 d . . . C47 C 0.6357(4) 0.6470(3) 0.3113(2) 0.0278(8) Uani 1 1 d . . . H47 H 0.6278 0.6445 0.3620 0.033 Uiso 1 1 calc R . . C48 C 0.6534(4) 0.7484(3) 0.2788(2) 0.0304(9) Uani 1 1 d . . . H48 H 0.6591 0.8148 0.3072 0.036 Uiso 1 1 calc R . . C49 C 0.6630(4) 0.7535(4) 0.2047(2) 0.0359(10) Uani 1 1 d . . . H49 H 0.6761 0.8234 0.1820 0.043 Uiso 1 1 calc R . . C50 C 0.6533(4) 0.6561(4) 0.1642(2) 0.0360(10) Uani 1 1 d . . . H50 H 0.6572 0.6584 0.1131 0.043 Uiso 1 1 calc R . . C51 C 0.6380(4) 0.5555(4) 0.1969(2) 0.0293(9) Uani 1 1 d . . . H51 H 0.6334 0.4900 0.1681 0.035 Uiso 1 1 calc R . . C52 C 0.4318(5) -0.0777(4) 0.3004(3) 0.0502(12) Uani 1 1 d . . . H52A H 0.4375 -0.0766 0.2472 0.060 Uiso 1 1 calc R . . H52B H 0.4349 -0.1508 0.3169 0.060 Uiso 1 1 calc R . . C53 C 0.5496(6) 0.0256(5) 0.3416(3) 0.0556(14) Uani 1 1 d . . . H53A H 0.5455 0.0974 0.3249 0.083 Uiso 1 1 calc R . . H53B H 0.6378 0.0245 0.3329 0.083 Uiso 1 1 calc R . . H53C H 0.5435 0.0233 0.3941 0.083 Uiso 1 1 calc R . . C54 C 0.1868(5) -0.1698(4) 0.2777(3) 0.0517(13) Uani 1 1 d . . . H54A H 0.1890 -0.2431 0.2942 0.062 Uiso 1 1 calc R . . H54B H 0.1888 -0.1708 0.2241 0.062 Uiso 1 1 calc R . . C55 C 0.0569(6) -0.1633(5) 0.2934(4) 0.0646(16) Uani 1 1 d . . . H55A H 0.0505 -0.1706 0.3457 0.097 Uiso 1 1 calc R . . H55B H -0.0238 -0.2272 0.2644 0.097 Uiso 1 1 calc R . . H55C H 0.0583 -0.0880 0.2805 0.097 Uiso 1 1 calc R . . C56 C 0.7938(4) 0.0157(3) 0.7975(2) 0.0221(8) Uani 1 1 d . . . C57 C 0.7731(4) -0.0252(3) 0.7224(2) 0.0220(8) Uani 1 1 d . . . C58 C 0.6523(4) -0.1183(3) 0.6908(2) 0.0256(8) Uani 1 1 d . . . H58 H 0.6436 -0.1459 0.6412 0.031 Uiso 1 1 calc R . . C59 C 0.5410(4) -0.1736(3) 0.7304(2) 0.0275(8) Uani 1 1 d . . . C60 C 0.5541(4) -0.1243(3) 0.8009(2) 0.0229(8) Uani 1 1 d . . . H60 H 0.4779 -0.1564 0.8274 0.028 Uiso 1 1 calc R . . C61 C 0.6737(4) -0.0304(3) 0.8337(2) 0.0224(8) Uani 1 1 d . . . C62 C 0.4132(4) -0.2797(4) 0.6968(2) 0.0319(9) Uani 1 1 d . . . H62A H 0.3597 -0.3183 0.7355 0.048 Uiso 1 1 calc R . . H62B H 0.4409 -0.3343 0.6717 0.048 Uiso 1 1 calc R . . H62C H 0.3556 -0.2558 0.6614 0.048 Uiso 1 1 calc R . . C63 C 0.8930(4) 0.0380(3) 0.67933(19) 0.0235(8) Uani 1 1 d . . . H63 H 0.9789 0.0393 0.7089 0.028 Uiso 1 1 calc R . . C64 C 0.9191(4) 0.1656(3) 0.6725(2) 0.0258(8) Uani 1 1 d . . . C65 C 1.0544(4) 0.2474(4) 0.6658(2) 0.0317(9) Uani 1 1 d . . . H65 H 1.1265 0.2220 0.6653 0.038 Uiso 1 1 calc R . . C66 C 1.0839(5) 0.3638(4) 0.6600(2) 0.0390(10) Uani 1 1 d . . . H66 H 1.1759 0.4179 0.6556 0.047 Uiso 1 1 calc R . . C67 C 0.9802(5) 0.4025(4) 0.6605(2) 0.0416(11) Uani 1 1 d . . . H67 H 1.0012 0.4831 0.6575 0.050 Uiso 1 1 calc R . . C68 C 0.8454(5) 0.3228(4) 0.6654(2) 0.0356(10) Uani 1 1 d . . . H68 H 0.7733 0.3486 0.6646 0.043 Uiso 1 1 calc R . . C69 C 0.8156(5) 0.2050(4) 0.6714(2) 0.0317(9) Uani 1 1 d . . . H69 H 0.7230 0.1510 0.6748 0.038 Uiso 1 1 calc R . . C70 C 0.8775(4) -0.0248(3) 0.6044(2) 0.0251(8) Uani 1 1 d . . . C71 C 0.8002(4) -0.0111(4) 0.5420(2) 0.0324(9) Uani 1 1 d . . . H71 H 0.7550 0.0395 0.5451 0.039 Uiso 1 1 calc R . . C72 C 0.7883(5) -0.0703(4) 0.4755(2) 0.0398(10) Uani 1 1 d . . . H72 H 0.7343 -0.0609 0.4333 0.048 Uiso 1 1 calc R . . C73 C 0.8548(4) -0.1432(4) 0.4702(2) 0.0344(10) Uani 1 1 d . . . H73 H 0.8468 -0.1837 0.4244 0.041 Uiso 1 1 calc R . . C74 C 0.9323(5) -0.1570(4) 0.5313(2) 0.0350(10) Uani 1 1 d . . . H74 H 0.9784 -0.2068 0.5279 0.042 Uiso 1 1 calc R . . C75 C 0.9431(4) -0.0976(3) 0.5984(2) 0.0290(9) Uani 1 1 d . . . H75 H 0.9967 -0.1075 0.6406 0.035 Uiso 1 1 calc R . . C76 C 0.6865(4) 0.0278(3) 0.9097(2) 0.0246(8) Uani 1 1 d . . . H76 H 0.7724 0.0297 0.9396 0.029 Uiso 1 1 calc R . . C77 C 0.7044(4) 0.1536(3) 0.9078(2) 0.0280(9) Uani 1 1 d . . . C78 C 0.6602(4) 0.1948(4) 0.8450(2) 0.0331(9) Uani 1 1 d . . . H78 H 0.6213 0.1443 0.8010 0.040 Uiso 1 1 calc R . . C79 C 0.6721(5) 0.3083(4) 0.8460(3) 0.0460(12) Uani 1 1 d . . . H79 H 0.6399 0.3344 0.8027 0.055 Uiso 1 1 calc R . . C80 C 0.7290(5) 0.3834(4) 0.9077(4) 0.0543(15) Uani 1 1 d . . . H80 H 0.7385 0.4618 0.9074 0.065 Uiso 1 1 calc R . . C81 C 0.7733(5) 0.3439(4) 0.9715(3) 0.0500(13) Uani 1 1 d . . . H81 H 0.8126 0.3952 1.0152 0.060 Uiso 1 1 calc R . . C82 C 0.7598(4) 0.2301(4) 0.9710(3) 0.0370(10) Uani 1 1 d . . . H82 H 0.7890 0.2035 1.0149 0.044 Uiso 1 1 calc R . . C83 C 0.5635(4) -0.0387(3) 0.9510(2) 0.0228(8) Uani 1 1 d . . . C84 C 0.4403(4) -0.0259(3) 0.9360(2) 0.0254(8) Uani 1 1 d . . . H84 H 0.4292 0.0188 0.8971 0.030 Uiso 1 1 calc R . . C85 C 0.3332(4) -0.0770(3) 0.9766(2) 0.0296(9) Uani 1 1 d . . . H85 H 0.2496 -0.0670 0.9660 0.035 Uiso 1 1 calc R . . C86 C 0.3488(4) -0.1424(4) 1.0324(2) 0.0345(10) Uani 1 1 d . . . H86 H 0.2769 -0.1756 1.0616 0.041 Uiso 1 1 calc R . . C87 C 0.4684(5) -0.1601(4) 1.0462(2) 0.0358(10) Uani 1 1 d . . . H87 H 0.4775 -0.2074 1.0838 0.043 Uiso 1 1 calc R . . C88 C 0.5753(4) -0.1088(3) 1.0051(2) 0.0306(9) Uani 1 1 d . . . H88 H 0.6570 -0.1220 1.0143 0.037 Uiso 1 1 calc R . . C89 C 1.1609(4) 0.1795(3) 0.9455(2) 0.0266(8) Uani 1 1 d . . . C90 C 1.1085(4) 0.2467(4) 0.9831(2) 0.0310(9) Uani 1 1 d . . . H90 H 1.0115 0.2268 0.9738 0.037 Uiso 1 1 calc R . . C91 C 1.1921(5) 0.3404(4) 1.0331(2) 0.0417(11) Uani 1 1 d . . . H91 H 1.1534 0.3851 1.0568 0.050 Uiso 1 1 calc R . . C92 C 1.3340(5) 0.3689(4) 1.0487(3) 0.0439(11) Uani 1 1 d . . . H92 H 1.3929 0.4331 1.0833 0.053 Uiso 1 1 calc R . . C93 C 1.3879(5) 0.3039(4) 1.0139(3) 0.0430(11) Uani 1 1 d . . . H93 H 1.4845 0.3229 1.0250 0.052 Uiso 1 1 calc R . . C94 C 1.3047(4) 0.2112(4) 0.9629(2) 0.0324(9) Uani 1 1 d . . . H94 H 1.3451 0.1681 0.9391 0.039 Uiso 1 1 calc R . . C95 C 0.9553(4) -0.0779(3) 0.9291(2) 0.0278(9) Uani 1 1 d . . . C96 C 0.8469(4) -0.1807(3) 0.8917(2) 0.0314(9) Uani 1 1 d . . . H96 H 0.8145 -0.1806 0.8414 0.038 Uiso 1 1 calc R . . C97 C 0.7867(5) -0.2817(4) 0.9268(3) 0.0371(10) Uani 1 1 d . . . H97 H 0.7149 -0.3501 0.9002 0.044 Uiso 1 1 calc R . . C98 C 0.8309(5) -0.2829(4) 0.9999(3) 0.0471(13) Uani 1 1 d . . . H98 H 0.7905 -0.3526 1.0237 0.057 Uiso 1 1 calc R . . C99 C 0.9341(5) -0.1829(4) 1.0390(3) 0.0444(12) Uani 1 1 d . . . H99 H 0.9632 -0.1830 1.0898 0.053 Uiso 1 1 calc R . . C100 C 0.9954(5) -0.0815(4) 1.0031(2) 0.0348(10) Uani 1 1 d . . . H100 H 1.0665 -0.0133 1.0302 0.042 Uiso 1 1 calc R . . C101 C 1.1478(4) 0.0177(3) 0.8168(2) 0.0255(8) Uani 1 1 d . . . C102 C 1.2435(4) 0.1071(4) 0.7809(2) 0.0318(9) Uani 1 1 d . . . H102 H 1.2562 0.1857 0.7900 0.038 Uiso 1 1 calc R . . C103 C 1.3190(4) 0.0818(4) 0.7327(2) 0.0356(10) Uani 1 1 d . . . H103 H 1.3818 0.1430 0.7088 0.043 Uiso 1 1 calc R . . C104 C 1.3040(5) -0.0303(4) 0.7191(2) 0.0353(10) Uani 1 1 d . . . H104 H 1.3561 -0.0469 0.6860 0.042 Uiso 1 1 calc R . . C105 C 1.2125(4) -0.1196(4) 0.7539(2) 0.0330(9) Uani 1 1 d . . . H105 H 1.2023 -0.1976 0.7451 0.040 Uiso 1 1 calc R . . C106 C 1.1351(4) -0.0948(4) 0.8020(2) 0.0288(8) Uani 1 1 d . . . H106 H 1.0719 -0.1569 0.8251 0.035 Uiso 1 1 calc R . . C107 C 1.3651(5) 0.5429(4) 0.8759(3) 0.0457(11) Uani 1 1 d . . . H10A H 1.3984 0.5496 0.9291 0.055 Uiso 1 1 calc R . . H10B H 1.4282 0.6134 0.8549 0.055 Uiso 1 1 calc R . . C108 C 1.3642(6) 0.4368(5) 0.8399(3) 0.0583(14) Uani 1 1 d . . . H10C H 1.2969 0.3674 0.8588 0.087 Uiso 1 1 calc R . . H10D H 1.4574 0.4385 0.8501 0.087 Uiso 1 1 calc R . . H10E H 1.3378 0.4340 0.7868 0.087 Uiso 1 1 calc R . . C109 C 1.2169(5) 0.6313(4) 0.8985(3) 0.0515(13) Uani 1 1 d . . . H10F H 1.2717 0.7028 0.8754 0.062 Uiso 1 1 calc R . . H10G H 1.2571 0.6418 0.9510 0.062 Uiso 1 1 calc R . . C110 C 1.0694(6) 0.6140(5) 0.8917(4) 0.0693(18) Uani 1 1 d . . . H11A H 1.0291 0.6013 0.8397 0.104 Uiso 1 1 calc R . . H11B H 1.0652 0.6837 0.9141 0.104 Uiso 1 1 calc R . . H11C H 1.0165 0.5456 0.9168 0.104 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 K1 0.0292(5) 0.0227(4) 0.0395(5) 0.0022(4) 0.0052(4) 0.0064(4) Si1 0.0168(5) 0.0224(5) 0.0238(5) -0.0001(4) 0.0040(4) 0.0041(4) O1 0.0306(17) 0.0254(15) 0.062(2) 0.0005(14) 0.0091(15) 0.0106(14) N1 0.0155(16) 0.0154(14) 0.0287(16) 0.0003(12) 0.0038(13) 0.0027(13) C1 0.0141(18) 0.0189(18) 0.0260(19) 0.0041(15) 0.0064(15) -0.0006(15) K2 0.0319(5) 0.0269(5) 0.0408(5) 0.0022(4) 0.0030(4) 0.0070(4) Si2 0.0192(5) 0.0242(5) 0.0245(5) 0.0027(4) 0.0037(4) 0.0080(5) O2 0.0313(17) 0.0300(16) 0.0508(19) -0.0002(14) 0.0065(14) 0.0064(14) N2 0.0233(17) 0.0218(16) 0.0246(16) 0.0025(13) 0.0040(14) 0.0075(14) C2 0.0134(18) 0.0237(19) 0.0244(19) 0.0063(15) 0.0069(15) 0.0010(16) C3 0.0149(19) 0.0225(19) 0.030(2) 0.0039(16) 0.0040(16) 0.0055(16) C4 0.020(2) 0.0253(19) 0.028(2) 0.0032(16) 0.0067(16) 0.0050(17) C5 0.019(2) 0.027(2) 0.0239(19) 0.0010(16) 0.0076(16) 0.0035(17) C6 0.0184(19) 0.0194(18) 0.0271(19) 0.0059(15) 0.0086(15) 0.0052(16) C7 0.028(2) 0.033(2) 0.037(2) -0.0038(18) -0.0011(18) 0.011(2) C8 0.0149(18) 0.0192(18) 0.0241(19) 0.0003(15) 0.0052(15) 0.0026(15) C9 0.0186(19) 0.0195(18) 0.036(2) 0.0052(16) 0.0043(16) 0.0088(17) C10 0.022(2) 0.027(2) 0.038(2) -0.0006(18) 0.0014(17) 0.0076(18) C11 0.028(2) 0.024(2) 0.057(3) -0.012(2) -0.006(2) 0.007(2) C12 0.020(2) 0.026(2) 0.072(3) 0.002(2) 0.005(2) 0.0032(19) C13 0.028(2) 0.026(2) 0.059(3) 0.011(2) 0.013(2) 0.005(2) C14 0.021(2) 0.024(2) 0.037(2) 0.0019(17) 0.0052(17) 0.0043(17) C15 0.022(2) 0.0189(18) 0.031(2) -0.0006(16) 0.0015(16) 0.0036(17) C16 0.042(3) 0.027(2) 0.041(2) 0.0086(19) 0.015(2) 0.010(2) C17 0.075(4) 0.038(3) 0.037(3) 0.015(2) 0.011(3) 0.023(3) C18 0.066(4) 0.033(3) 0.048(3) 0.000(2) -0.021(3) 0.021(3) C19 0.029(3) 0.030(2) 0.073(3) 0.005(2) -0.014(2) 0.009(2) C20 0.020(2) 0.026(2) 0.053(3) 0.0122(19) 0.0062(19) 0.0052(18) C21 0.0190(19) 0.0228(19) 0.0263(19) 0.0033(15) 0.0053(16) 0.0050(16) C22 0.025(2) 0.026(2) 0.0200(19) 0.0030(15) 0.0034(16) 0.0081(18) C23 0.027(2) 0.032(2) 0.030(2) 0.0059(17) 0.0067(17) 0.0096(19) C24 0.029(2) 0.039(2) 0.033(2) 0.0078(19) 0.0081(18) 0.007(2) C25 0.041(3) 0.031(2) 0.035(2) 0.0073(19) 0.007(2) 0.004(2) C26 0.043(3) 0.030(2) 0.040(2) 0.0099(19) 0.007(2) 0.015(2) C27 0.030(2) 0.031(2) 0.033(2) 0.0026(18) 0.0043(18) 0.0101(19) C28 0.034(2) 0.0209(19) 0.027(2) 0.0048(15) 0.0062(17) 0.0134(18) C29 0.034(3) 0.048(3) 0.031(2) -0.0006(19) 0.0048(19) 0.019(2) C30 0.054(3) 0.063(3) 0.025(2) 0.003(2) 0.005(2) 0.031(3) C31 0.055(3) 0.036(3) 0.035(2) -0.002(2) -0.006(2) 0.020(3) C32 0.038(3) 0.030(2) 0.044(3) 0.0029(19) -0.002(2) 0.007(2) C33 0.030(2) 0.028(2) 0.033(2) 0.0060(18) 0.0073(18) 0.0065(19) C34 0.023(2) 0.0244(19) 0.027(2) 0.0056(16) 0.0067(16) 0.0078(17) C35 0.026(2) 0.029(2) 0.032(2) -0.0011(17) 0.0018(17) 0.0092(19) C36 0.034(3) 0.040(2) 0.036(2) -0.0081(19) -0.002(2) 0.009(2) C37 0.045(3) 0.045(3) 0.043(3) -0.009(2) 0.007(2) 0.021(2) C38 0.037(3) 0.048(3) 0.044(3) -0.003(2) 0.012(2) 0.021(2) C39 0.024(2) 0.035(2) 0.035(2) -0.0036(18) 0.0066(18) 0.0095(19) C40 0.019(2) 0.032(2) 0.025(2) -0.0022(16) 0.0052(16) 0.0072(18) C41 0.024(2) 0.033(2) 0.035(2) -0.0041(18) 0.0031(18) 0.0085(19) C42 0.034(2) 0.048(3) 0.028(2) 0.0027(19) 0.0025(18) 0.022(2) C43 0.022(2) 0.053(3) 0.028(2) -0.0050(19) -0.0049(17) 0.015(2) C44 0.020(2) 0.041(2) 0.040(2) -0.004(2) 0.0033(19) 0.004(2) C45 0.024(2) 0.035(2) 0.031(2) 0.0001(17) 0.0040(17) 0.0082(19) C46 0.0116(18) 0.028(2) 0.028(2) 0.0062(16) 0.0004(15) 0.0011(16) C47 0.0165(19) 0.028(2) 0.030(2) 0.0020(17) 0.0031(16) 0.0005(17) C48 0.020(2) 0.024(2) 0.040(2) 0.0014(17) 0.0028(17) 0.0024(17) C49 0.022(2) 0.031(2) 0.044(3) 0.012(2) 0.0028(19) 0.0013(19) C50 0.026(2) 0.047(3) 0.029(2) 0.013(2) 0.0083(18) 0.008(2) C51 0.021(2) 0.034(2) 0.027(2) -0.0011(17) 0.0032(17) 0.0061(19) C52 0.043(3) 0.045(3) 0.069(3) 0.005(2) 0.019(3) 0.022(3) C53 0.037(3) 0.044(3) 0.083(4) 0.018(3) 0.009(3) 0.014(3) C54 0.043(3) 0.034(3) 0.067(3) -0.011(2) -0.002(3) 0.010(2) C55 0.034(3) 0.041(3) 0.111(5) 0.010(3) 0.008(3) 0.010(3) C56 0.023(2) 0.0172(18) 0.0271(19) 0.0028(15) 0.0027(16) 0.0093(16) C57 0.022(2) 0.0195(18) 0.0248(19) 0.0040(15) 0.0012(16) 0.0091(17) C58 0.023(2) 0.027(2) 0.0253(19) 0.0005(16) 0.0062(16) 0.0089(18) C59 0.023(2) 0.025(2) 0.032(2) 0.0012(16) 0.0052(17) 0.0078(18) C60 0.0174(19) 0.0223(18) 0.027(2) 0.0059(15) 0.0064(16) 0.0056(16) C61 0.022(2) 0.0227(19) 0.0251(19) 0.0017(15) 0.0023(16) 0.0118(17) C62 0.024(2) 0.033(2) 0.033(2) -0.0053(18) 0.0042(18) 0.0073(19) C63 0.0153(19) 0.027(2) 0.0233(19) 0.0047(15) 0.0010(15) 0.0047(17) C64 0.028(2) 0.027(2) 0.0189(18) 0.0021(15) 0.0012(16) 0.0097(18) C65 0.029(2) 0.032(2) 0.030(2) 0.0049(17) 0.0048(18) 0.0078(19) C66 0.036(3) 0.034(2) 0.039(2) 0.008(2) 0.004(2) 0.006(2) C67 0.050(3) 0.029(2) 0.039(3) 0.0051(19) 0.002(2) 0.011(2) C68 0.040(3) 0.034(2) 0.037(2) 0.0042(19) 0.002(2) 0.020(2) C69 0.032(2) 0.034(2) 0.026(2) 0.0042(17) 0.0019(18) 0.012(2) C70 0.019(2) 0.0230(19) 0.0269(19) 0.0055(16) 0.0083(16) 0.0016(16) C71 0.026(2) 0.038(2) 0.032(2) 0.0019(18) 0.0045(18) 0.011(2) C72 0.032(2) 0.051(3) 0.028(2) 0.0037(19) 0.0020(19) 0.010(2) C73 0.031(2) 0.030(2) 0.030(2) -0.0009(18) 0.0100(19) 0.000(2) C74 0.036(2) 0.026(2) 0.041(2) 0.0007(18) 0.012(2) 0.009(2) C75 0.029(2) 0.0199(19) 0.031(2) 0.0036(16) 0.0050(17) 0.0036(18) C76 0.0200(19) 0.029(2) 0.0263(19) 0.0003(16) 0.0045(16) 0.0117(17) C77 0.0131(19) 0.024(2) 0.043(2) 0.0005(18) 0.0098(17) 0.0029(17) C78 0.022(2) 0.031(2) 0.050(3) 0.0072(19) 0.0117(19) 0.0117(19) C79 0.035(3) 0.028(2) 0.078(4) 0.014(2) 0.022(3) 0.012(2) C80 0.031(3) 0.023(2) 0.111(5) 0.005(3) 0.026(3) 0.009(2) C81 0.028(3) 0.028(2) 0.084(4) -0.018(2) 0.014(3) 0.003(2) C82 0.025(2) 0.033(2) 0.049(3) -0.004(2) 0.011(2) 0.008(2) C83 0.0201(19) 0.0223(19) 0.0249(19) -0.0022(15) 0.0036(15) 0.0081(17) C84 0.026(2) 0.0242(19) 0.026(2) 0.0027(16) 0.0071(16) 0.0104(17) C85 0.020(2) 0.030(2) 0.040(2) 0.0048(18) 0.0105(18) 0.0107(18) C86 0.029(2) 0.036(2) 0.035(2) 0.0078(19) 0.0127(19) 0.008(2) C87 0.039(3) 0.033(2) 0.034(2) 0.0116(18) 0.0074(19) 0.013(2) C88 0.023(2) 0.033(2) 0.035(2) 0.0002(18) -0.0010(17) 0.0134(19) C89 0.024(2) 0.025(2) 0.028(2) 0.0082(16) 0.0019(16) 0.0071(18) C90 0.026(2) 0.034(2) 0.028(2) -0.0024(17) 0.0014(17) 0.0091(19) C91 0.042(3) 0.046(3) 0.035(2) -0.006(2) 0.002(2) 0.018(2) C92 0.036(3) 0.038(3) 0.041(3) -0.010(2) -0.008(2) 0.003(2) C93 0.026(2) 0.046(3) 0.048(3) 0.001(2) -0.003(2) 0.010(2) C94 0.026(2) 0.036(2) 0.032(2) 0.0019(18) -0.0001(18) 0.012(2) C95 0.023(2) 0.030(2) 0.038(2) 0.0092(18) 0.0156(18) 0.0157(18) C96 0.029(2) 0.029(2) 0.041(2) 0.0055(18) 0.0077(19) 0.0154(19) C97 0.033(2) 0.027(2) 0.056(3) 0.008(2) 0.020(2) 0.014(2) C98 0.050(3) 0.036(3) 0.068(3) 0.025(2) 0.034(3) 0.022(3) C99 0.054(3) 0.058(3) 0.036(2) 0.022(2) 0.023(2) 0.033(3) C100 0.031(2) 0.044(3) 0.034(2) 0.0076(19) 0.0096(19) 0.018(2) C101 0.0169(19) 0.035(2) 0.0224(19) 0.0019(16) -0.0015(15) 0.0103(18) C102 0.025(2) 0.038(2) 0.033(2) 0.0068(18) 0.0061(18) 0.013(2) C103 0.024(2) 0.052(3) 0.031(2) 0.014(2) 0.0102(18) 0.014(2) C104 0.032(2) 0.056(3) 0.026(2) 0.0011(19) 0.0046(18) 0.026(2) C105 0.026(2) 0.040(2) 0.035(2) -0.0007(19) 0.0012(18) 0.018(2) C106 0.022(2) 0.035(2) 0.027(2) 0.0028(17) 0.0011(16) 0.0111(19) C107 0.035(3) 0.047(3) 0.048(3) 0.012(2) 0.005(2) 0.011(2) C108 0.047(3) 0.047(3) 0.085(4) 0.016(3) 0.016(3) 0.021(3) C109 0.040(3) 0.030(2) 0.072(4) -0.003(2) 0.015(3) 0.001(2) C110 0.045(3) 0.041(3) 0.120(5) -0.001(3) 0.019(3) 0.014(3) _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 K1 N1 2.649(3) . ? K1 O1 2.778(3) . ? Si1 N1 1.675(3) . ? Si1 C34 1.872(4) . ? Si1 C40 1.903(4) . ? Si1 C46 1.904(4) . ? O1 C54 1.411(6) . ? O1 C52 1.441(5) . ? N1 C1 1.390(5) . ? C1 C6 1.422(5) . ? C1 C2 1.426(5) . ? K2 N2 2.647(3) . ? K2 O2 2.769(3) . ? Si2 N2 1.671(3) . ? Si2 C89 1.874(4) . ? Si2 C95 1.898(4) . ? Si2 C101 1.906(4) . ? O2 C109 1.402(5) . ? O2 C107 1.444(6) . ? N2 C56 1.381(5) . ? C2 C3 1.372(5) . ? C2 C8 1.528(5) . ? C3 C4 1.386(6) . ? C3 H3 0.9500 . ? C4 C5 1.395(5) . ? C4 C7 1.508(5) . ? C5 C6 1.382(5) . ? C5 H5 0.9500 . ? C6 C21 1.525(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C15 1.506(5) . ? C8 C9 1.534(5) . ? C8 H8 1.0000 . ? C9 C10 1.376(6) . ? C9 C14 1.403(5) . ? C10 C11 1.391(6) . ? C10 H10 0.9500 . ? C11 C12 1.378(7) . ? C11 H11 0.9500 . ? C12 C13 1.357(7) . ? C12 H12 0.9500 . ? C13 C14 1.390(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.386(6) . ? C15 C20 1.400(5) . ? C16 C17 1.379(7) . ? C16 H16 0.9500 . ? C17 C18 1.369(8) . ? C17 H17 0.9500 . ? C18 C19 1.382(8) . ? C18 H18 0.9500 . ? C19 C20 1.362(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C28 1.512(6) . ? C21 C22 1.536(5) . ? C21 H21 1.0000 . ? C22 C27 1.379(5) . ? C22 C23 1.390(6) . ? C23 C24 1.403(6) . ? C23 H23 0.9500 . ? C24 C25 1.370(6) . ? C24 H24 0.9500 . ? C25 C26 1.387(7) . ? C25 H25 0.9500 . ? C26 C27 1.396(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.388(5) . ? C28 C33 1.388(6) . ? C29 C30 1.397(6) . ? C29 H29 0.9500 . ? C30 C31 1.393(7) . ? C30 H30 0.9500 . ? C31 C32 1.371(6) . ? C31 H31 0.9500 . ? C32 C33 1.387(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.392(6) . ? C34 C39 1.407(5) . ? C35 C36 1.384(6) . ? C35 H35 0.9500 . ? C36 C37 1.397(6) . ? C36 H36 0.9500 . ? C37 C38 1.361(7) . ? C37 H37 0.9500 . ? C38 C39 1.376(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.396(6) . ? C40 C45 1.395(6) . ? C41 C42 1.394(6) . ? C41 H41 0.9500 . ? C42 C43 1.390(6) . ? C42 H42 0.9500 . ? C43 C44 1.364(6) . ? C43 H43 0.9500 . ? C44 C45 1.391(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.396(5) . ? C46 C51 1.407(5) . ? C47 C48 1.379(6) . ? C47 H47 0.9500 . ? C48 C49 1.384(6) . ? C48 H48 0.9500 . ? C49 C50 1.378(6) . ? C49 H49 0.9500 . ? C50 C51 1.376(6) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.482(8) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.485(7) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.422(5) . ? C56 C61 1.429(5) . ? C57 C58 1.376(6) . ? C57 C63 1.532(5) . ? C58 C59 1.410(5) . ? C58 H58 0.9500 . ? C59 C60 1.389(5) . ? C59 C62 1.503(6) . ? C60 C61 1.381(5) . ? C60 H60 0.9500 . ? C61 C76 1.526(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.526(5) . ? C63 C70 1.528(5) . ? C63 H63 1.0000 . ? C64 C69 1.385(5) . ? C64 C65 1.407(6) . ? C65 C66 1.377(6) . ? C65 H65 0.9500 . ? C66 C67 1.384(6) . ? C66 H66 0.9500 . ? C67 C68 1.386(7) . ? C67 H67 0.9500 . ? C68 C69 1.394(6) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C75 1.376(5) . ? C70 C71 1.388(6) . ? C71 C72 1.380(6) . ? C71 H71 0.9500 . ? C72 C73 1.383(6) . ? C72 H72 0.9500 . ? C73 C74 1.372(6) . ? C73 H73 0.9500 . ? C74 C75 1.393(6) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C77 1.518(5) . ? C76 C83 1.543(5) . ? C76 H76 1.0000 . ? C77 C82 1.388(6) . ? C77 C78 1.391(6) . ? C78 C79 1.383(6) . ? C78 H78 0.9500 . ? C79 C80 1.359(8) . ? C79 H79 0.9500 . ? C80 C81 1.395(8) . ? C80 H80 0.9500 . ? C81 C82 1.381(6) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C88 1.380(5) . ? C83 C84 1.385(5) . ? C84 C85 1.383(5) . ? C84 H84 0.9500 . ? C85 C86 1.373(6) . ? C85 H85 0.9500 . ? C86 C87 1.380(6) . ? C86 H86 0.9500 . ? C87 C88 1.388(6) . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? C89 C90 1.403(5) . ? C89 C94 1.407(6) . ? C90 C91 1.377(6) . ? C90 H90 0.9500 . ? C91 C92 1.393(7) . ? C91 H91 0.9500 . ? C92 C93 1.367(6) . ? C92 H92 0.9500 . ? C93 C94 1.380(6) . ? C93 H93 0.9500 . ? C94 H94 0.9500 . ? C95 C100 1.385(6) . ? C95 C96 1.413(6) . ? C96 C97 1.386(6) . ? C96 H96 0.9500 . ? C97 C98 1.375(7) . ? C97 H97 0.9500 . ? C98 C99 1.385(8) . ? C98 H98 0.9500 . ? C99 C100 1.400(6) . ? C99 H99 0.9500 . ? C100 H100 0.9500 . ? C101 C106 1.383(6) . ? C101 C102 1.417(6) . ? C102 C103 1.384(5) . ? C102 H102 0.9500 . ? C103 C104 1.366(6) . ? C103 H103 0.9500 . ? C104 C105 1.384(6) . ? C104 H104 0.9500 . ? C105 C106 1.395(5) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 C108 1.471(7) . ? C107 H10A 0.9900 . ? C107 H10B 0.9900 . ? C108 H10C 0.9800 . ? C108 H10D 0.9800 . ? C108 H10E 0.9800 . ? C109 C110 1.486(8) . ? C109 H10F 0.9900 . ? C109 H10G 0.9900 . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 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 K1 O1 136.17(9) . . ? N1 Si1 C34 109.43(16) . . ? N1 Si1 C40 116.24(16) . . ? C34 Si1 C40 105.50(17) . . ? N1 Si1 C46 112.67(15) . . ? C34 Si1 C46 107.81(16) . . ? C40 Si1 C46 104.64(17) . . ? C54 O1 C52 111.2(3) . . ? C54 O1 K1 123.5(3) . . ? C52 O1 K1 121.8(3) . . ? C1 N1 Si1 118.8(2) . . ? C1 N1 K1 119.9(2) . . ? Si1 N1 K1 121.27(14) . . ? N1 C1 C6 122.4(3) . . ? N1 C1 C2 121.4(3) . . ? C6 C1 C2 116.2(3) . . ? N2 K2 O2 138.52(10) . . ? N2 Si2 C89 108.09(16) . . ? N2 Si2 C95 112.73(17) . . ? C89 Si2 C95 107.81(18) . . ? N2 Si2 C101 115.89(16) . . ? C89 Si2 C101 106.85(17) . . ? C95 Si2 C101 105.07(16) . . ? C109 O2 C107 111.2(4) . . ? C109 O2 K2 120.4(3) . . ? C107 O2 K2 123.9(3) . . ? C56 N2 Si2 121.2(2) . . ? C56 N2 K2 120.8(2) . . ? Si2 N2 K2 118.00(16) . . ? C3 C2 C1 120.3(3) . . ? C3 C2 C8 123.1(3) . . ? C1 C2 C8 116.6(3) . . ? C2 C3 C4 123.1(3) . . ? C2 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C3 C4 C5 116.3(3) . . ? C3 C4 C7 121.8(3) . . ? C5 C4 C7 121.9(3) . . ? C6 C5 C4 122.7(4) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C5 C6 C1 120.1(3) . . ? C5 C6 C21 122.8(3) . . ? C1 C6 C21 117.1(3) . . ? 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 . . ? C15 C8 C2 115.9(3) . . ? C15 C8 C9 108.4(3) . . ? C2 C8 C9 111.8(3) . . ? C15 C8 H8 106.7 . . ? C2 C8 H8 106.7 . . ? C9 C8 H8 106.7 . . ? C10 C9 C14 118.2(4) . . ? C10 C9 C8 120.3(3) . . ? C14 C9 C8 121.4(3) . . ? C9 C10 C11 121.4(4) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 119.8(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 121.2(4) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C9 119.7(4) . . ? C13 C14 H14 120.2 . . ? C9 C14 H14 120.2 . . ? C16 C15 C20 117.0(4) . . ? C16 C15 C8 120.0(3) . . ? C20 C15 C8 122.9(3) . . ? C17 C16 C15 120.9(4) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C18 C17 C16 121.1(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 118.8(4) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C20 C19 C18 120.4(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C15 121.7(4) . . ? C19 C20 H20 119.1 . . ? C15 C20 H20 119.1 . . ? C28 C21 C6 114.2(3) . . ? C28 C21 C22 112.0(3) . . ? C6 C21 C22 112.2(3) . . ? C28 C21 H21 105.9 . . ? C6 C21 H21 105.9 . . ? C22 C21 H21 105.9 . . ? C27 C22 C23 118.6(4) . . ? C27 C22 C21 119.4(3) . . ? C23 C22 C21 122.0(3) . . ? C22 C23 C24 119.9(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 121.0(4) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 119.5(4) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 119.5(4) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C22 C27 C26 121.5(4) . . ? C22 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C29 C28 C33 118.0(4) . . ? C29 C28 C21 123.0(4) . . ? C33 C28 C21 119.0(3) . . ? C28 C29 C30 120.9(4) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C31 C30 C29 119.7(4) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C32 C31 C30 119.8(4) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 120.1(5) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 121.5(4) . . ? C32 C33 H33 119.3 . . ? C28 C33 H33 119.3 . . ? C35 C34 C39 115.8(3) . . ? C35 C34 Si1 121.6(3) . . ? C39 C34 Si1 122.5(3) . . ? C36 C35 C34 122.8(4) . . ? C36 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? C35 C36 C37 119.0(4) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C38 C37 C36 119.6(4) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 120.8(4) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C38 C39 C34 121.9(4) . . ? C38 C39 H39 119.1 . . ? C34 C39 H39 119.1 . . ? C41 C40 C45 116.6(4) . . ? C41 C40 Si1 119.7(3) . . ? C45 C40 Si1 123.6(3) . . ? C42 C41 C40 122.2(4) . . ? C42 C41 H41 118.9 . . ? C40 C41 H41 118.9 . . ? C43 C42 C41 119.2(4) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C44 C43 C42 119.7(4) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.8(4) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C44 C45 C40 121.4(4) . . ? C44 C45 H45 119.3 . . ? C40 C45 H45 119.3 . . ? C47 C46 C51 116.4(3) . . ? C47 C46 Si1 120.4(3) . . ? C51 C46 Si1 123.1(3) . . ? C48 C47 C46 122.3(4) . . ? C48 C47 H47 118.9 . . ? C46 C47 H47 118.9 . . ? C47 C48 C49 119.9(4) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C50 C49 C48 119.2(4) . . ? C50 C49 H49 120.4 . . ? C48 C49 H49 120.4 . . ? C51 C50 C49 120.9(4) . . ? C51 C50 H50 119.6 . . ? C49 C50 H50 119.6 . . ? C50 C51 C46 121.3(4) . . ? C50 C51 H51 119.3 . . ? C46 C51 H51 119.3 . . ? O1 C52 C53 107.8(4) . . ? O1 C52 H52A 110.1 . . ? C53 C52 H52A 110.1 . . ? O1 C52 H52B 110.1 . . ? C53 C52 H52B 110.1 . . ? H52A C52 H52B 108.5 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O1 C54 C55 110.2(4) . . ? O1 C54 H54A 109.6 . . ? C55 C54 H54A 109.6 . . ? O1 C54 H54B 109.6 . . ? C55 C54 H54B 109.6 . . ? H54A C54 H54B 108.1 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N2 C56 C57 123.0(3) . . ? N2 C56 C61 121.1(3) . . ? C57 C56 C61 115.9(3) . . ? C58 C57 C56 121.3(3) . . ? C58 C57 C63 122.1(3) . . ? C56 C57 C63 116.6(3) . . ? C57 C58 C59 121.6(4) . . ? C57 C58 H58 119.2 . . ? C59 C58 H58 119.2 . . ? C60 C59 C58 117.0(4) . . ? C60 C59 C62 121.9(3) . . ? C58 C59 C62 121.1(3) . . ? C61 C60 C59 122.4(3) . . ? C61 C60 H60 118.8 . . ? C59 C60 H60 118.8 . . ? C60 C61 C56 120.6(3) . . ? C60 C61 C76 122.7(3) . . ? C56 C61 C76 116.7(3) . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C70 111.0(3) . . ? C64 C63 C57 112.0(3) . . ? C70 C63 C57 114.0(3) . . ? C64 C63 H63 106.4 . . ? C70 C63 H63 106.4 . . ? C57 C63 H63 106.4 . . ? C69 C64 C65 118.1(4) . . ? C69 C64 C63 123.3(4) . . ? C65 C64 C63 118.6(3) . . ? C66 C65 C64 121.0(4) . . ? C66 C65 H65 119.5 . . ? C64 C65 H65 119.5 . . ? C65 C66 C67 120.3(4) . . ? C65 C66 H66 119.8 . . ? C67 C66 H66 119.8 . . ? C66 C67 C68 119.6(4) . . ? C66 C67 H67 120.2 . . ? C68 C67 H67 120.2 . . ? C67 C68 C69 120.0(4) . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C64 C69 C68 120.9(4) . . ? C64 C69 H69 119.5 . . ? C68 C69 H69 119.5 . . ? C75 C70 C71 118.6(4) . . ? C75 C70 C63 118.7(3) . . ? C71 C70 C63 122.7(3) . . ? C72 C71 C70 120.6(4) . . ? C72 C71 H71 119.7 . . ? C70 C71 H71 119.7 . . ? C71 C72 C73 120.2(4) . . ? C71 C72 H72 119.9 . . ? C73 C72 H72 119.9 . . ? C74 C73 C72 119.8(4) . . ? C74 C73 H73 120.1 . . ? C72 C73 H73 120.1 . . ? C73 C74 C75 119.7(4) . . ? C73 C74 H74 120.2 . . ? C75 C74 H74 120.2 . . ? C70 C75 C74 121.1(4) . . ? C70 C75 H75 119.5 . . ? C74 C75 H75 119.5 . . ? C77 C76 C61 112.8(3) . . ? C77 C76 C83 108.2(3) . . ? C61 C76 C83 114.0(3) . . ? C77 C76 H76 107.2 . . ? C61 C76 H76 107.2 . . ? C83 C76 H76 107.2 . . ? C82 C77 C78 117.8(4) . . ? C82 C77 C76 120.1(4) . . ? C78 C77 C76 122.1(4) . . ? C79 C78 C77 120.7(4) . . ? C79 C78 H78 119.7 . . ? C77 C78 H78 119.7 . . ? C80 C79 C78 121.2(5) . . ? C80 C79 H79 119.4 . . ? C78 C79 H79 119.4 . . ? C79 C80 C81 119.1(4) . . ? C79 C80 H80 120.4 . . ? C81 C80 H80 120.4 . . ? C82 C81 C80 119.8(5) . . ? C82 C81 H81 120.1 . . ? C80 C81 H81 120.1 . . ? C81 C82 C77 121.3(5) . . ? C81 C82 H82 119.3 . . ? C77 C82 H82 119.3 . . ? C88 C83 C84 118.8(3) . . ? C88 C83 C76 120.8(3) . . ? C84 C83 C76 120.4(3) . . ? C85 C84 C83 121.2(4) . . ? C85 C84 H84 119.4 . . ? C83 C84 H84 119.4 . . ? C86 C85 C84 119.4(4) . . ? C86 C85 H85 120.3 . . ? C84 C85 H85 120.3 . . ? C85 C86 C87 120.2(4) . . ? C85 C86 H86 119.9 . . ? C87 C86 H86 119.9 . . ? C86 C87 C88 120.1(4) . . ? C86 C87 H87 120.0 . . ? C88 C87 H87 120.0 . . ? C83 C88 C87 120.2(4) . . ? C83 C88 H88 119.9 . . ? C87 C88 H88 119.9 . . ? C90 C89 C94 116.2(4) . . ? C90 C89 Si2 118.8(3) . . ? C94 C89 Si2 125.0(3) . . ? C91 C90 C89 122.6(4) . . ? C91 C90 H90 118.7 . . ? C89 C90 H90 118.7 . . ? C90 C91 C92 119.3(4) . . ? C90 C91 H91 120.3 . . ? C92 C91 H91 120.3 . . ? C93 C92 C91 119.5(4) . . ? C93 C92 H92 120.3 . . ? C91 C92 H92 120.3 . . ? C92 C93 C94 121.3(4) . . ? C92 C93 H93 119.3 . . ? C94 C93 H93 119.3 . . ? C93 C94 C89 121.0(4) . . ? C93 C94 H94 119.5 . . ? C89 C94 H94 119.5 . . ? C100 C95 C96 116.9(4) . . ? C100 C95 Si2 123.6(3) . . ? C96 C95 Si2 119.5(3) . . ? C97 C96 C95 121.6(4) . . ? C97 C96 H96 119.2 . . ? C95 C96 H96 119.2 . . ? C98 C97 C96 120.0(4) . . ? C98 C97 H97 120.0 . . ? C96 C97 H97 120.0 . . ? C97 C98 C99 120.1(4) . . ? C97 C98 H98 119.9 . . ? C99 C98 H98 119.9 . . ? C98 C99 C100 119.6(5) . . ? C98 C99 H99 120.2 . . ? C100 C99 H99 120.2 . . ? C95 C100 C99 121.8(4) . . ? C95 C100 H100 119.1 . . ? C99 C100 H100 119.1 . . ? C106 C101 C102 116.7(3) . . ? C106 C101 Si2 123.9(3) . . ? C102 C101 Si2 119.3(3) . . ? C103 C102 C101 121.1(4) . . ? C103 C102 H102 119.4 . . ? C101 C102 H102 119.4 . . ? C104 C103 C102 120.7(4) . . ? C104 C103 H103 119.7 . . ? C102 C103 H103 119.7 . . ? C103 C104 C105 119.7(4) . . ? C103 C104 H104 120.1 . . ? C105 C104 H104 120.1 . . ? C104 C105 C106 119.8(4) . . ? C104 C105 H105 120.1 . . ? C106 C105 H105 120.1 . . ? C101 C106 C105 121.9(4) . . ? C101 C106 H106 119.1 . . ? C105 C106 H106 119.1 . . ? O2 C107 C108 108.1(4) . . ? O2 C107 H10A 110.1 . . ? C108 C107 H10A 110.1 . . ? O2 C107 H10B 110.1 . . ? C108 C107 H10B 110.1 . . ? H10A C107 H10B 108.4 . . ? C107 C108 H10C 109.5 . . ? C107 C108 H10D 109.5 . . ? H10C C108 H10D 109.5 . . ? C107 C108 H10E 109.5 . . ? H10C C108 H10E 109.5 . . ? H10D C108 H10E 109.5 . . ? O2 C109 C110 109.9(4) . . ? O2 C109 H10F 109.7 . . ? C110 C109 H10F 109.7 . . ? O2 C109 H10G 109.7 . . ? C110 C109 H10G 109.7 . . ? H10F C109 H10G 108.2 . . ? C109 C110 H11A 109.5 . . ? C109 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? C109 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.468 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.060 # Attachment '- compound1.CIF' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 822598' #TrackingRef '- compound1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H37 N Si' _chemical_formula_weight 511.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 16.6936(8) _cell_length_b 22.4261(9) _cell_length_c 7.6390(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2859.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.945 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 37410 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2569 _reflns_number_gt 1846 _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^)+(0.0413P)^2^+2.0258P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2569 _refine_ls_number_parameters 188 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.73170(6) 0.2500 0.09823(14) 0.0368(3) Uani 1 2 d S . . N1 N 0.83333(16) 0.2500 0.1417(3) 0.0285(6) Uani 1 2 d SD . . C1 C 0.87127(17) 0.2500 0.3099(4) 0.0230(7) Uani 1 2 d S . . C2 C 0.89031(12) 0.30382(9) 0.3917(3) 0.0239(5) Uani 1 1 d . . . C3 C 0.92921(13) 0.30278(9) 0.5523(3) 0.0263(5) Uani 1 1 d . . . H3 H 0.9419 0.3395 0.6079 0.032 Uiso 1 1 calc R . . C4 C 0.95010(18) 0.2500 0.6338(4) 0.0254(7) Uani 1 2 d S . . C5 C 0.9943(2) 0.2500 0.8059(4) 0.0325(8) Uani 1 2 d S . . H5A H 0.9687 0.2782 0.8863 0.049 Uiso 0.50 1 calc PR . . H5B H 1.0501 0.2619 0.7865 0.049 Uiso 0.50 1 calc PR . . H5C H 0.9928 0.2099 0.8568 0.049 Uiso 0.50 1 calc PR . . C6 C 0.87129(13) 0.36256(9) 0.3010(3) 0.0248(5) Uani 1 1 d . . . H6 H 0.8204 0.3557 0.2347 0.030 Uiso 1 1 calc R . . C7 C 0.85411(12) 0.41356(9) 0.4271(3) 0.0256(5) Uani 1 1 d . . . C8 C 0.89424(14) 0.46745(9) 0.4217(3) 0.0298(5) Uani 1 1 d . . . H8 H 0.9369 0.4728 0.3409 0.036 Uiso 1 1 calc R . . C9 C 0.87321(15) 0.51373(10) 0.5324(3) 0.0373(6) Uani 1 1 d . . . H9 H 0.9015 0.5504 0.5269 0.045 Uiso 1 1 calc R . . C10 C 0.81167(15) 0.50693(11) 0.6504(3) 0.0419(7) Uani 1 1 d . . . H10 H 0.7968 0.5389 0.7251 0.050 Uiso 1 1 calc R . . C11 C 0.77188(15) 0.45323(12) 0.6590(3) 0.0411(6) Uani 1 1 d . . . H11 H 0.7298 0.4480 0.7414 0.049 Uiso 1 1 calc R . . C12 C 0.79264(13) 0.40723(11) 0.5492(3) 0.0332(6) Uani 1 1 d . . . H12 H 0.7646 0.3705 0.5567 0.040 Uiso 1 1 calc R . . C13 C 0.93397(13) 0.37886(9) 0.1650(3) 0.0247(5) Uani 1 1 d . . . C14 C 0.91146(14) 0.40788(10) 0.0137(3) 0.0319(6) Uani 1 1 d . . . H14 H 0.8563 0.4153 -0.0076 0.038 Uiso 1 1 calc R . . C15 C 0.96734(16) 0.42637(11) -0.1069(3) 0.0396(6) Uani 1 1 d . . . H15 H 0.9506 0.4462 -0.2106 0.047 Uiso 1 1 calc R . . C16 C 1.04744(16) 0.41619(11) -0.0774(3) 0.0417(7) Uani 1 1 d . . . H16 H 1.0863 0.4291 -0.1600 0.050 Uiso 1 1 calc R . . C17 C 1.07068(15) 0.38722(11) 0.0720(3) 0.0396(6) Uani 1 1 d . . . H17 H 1.1260 0.3802 0.0927 0.047 Uiso 1 1 calc R . . C18 C 1.01478(13) 0.36816(10) 0.1927(3) 0.0322(6) Uani 1 1 d . . . H18 H 1.0317 0.3477 0.2950 0.039 Uiso 1 1 calc R . . C19 C 0.6800(2) 0.2500 0.3130(6) 0.0562(11) Uani 1 2 d S . . H19A H 0.6998 0.2167 0.3840 0.084 Uiso 0.50 1 calc PR . . H19B H 0.6222 0.2456 0.2949 0.084 Uiso 0.50 1 calc PR . . H19C H 0.6908 0.2877 0.3737 0.084 Uiso 0.50 1 calc PR . . C20 C 0.70246(18) 0.31666(13) -0.0309(4) 0.0643(9) Uani 1 1 d . . . H20A H 0.7108 0.3526 0.0397 0.097 Uiso 1 1 calc R . . H20B H 0.6458 0.3137 -0.0634 0.097 Uiso 1 1 calc R . . H20C H 0.7353 0.3189 -0.1370 0.097 Uiso 1 1 calc R . . H1 H 0.861(2) 0.2685(17) 0.059(4) 0.039(15) Uiso 0.50 1 d PD . . 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 0.0322(6) 0.0282(5) 0.0499(6) 0.000 -0.0133(5) 0.000 N1 0.0299(16) 0.0328(15) 0.0227(16) 0.000 -0.0021(13) 0.000 C1 0.0193(16) 0.0268(16) 0.0229(17) 0.000 0.0010(14) 0.000 C2 0.0203(11) 0.0251(11) 0.0264(12) 0.0001(9) 0.0036(10) 0.0009(9) C3 0.0258(12) 0.0255(11) 0.0274(12) -0.0029(10) -0.0005(10) -0.0019(9) C4 0.0246(17) 0.0276(16) 0.0241(17) 0.000 0.0020(14) 0.000 C5 0.040(2) 0.0298(18) 0.0277(19) 0.000 -0.0044(16) 0.000 C6 0.0233(11) 0.0236(11) 0.0276(12) 0.0008(9) -0.0025(10) -0.0010(9) C7 0.0238(12) 0.0266(12) 0.0265(12) 0.0026(9) -0.0046(10) 0.0049(9) C8 0.0335(13) 0.0268(12) 0.0292(13) 0.0023(10) -0.0011(11) 0.0041(10) C9 0.0478(16) 0.0263(12) 0.0378(14) -0.0013(11) -0.0083(13) 0.0062(11) C10 0.0460(16) 0.0427(15) 0.0370(15) -0.0110(12) -0.0048(13) 0.0181(13) C11 0.0306(14) 0.0572(17) 0.0355(14) -0.0061(12) 0.0024(12) 0.0113(13) C12 0.0249(13) 0.0396(13) 0.0352(14) -0.0002(11) 0.0000(11) 0.0013(10) C13 0.0298(13) 0.0192(11) 0.0250(12) -0.0032(9) -0.0016(10) -0.0009(9) C14 0.0325(13) 0.0324(13) 0.0309(14) 0.0029(11) -0.0016(11) -0.0004(10) C15 0.0521(17) 0.0363(14) 0.0304(14) 0.0076(11) 0.0005(12) -0.0007(12) C16 0.0451(17) 0.0393(14) 0.0407(16) 0.0031(12) 0.0138(13) -0.0041(12) C17 0.0296(13) 0.0427(15) 0.0464(16) 0.0024(12) 0.0051(12) 0.0011(11) C18 0.0304(13) 0.0344(13) 0.0317(13) 0.0038(10) -0.0009(11) 0.0005(10) C19 0.034(2) 0.053(2) 0.082(3) 0.000 0.007(2) 0.000 C20 0.0574(19) 0.0522(17) 0.083(2) 0.0184(16) -0.0286(18) 0.0021(15) _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 1.729(3) . ? Si1 C19 1.854(4) . ? Si1 C20 1.856(3) 8_565 ? Si1 C20 1.856(3) . ? N1 C1 1.433(4) . ? N1 H1 0.882(19) . ? C1 C2 1.396(2) . ? C1 C2 1.396(2) 8_565 ? C2 C3 1.388(3) . ? C2 C6 1.522(3) . ? C3 C4 1.382(3) . ? C3 H3 0.9500 . ? C4 C3 1.382(3) 8_565 ? C4 C5 1.508(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C13 1.519(3) . ? C6 C7 1.523(3) . ? C6 H6 1.0000 . ? C7 C8 1.383(3) . ? C7 C12 1.394(3) . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.375(3) . ? C9 H9 0.9500 . ? C10 C11 1.377(4) . ? C10 H10 0.9500 . ? C11 C12 1.374(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.378(3) . ? C13 C18 1.386(3) . ? C14 C15 1.375(3) . ? C14 H14 0.9500 . ? C15 C16 1.375(3) . ? C15 H15 0.9500 . ? C16 C17 1.369(3) . ? C16 H16 0.9500 . ? C17 C18 1.380(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 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 C19 106.67(16) . . ? N1 Si1 C20 111.10(11) . 8_565 ? C19 Si1 C20 110.36(13) . 8_565 ? N1 Si1 C20 111.10(11) . . ? C19 Si1 C20 110.36(13) . . ? C20 Si1 C20 107.3(2) 8_565 . ? C1 N1 Si1 127.3(2) . . ? C1 N1 H1 114(3) . . ? Si1 N1 H1 112(3) . . ? C2 C1 C2 119.7(3) . 8_565 ? C2 C1 N1 120.15(14) . . ? C2 C1 N1 120.15(14) 8_565 . ? C3 C2 C1 119.2(2) . . ? C3 C2 C6 120.97(18) . . ? C1 C2 C6 119.8(2) . . ? C4 C3 C2 122.0(2) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C3 117.8(3) 8_565 . ? C3 C4 C5 121.08(14) 8_565 . ? C3 C4 C5 121.08(14) . . ? 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 . . ? C13 C6 C2 112.09(17) . . ? C13 C6 C7 112.44(17) . . ? C2 C6 C7 113.65(17) . . ? C13 C6 H6 106.0 . . ? C2 C6 H6 106.0 . . ? C7 C6 H6 106.0 . . ? C8 C7 C12 117.8(2) . . ? C8 C7 C6 123.13(19) . . ? C12 C7 C6 119.05(19) . . ? C7 C8 C9 121.0(2) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 120.5(2) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.3(2) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 120.4(2) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 121.2(2) . . ? C11 C12 H12 119.4 . . ? C7 C12 H12 119.4 . . ? C14 C13 C18 118.4(2) . . ? C14 C13 C6 119.94(19) . . ? C18 C13 C6 121.61(19) . . ? C15 C14 C13 121.3(2) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 120.0(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 119.4(2) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.8(2) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 120.2(2) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.303 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.046 # Attachment '- compound10.CIF' data_compound10 _database_code_depnum_ccdc_archive 'CCDC 822599' #TrackingRef '- compound10.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H88 Cl2 N2 Pb2 Si2' _chemical_formula_weight 1691.04 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 '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 9.8669(4) _cell_length_b 13.0330(5) _cell_length_c 15.5728(7) _cell_angle_alpha 79.153(2) _cell_angle_beta 84.525(2) _cell_angle_gamma 72.621(2) _cell_volume 1875.38(13) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 4.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 0.800 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 41818 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7238 _reflns_number_gt 5844 _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. the C atoms of one molecule of toluene of crystallisation in the asymmetric unit were refined anisotropically. The DFIX and FLAT commands of SHELX-L were used to constrain the geometry of this toluene molecule, giving rise to the 23 restraints used in the final refinement. ; _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^)+(0.0320P)^2^+0.9266P] 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 7238 _refine_ls_number_parameters 429 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _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 Pb1 Pb 0.52254(2) 0.543201(16) 0.623619(11) 0.02941(7) Uani 1 1 d . . . Cl1 Cl 0.53478(15) 0.36729(10) 0.55309(8) 0.0403(3) Uani 1 1 d . . . Si1 Si 0.16141(14) 0.53634(11) 0.64334(8) 0.0275(3) Uani 1 1 d . . . N1 N 0.3018(4) 0.5717(3) 0.6764(2) 0.0225(8) Uani 1 1 d . . . C1 C 0.2780(4) 0.6284(3) 0.7490(3) 0.0197(10) Uani 1 1 d . . . C2 C 0.2393(4) 0.7428(4) 0.7364(3) 0.0227(10) Uani 1 1 d . . . C3 C 0.2072(5) 0.7955(4) 0.8086(3) 0.0260(11) Uani 1 1 d . . . H3 H 0.1782 0.8729 0.7995 0.031 Uiso 1 1 calc R . . C4 C 0.2162(5) 0.7390(4) 0.8928(3) 0.0253(10) Uani 1 1 d . . . C5 C 0.2606(5) 0.6264(4) 0.9044(3) 0.0238(10) Uani 1 1 d . . . H5 H 0.2699 0.5861 0.9622 0.029 Uiso 1 1 calc R . . C6 C 0.2917(4) 0.5710(3) 0.8350(3) 0.0212(10) Uani 1 1 d . . . C7 C 0.1773(6) 0.7999(4) 0.9689(3) 0.0377(13) Uani 1 1 d . . . H7A H 0.0748 0.8156 0.9824 0.056 Uiso 1 1 calc R . . H7B H 0.2026 0.8685 0.9537 0.056 Uiso 1 1 calc R . . H7C H 0.2291 0.7552 1.0200 0.056 Uiso 1 1 calc R . . C8 C 0.2481(5) 0.8070(3) 0.6449(3) 0.0221(10) Uani 1 1 d . . . H8 H 0.2278 0.7634 0.6039 0.027 Uiso 1 1 calc R . . C9 C 0.3991(5) 0.8140(3) 0.6210(3) 0.0219(10) Uani 1 1 d . . . C10 C 0.4390(5) 0.8450(4) 0.5351(3) 0.0348(12) Uani 1 1 d . . . H10 H 0.3703 0.8648 0.4915 0.042 Uiso 1 1 calc R . . C11 C 0.5744(6) 0.8479(5) 0.5109(3) 0.0451(14) Uani 1 1 d . . . H11 H 0.5980 0.8698 0.4511 0.054 Uiso 1 1 calc R . . C12 C 0.6758(6) 0.8205(4) 0.5703(4) 0.0440(14) Uani 1 1 d . . . H12 H 0.7698 0.8231 0.5529 0.053 Uiso 1 1 calc R . . C13 C 0.6402(6) 0.7890(5) 0.6554(4) 0.0578(17) Uani 1 1 d . . . H13 H 0.7105 0.7687 0.6979 0.069 Uiso 1 1 calc R . . C14 C 0.5037(5) 0.7859(5) 0.6811(3) 0.0444(14) Uani 1 1 d . . . H14 H 0.4813 0.7641 0.7411 0.053 Uiso 1 1 calc R . . C15 C 0.1349(5) 0.9164(4) 0.6315(3) 0.0257(11) Uani 1 1 d . . . C16 C -0.0021(5) 0.9191(4) 0.6169(3) 0.0383(13) Uani 1 1 d . . . H16 H -0.0217 0.8525 0.6151 0.046 Uiso 1 1 calc R . . C17 C -0.1103(6) 1.0138(5) 0.6049(4) 0.0465(14) Uani 1 1 d . . . H17 H -0.2033 1.0127 0.5950 0.056 Uiso 1 1 calc R . . C18 C -0.0835(6) 1.1104(4) 0.6074(3) 0.0421(14) Uani 1 1 d . . . H18 H -0.1579 1.1769 0.5990 0.051 Uiso 1 1 calc R . . C19 C 0.0510(6) 1.1106(4) 0.6218(3) 0.0457(14) Uani 1 1 d . . . H19 H 0.0699 1.1775 0.6233 0.055 Uiso 1 1 calc R . . C20 C 0.1605(6) 1.0130(4) 0.6345(3) 0.0381(13) Uani 1 1 d . . . H20 H 0.2534 1.0138 0.6452 0.046 Uiso 1 1 calc R . . C21 C 0.3548(5) 0.4475(3) 0.8489(3) 0.0225(10) Uani 1 1 d . . . H21 H 0.3145 0.4212 0.8035 0.027 Uiso 1 1 calc R . . C22 C 0.3136(5) 0.3890(4) 0.9371(3) 0.0240(10) Uani 1 1 d . . . C23 C 0.1721(5) 0.3955(4) 0.9565(3) 0.0411(13) Uani 1 1 d . . . H23 H 0.1028 0.4385 0.9158 0.049 Uiso 1 1 calc R . . C24 C 0.1294(6) 0.3405(5) 1.0343(4) 0.0489(15) Uani 1 1 d . . . H24 H 0.0315 0.3470 1.0472 0.059 Uiso 1 1 calc R . . C25 C 0.2287(7) 0.2768(4) 1.0925(3) 0.0471(15) Uani 1 1 d . . . H25 H 0.2001 0.2375 1.1454 0.057 Uiso 1 1 calc R . . C26 C 0.3688(6) 0.2700(4) 1.0744(3) 0.0422(14) Uani 1 1 d . . . H26 H 0.4379 0.2259 1.1148 0.051 Uiso 1 1 calc R . . C27 C 0.4105(5) 0.3269(4) 0.9977(3) 0.0294(11) Uani 1 1 d . . . H27 H 0.5081 0.3230 0.9865 0.035 Uiso 1 1 calc R . . C28 C 0.5138(5) 0.4199(4) 0.8289(3) 0.0238(10) Uani 1 1 d . . . C29 C 0.5829(5) 0.3329(4) 0.7869(3) 0.0348(12) Uani 1 1 d . . . H29 H 0.5301 0.2896 0.7712 0.042 Uiso 1 1 calc R . . C30 C 0.7281(6) 0.3079(5) 0.7674(3) 0.0469(14) Uani 1 1 d . . . H30 H 0.7736 0.2481 0.7381 0.056 Uiso 1 1 calc R . . C31 C 0.8061(6) 0.3688(5) 0.7902(3) 0.0478(15) Uani 1 1 d . . . H31 H 0.9051 0.3523 0.7755 0.057 Uiso 1 1 calc R . . C32 C 0.7419(5) 0.4530(5) 0.8337(3) 0.0392(13) Uani 1 1 d . . . H32 H 0.7966 0.4936 0.8515 0.047 Uiso 1 1 calc R . . C33 C 0.5948(5) 0.4798(4) 0.8524(3) 0.0292(11) Uani 1 1 d . . . H33 H 0.5502 0.5399 0.8816 0.035 Uiso 1 1 calc R . . C34 C 0.1224(6) 0.5920(5) 0.5261(3) 0.0501(16) Uani 1 1 d . . . H34A H 0.1127 0.6704 0.5149 0.075 Uiso 1 1 calc R . . H34B H 0.0337 0.5800 0.5131 0.075 Uiso 1 1 calc R . . H34C H 0.2004 0.5550 0.4889 0.075 Uiso 1 1 calc R . . C35 C 0.0005(5) 0.5947(4) 0.7101(3) 0.0406(13) Uani 1 1 d . . . H35A H 0.0156 0.5630 0.7719 0.061 Uiso 1 1 calc R . . H35B H -0.0812 0.5779 0.6910 0.061 Uiso 1 1 calc R . . H35C H -0.0179 0.6739 0.7025 0.061 Uiso 1 1 calc R . . C36 C 0.1863(6) 0.3872(4) 0.6582(4) 0.0474(15) Uani 1 1 d . . . H36A H 0.2754 0.3523 0.6282 0.071 Uiso 1 1 calc R . . H36B H 0.1067 0.3738 0.6335 0.071 Uiso 1 1 calc R . . H36C H 0.1900 0.3567 0.7207 0.071 Uiso 1 1 calc R . . C37 C 0.6549(9) 0.0345(5) 0.8502(6) 0.080(2) Uani 1 1 d D . . C38 C 0.5503(10) 0.0793(6) 0.9026(5) 0.087(2) Uani 1 1 d D . . H38 H 0.5736 0.0932 0.9563 0.105 Uiso 1 1 calc R . . C39 C 0.4108(10) 0.1069(6) 0.8841(6) 0.093(3) Uani 1 1 d D . . H39 H 0.3396 0.1375 0.9251 0.112 Uiso 1 1 calc R . . C40 C 0.3729(10) 0.0908(7) 0.8066(7) 0.105(3) Uani 1 1 d DU . . H40 H 0.2769 0.1093 0.7906 0.126 Uiso 1 1 calc R . . C41 C 0.4894(12) 0.0440(9) 0.7528(6) 0.129(3) Uani 1 1 d DU . . H41 H 0.4719 0.0340 0.6965 0.155 Uiso 1 1 calc R . . C42 C 0.6252(9) 0.0128(8) 0.7781(6) 0.097(3) Uani 1 1 d D . . H42 H 0.6993 -0.0255 0.7424 0.116 Uiso 1 1 calc R . . C43 C 0.8125(10) 0.0056(8) 0.8714(7) 0.138(4) Uani 1 1 d D . . H43A H 0.8452 0.0709 0.8555 0.207 Uiso 1 1 calc R . . H43B H 0.8692 -0.0505 0.8381 0.207 Uiso 1 1 calc R . . H43C H 0.8234 -0.0221 0.9342 0.207 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 Pb1 0.02398(11) 0.04102(13) 0.02612(11) -0.01281(8) 0.00375(7) -0.01075(8) Cl1 0.0592(9) 0.0305(7) 0.0291(7) -0.0041(5) 0.0035(6) -0.0120(7) Si1 0.0270(8) 0.0312(8) 0.0281(7) -0.0041(6) -0.0039(6) -0.0140(6) N1 0.022(2) 0.027(2) 0.0204(19) -0.0045(16) -0.0004(16) -0.0090(17) C1 0.014(2) 0.024(3) 0.022(2) -0.0035(19) -0.0010(18) -0.008(2) C2 0.017(2) 0.028(3) 0.023(2) 0.000(2) -0.0056(19) -0.008(2) C3 0.024(3) 0.024(3) 0.029(3) -0.003(2) -0.003(2) -0.006(2) C4 0.021(3) 0.032(3) 0.024(2) -0.006(2) 0.0000(19) -0.006(2) C5 0.020(3) 0.029(3) 0.020(2) -0.001(2) -0.0014(19) -0.006(2) C6 0.017(2) 0.023(3) 0.023(2) -0.0018(19) 0.0007(19) -0.008(2) C7 0.047(3) 0.038(3) 0.026(3) -0.014(2) 0.000(2) -0.005(3) C8 0.025(3) 0.023(3) 0.020(2) -0.0034(19) -0.0045(19) -0.008(2) C9 0.022(3) 0.018(2) 0.026(2) -0.0060(19) -0.001(2) -0.004(2) C10 0.030(3) 0.041(3) 0.032(3) 0.002(2) -0.004(2) -0.012(2) C11 0.036(3) 0.063(4) 0.036(3) -0.002(3) 0.009(3) -0.020(3) C12 0.029(3) 0.055(4) 0.057(4) -0.024(3) 0.011(3) -0.022(3) C13 0.033(3) 0.096(5) 0.048(4) -0.012(3) -0.012(3) -0.021(3) C14 0.029(3) 0.070(4) 0.034(3) -0.004(3) -0.004(2) -0.016(3) C15 0.031(3) 0.022(3) 0.020(2) -0.0003(19) -0.003(2) -0.005(2) C16 0.030(3) 0.037(3) 0.047(3) 0.002(2) -0.005(2) -0.013(3) C17 0.026(3) 0.047(4) 0.055(4) 0.009(3) -0.007(3) -0.002(3) C18 0.038(3) 0.037(3) 0.034(3) -0.002(2) 0.002(2) 0.012(3) C19 0.059(4) 0.029(3) 0.045(3) -0.008(2) -0.001(3) -0.004(3) C20 0.036(3) 0.027(3) 0.048(3) -0.004(2) -0.007(3) -0.003(3) C21 0.026(3) 0.022(2) 0.019(2) -0.0013(19) -0.0002(19) -0.007(2) C22 0.025(3) 0.024(3) 0.025(2) -0.004(2) 0.002(2) -0.011(2) C23 0.030(3) 0.046(3) 0.042(3) 0.007(3) -0.004(2) -0.012(3) C24 0.037(3) 0.053(4) 0.057(4) 0.002(3) 0.014(3) -0.025(3) C25 0.070(4) 0.037(3) 0.034(3) 0.001(3) 0.012(3) -0.023(3) C26 0.053(4) 0.045(3) 0.024(3) 0.006(2) 0.000(3) -0.013(3) C27 0.031(3) 0.032(3) 0.026(3) -0.004(2) -0.002(2) -0.011(2) C28 0.027(3) 0.025(3) 0.015(2) 0.0025(19) 0.0045(19) -0.006(2) C29 0.038(3) 0.033(3) 0.031(3) -0.004(2) -0.001(2) -0.006(3) C30 0.042(4) 0.048(4) 0.039(3) -0.013(3) 0.008(3) 0.005(3) C31 0.024(3) 0.067(4) 0.040(3) 0.004(3) 0.010(2) -0.006(3) C32 0.029(3) 0.054(4) 0.034(3) 0.002(3) 0.003(2) -0.019(3) C33 0.030(3) 0.037(3) 0.022(3) -0.005(2) 0.003(2) -0.012(2) C34 0.055(4) 0.069(4) 0.036(3) 0.004(3) -0.017(3) -0.036(3) C35 0.031(3) 0.046(3) 0.049(3) -0.006(3) -0.002(2) -0.018(3) C36 0.046(4) 0.037(3) 0.068(4) -0.015(3) -0.005(3) -0.021(3) C37 0.084(6) 0.039(4) 0.122(7) -0.014(4) -0.030(6) -0.018(4) C38 0.088(7) 0.091(6) 0.082(6) -0.022(5) -0.024(5) -0.015(5) C39 0.094(7) 0.062(5) 0.125(8) -0.039(5) 0.045(6) -0.025(5) C40 0.090(5) 0.089(5) 0.152(6) -0.018(5) -0.045(5) -0.037(4) C41 0.137(6) 0.151(6) 0.095(5) -0.034(5) -0.042(5) -0.016(5) C42 0.083(7) 0.121(8) 0.081(6) -0.001(5) -0.004(5) -0.032(6) C43 0.125(9) 0.112(8) 0.184(11) -0.027(7) -0.045(8) -0.031(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 Pb1 N1 2.202(3) . ? Pb1 Cl1 2.6897(12) . ? Pb1 Cl1 2.8192(12) 2_666 ? Cl1 Pb1 2.8192(12) 2_666 ? Si1 N1 1.734(4) . ? Si1 C35 1.854(5) . ? Si1 C36 1.858(5) . ? Si1 C34 1.864(5) . ? N1 C1 1.427(5) . ? C1 C6 1.403(6) . ? C1 C2 1.404(6) . ? C2 C3 1.389(6) . ? C2 C8 1.519(6) . ? C3 C4 1.374(6) . ? C4 C5 1.382(6) . ? C4 C7 1.505(6) . ? C5 C6 1.372(6) . ? C6 C21 1.524(6) . ? C8 C15 1.519(6) . ? C8 C9 1.526(6) . ? C9 C10 1.379(6) . ? C9 C14 1.380(6) . ? C10 C11 1.363(7) . ? C11 C12 1.350(7) . ? C12 C13 1.356(7) . ? C13 C14 1.378(7) . ? C15 C20 1.366(6) . ? C15 C16 1.381(7) . ? C16 C17 1.364(7) . ? C17 C18 1.369(7) . ? C18 C19 1.368(8) . ? C19 C20 1.396(7) . ? C21 C28 1.516(6) . ? C21 C22 1.524(6) . ? C22 C27 1.371(6) . ? C22 C23 1.381(6) . ? C23 C24 1.383(7) . ? C24 C25 1.367(8) . ? C25 C26 1.365(8) . ? C26 C27 1.379(6) . ? C28 C29 1.381(6) . ? C28 C33 1.386(6) . ? C29 C30 1.389(7) . ? C30 C31 1.368(8) . ? C31 C32 1.360(8) . ? C32 C33 1.402(7) . ? C37 C42 1.288(9) . ? C37 C38 1.316(9) . ? C37 C43 1.540(10) . ? C38 C39 1.360(10) . ? C39 C40 1.367(10) . ? C40 C41 1.409(11) . ? C41 C42 1.353(10) . ? 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 Pb1 Cl1 96.87(9) . . ? N1 Pb1 Cl1 98.38(9) . 2_666 ? Cl1 Pb1 Cl1 77.18(4) . 2_666 ? Pb1 Cl1 Pb1 102.82(4) . 2_666 ? N1 Si1 C35 108.0(2) . . ? N1 Si1 C36 114.5(2) . . ? C35 Si1 C36 107.0(2) . . ? N1 Si1 C34 112.6(2) . . ? C35 Si1 C34 107.6(3) . . ? C36 Si1 C34 106.8(3) . . ? C1 N1 Si1 118.4(3) . . ? C1 N1 Pb1 111.5(2) . . ? Si1 N1 Pb1 130.10(19) . . ? C6 C1 C2 118.2(4) . . ? C6 C1 N1 120.7(4) . . ? C2 C1 N1 121.0(4) . . ? C3 C2 C1 119.5(4) . . ? C3 C2 C8 120.5(4) . . ? C1 C2 C8 119.7(4) . . ? C4 C3 C2 122.0(4) . . ? C3 C4 C5 118.0(4) . . ? C3 C4 C7 120.0(4) . . ? C5 C4 C7 122.0(4) . . ? C6 C5 C4 121.9(4) . . ? C5 C6 C1 120.3(4) . . ? C5 C6 C21 121.0(4) . . ? C1 C6 C21 118.5(4) . . ? C2 C8 C15 112.6(4) . . ? C2 C8 C9 110.8(3) . . ? C15 C8 C9 114.0(3) . . ? C10 C9 C14 116.4(4) . . ? C10 C9 C8 120.1(4) . . ? C14 C9 C8 123.4(4) . . ? C11 C10 C9 121.7(5) . . ? C12 C11 C10 121.4(5) . . ? C11 C12 C13 118.4(5) . . ? C12 C13 C14 121.1(5) . . ? C13 C14 C9 121.1(5) . . ? C20 C15 C16 117.8(4) . . ? C20 C15 C8 123.5(4) . . ? C16 C15 C8 118.8(4) . . ? C17 C16 C15 122.5(5) . . ? C16 C17 C18 119.4(5) . . ? C19 C18 C17 119.6(5) . . ? C18 C19 C20 120.4(5) . . ? C15 C20 C19 120.3(5) . . ? C28 C21 C22 113.9(4) . . ? C28 C21 C6 109.2(3) . . ? C22 C21 C6 114.2(4) . . ? C27 C22 C23 117.9(4) . . ? C27 C22 C21 123.3(4) . . ? C23 C22 C21 118.7(4) . . ? C22 C23 C24 121.1(5) . . ? C25 C24 C23 119.8(5) . . ? C26 C25 C24 119.7(5) . . ? C25 C26 C27 120.2(5) . . ? C22 C27 C26 121.2(5) . . ? C29 C28 C33 117.8(4) . . ? C29 C28 C21 120.7(4) . . ? C33 C28 C21 121.6(4) . . ? C28 C29 C30 121.1(5) . . ? C31 C30 C29 120.3(5) . . ? C32 C31 C30 120.0(5) . . ? C31 C32 C33 120.0(5) . . ? C28 C33 C32 120.8(5) . . ? C42 C37 C38 119.0(8) . . ? C42 C37 C43 118.1(9) . . ? C38 C37 C43 122.9(9) . . ? C37 C38 C39 123.6(8) . . ? C38 C39 C40 120.1(8) . . ? C39 C40 C41 113.7(8) . . ? C42 C41 C40 122.7(9) . . ? C37 C42 C41 120.6(9) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.180 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.120 # Attachment '- compound12.CIF' data_compound12 _database_code_depnum_ccdc_archive 'CCDC 822600' #TrackingRef '- compound12.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 Cl3 N Si2' _chemical_formula_weight 645.19 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0788(7) _cell_length_b 13.1075(9) _cell_length_c 13.1687(9) _cell_angle_alpha 90.754(3) _cell_angle_beta 108.006(4) _cell_angle_gamma 96.141(4) _cell_volume 1643.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 0.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 46831 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6423 _reflns_number_gt 5922 _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. The atoms of the SiCl3 and SiMe3 groups of the molecule were found to be disordered over two sites. This disorder was successfully modelled. The DFIX comand of SHELX-L was used to constrain the Si-C distances in both disordered sets, giving rise to the 6 constraints used in the final refinement cycle. ; _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^)+(0.0303P)^2^+1.1296P] 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 6423 _refine_ls_number_parameters 441 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1021 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.2881(4) 0.7532(5) 0.3032(5) 0.0367(10) Uani 0.454(2) 1 d P A 1 Cl1A Cl 0.6882(3) 0.5585(2) 0.1885(2) 0.0322(6) Uani 0.546(2) 1 d P A 2 Cl2 Cl 0.3837(5) 0.8994(5) 0.1389(3) 0.0327(10) Uani 0.454(2) 1 d P A 1 Cl2A Cl 0.3872(3) 0.6363(2) 0.05625(17) 0.0372(5) Uani 0.546(2) 1 d P A 2 Cl3 Cl 0.5463(5) 0.9360(4) 0.3938(4) 0.0300(9) Uani 0.454(2) 1 d P A 1 Cl3A Cl 0.4211(3) 0.5257(2) 0.2767(3) 0.0319(6) Uani 0.546(2) 1 d P A 2 Si1 Si 0.52250(6) 0.62368(5) 0.20292(5) 0.02562(15) Uani 1 1 d D . . Si2 Si 0.45657(6) 0.82766(4) 0.27437(5) 0.02370(15) Uani 1 1 d D . . N1 N 0.57794(16) 0.74316(12) 0.27048(13) 0.0201(4) Uani 1 1 d . A . C1 C 0.72638(19) 0.77594(15) 0.32839(15) 0.0185(4) Uani 1 1 d . . . C2 C 0.78702(19) 0.74627(15) 0.43324(15) 0.0192(4) Uani 1 1 d . A . C3 C 0.9261(2) 0.78362(15) 0.48771(16) 0.0212(4) Uani 1 1 d . . . H3 H 0.9680 0.7615 0.5576 0.025 Uiso 1 1 calc R A . C4 C 1.00559(19) 0.85178(15) 0.44391(16) 0.0214(4) Uani 1 1 d . A . C5 C 0.9443(2) 0.87907(16) 0.34034(16) 0.0229(4) Uani 1 1 d . . . H5 H 0.9973 0.9255 0.3088 0.028 Uiso 1 1 calc R A . C6 C 0.8076(2) 0.84104(15) 0.28047(16) 0.0208(4) Uani 1 1 d . A . C7 C 1.1529(2) 0.89583(18) 0.50696(18) 0.0314(5) Uani 1 1 d . . . H7A H 1.2190 0.8482 0.5008 0.047 Uiso 1 1 calc R A . H7B H 1.1595 0.9061 0.5823 0.047 Uiso 1 1 calc R . . H7C H 1.1762 0.9619 0.4788 0.047 Uiso 1 1 calc R . . C8 C 0.7064(2) 0.67646(15) 0.49144(16) 0.0215(4) Uani 1 1 d . . . H8 H 0.6222 0.6414 0.4351 0.026 Uiso 1 1 calc R A . C9 C 0.6508(2) 0.73422(16) 0.56792(16) 0.0232(4) Uani 1 1 d . A . C10 C 0.7268(2) 0.81861(17) 0.63349(17) 0.0287(5) Uani 1 1 d . . . H10 H 0.8164 0.8448 0.6291 0.034 Uiso 1 1 calc R A . C11 C 0.6733(3) 0.86460(19) 0.70484(19) 0.0350(5) Uani 1 1 d . A . H11 H 0.7265 0.9218 0.7495 0.042 Uiso 1 1 calc R . . C12 C 0.5431(3) 0.8282(2) 0.7118(2) 0.0393(6) Uani 1 1 d . . . H12 H 0.5064 0.8602 0.7608 0.047 Uiso 1 1 calc R A . C13 C 0.4666(3) 0.7450(2) 0.6472(2) 0.0383(6) Uani 1 1 d . A . H13 H 0.3767 0.7197 0.6516 0.046 Uiso 1 1 calc R . . C14 C 0.5201(2) 0.69813(18) 0.57587(18) 0.0302(5) Uani 1 1 d . . . H14 H 0.4667 0.6406 0.5319 0.036 Uiso 1 1 calc R A . C15 C 0.7914(2) 0.59152(16) 0.54623(16) 0.0225(4) Uani 1 1 d . A . C16 C 0.7890(2) 0.50262(17) 0.48732(19) 0.0298(5) Uani 1 1 d . . . H16 H 0.7332 0.4952 0.4143 0.036 Uiso 1 1 calc R A . C17 C 0.8664(2) 0.42438(18) 0.5330(2) 0.0360(6) Uani 1 1 d . A . H17 H 0.8628 0.3639 0.4913 0.043 Uiso 1 1 calc R . . C18 C 0.9484(2) 0.43389(18) 0.6385(2) 0.0355(6) Uani 1 1 d . . . H18 H 1.0024 0.3806 0.6695 0.043 Uiso 1 1 calc R A . C19 C 0.9514(2) 0.5215(2) 0.69863(19) 0.0368(6) Uani 1 1 d . A . H19 H 1.0076 0.5283 0.7716 0.044 Uiso 1 1 calc R . . C20 C 0.8728(2) 0.60007(18) 0.65346(18) 0.0306(5) Uani 1 1 d . . . H20 H 0.8748 0.6597 0.6959 0.037 Uiso 1 1 calc R A . C21 C 0.7552(2) 0.86775(16) 0.16302(16) 0.0233(4) Uani 1 1 d . . . H21 H 0.6503 0.8603 0.1416 0.028 Uiso 1 1 calc R A . C22 C 0.8030(2) 0.98023(16) 0.14937(16) 0.0246(4) Uani 1 1 d . A . C23 C 0.9126(2) 1.01045(18) 0.10982(19) 0.0324(5) Uani 1 1 d . . . H23 H 0.9595 0.9598 0.0871 0.039 Uiso 1 1 calc R A . C24 C 0.9549(3) 1.11388(19) 0.1029(2) 0.0377(6) Uani 1 1 d . A . H24 H 1.0311 1.1332 0.0764 0.045 Uiso 1 1 calc R . . C25 C 0.8876(3) 1.18800(19) 0.13382(19) 0.0377(6) Uani 1 1 d . . . H25 H 0.9162 1.2586 0.1281 0.045 Uiso 1 1 calc R A . C26 C 0.7784(3) 1.1595(2) 0.1733(2) 0.0463(7) Uani 1 1 d . A . H26 H 0.7312 1.2105 0.1951 0.056 Uiso 1 1 calc R . . C27 C 0.7373(3) 1.05625(19) 0.1811(2) 0.0393(6) Uani 1 1 d . . . H27 H 0.6622 1.0374 0.2089 0.047 Uiso 1 1 calc R A . C28 C 0.7941(2) 0.79178(16) 0.09163(16) 0.0254(5) Uani 1 1 d . A . C29 C 0.7012(3) 0.76493(18) -0.01026(18) 0.0351(5) Uani 1 1 d . . . H29 H 0.6171 0.7965 -0.0347 0.042 Uiso 1 1 calc R A . C30 C 0.7291(3) 0.6933(2) -0.0763(2) 0.0437(6) Uani 1 1 d . A . H30 H 0.6644 0.6763 -0.1456 0.052 Uiso 1 1 calc R . . C31 C 0.8499(3) 0.64631(19) -0.0426(2) 0.0413(6) Uani 1 1 d . . . H31 H 0.8675 0.5954 -0.0873 0.050 Uiso 1 1 calc R A . C32 C 0.9455(3) 0.67395(19) 0.0570(2) 0.0370(6) Uani 1 1 d . A . H32 H 1.0307 0.6435 0.0801 0.044 Uiso 1 1 calc R . . C33 C 0.9173(2) 0.74612(18) 0.12333(18) 0.0305(5) Uani 1 1 d . . . H33 H 0.9836 0.7645 0.1917 0.037 Uiso 1 1 calc R A . C34 C 0.6721(15) 0.5608(14) 0.1867(17) 0.079(7) Uani 0.454(2) 1 d PD A 1 H34A H 0.7076 0.5961 0.1335 0.119 Uiso 0.454(2) 1 calc PR A 1 H34B H 0.6403 0.4887 0.1628 0.119 Uiso 0.454(2) 1 calc PR A 1 H34C H 0.7473 0.5645 0.2553 0.119 Uiso 0.454(2) 1 calc PR A 1 C34A C 0.2978(15) 0.7569(17) 0.2953(18) 0.052(6) Uani 0.546(2) 1 d PD A 2 H34D H 0.2523 0.7070 0.2353 0.079 Uiso 0.546(2) 1 calc PR A 2 H34E H 0.2322 0.8056 0.2996 0.079 Uiso 0.546(2) 1 calc PR A 2 H34F H 0.3253 0.7208 0.3620 0.079 Uiso 0.546(2) 1 calc PR A 2 C35 C 0.4009(18) 0.6400(16) 0.0669(8) 0.083(8) Uani 0.454(2) 1 d PD A 1 H35A H 0.3184 0.6698 0.0730 0.124 Uiso 0.454(2) 1 calc PR A 1 H35B H 0.3711 0.5730 0.0281 0.124 Uiso 0.454(2) 1 calc PR A 1 H35C H 0.4492 0.6858 0.0280 0.124 Uiso 0.454(2) 1 calc PR A 1 C35A C 0.388(2) 0.8921(16) 0.1464(10) 0.050(6) Uani 0.546(2) 1 d PD A 2 H35D H 0.4636 0.9391 0.1346 0.075 Uiso 0.546(2) 1 calc PR A 2 H35E H 0.3115 0.9309 0.1500 0.075 Uiso 0.546(2) 1 calc PR A 2 H35F H 0.3525 0.8401 0.0872 0.075 Uiso 0.546(2) 1 calc PR A 2 C36 C 0.4255(18) 0.5305(12) 0.2681(15) 0.064(7) Uani 0.454(2) 1 d PD A 1 H36A H 0.4928 0.4985 0.3256 0.096 Uiso 0.454(2) 1 calc PR A 1 H36B H 0.3680 0.4773 0.2151 0.096 Uiso 0.454(2) 1 calc PR A 1 H36C H 0.3647 0.5666 0.2980 0.096 Uiso 0.454(2) 1 calc PR A 1 C36A C 0.5406(19) 0.9256(11) 0.3848(11) 0.036(5) Uani 0.546(2) 1 d PD A 2 H36D H 0.5734 0.8914 0.4523 0.054 Uiso 0.546(2) 1 calc PR A 2 H36E H 0.4721 0.9717 0.3897 0.054 Uiso 0.546(2) 1 calc PR A 2 H36F H 0.6206 0.9654 0.3709 0.054 Uiso 0.546(2) 1 calc PR A 2 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 0.0171(13) 0.041(2) 0.0526(19) 0.0019(14) 0.0148(13) -0.0044(11) Cl1A 0.0331(8) 0.0259(12) 0.0394(14) -0.0055(10) 0.0142(8) 0.0042(8) Cl2 0.0324(18) 0.0406(19) 0.0217(14) 0.0088(13) 0.0000(12) 0.0147(14) Cl2A 0.0367(9) 0.0367(12) 0.0246(8) -0.0037(7) -0.0077(7) -0.0027(8) Cl3 0.0291(15) 0.0256(12) 0.0307(14) -0.0084(10) 0.0035(10) 0.0016(10) Cl3A 0.0329(11) 0.0232(11) 0.0368(12) 0.0005(9) 0.0110(9) -0.0101(8) Si1 0.0263(3) 0.0224(3) 0.0246(3) -0.0034(2) 0.0047(2) -0.0030(2) Si2 0.0196(3) 0.0237(3) 0.0255(3) -0.0012(2) 0.0048(2) -0.0007(2) N1 0.0170(8) 0.0191(9) 0.0201(8) -0.0008(7) 0.0021(6) -0.0039(6) C1 0.0160(9) 0.0173(10) 0.0200(10) -0.0028(8) 0.0040(7) -0.0014(7) C2 0.0204(9) 0.0175(10) 0.0206(10) 0.0009(8) 0.0081(8) 0.0009(8) C3 0.0214(9) 0.0223(10) 0.0183(10) 0.0008(8) 0.0038(8) 0.0020(8) C4 0.0182(9) 0.0214(10) 0.0230(10) -0.0027(8) 0.0055(8) -0.0013(8) C5 0.0217(10) 0.0227(10) 0.0240(10) 0.0003(9) 0.0090(8) -0.0046(8) C6 0.0219(9) 0.0200(10) 0.0197(10) 0.0013(8) 0.0057(8) 0.0007(8) C7 0.0221(10) 0.0376(13) 0.0288(12) -0.0008(10) 0.0030(9) -0.0072(9) C8 0.0190(9) 0.0230(11) 0.0216(10) 0.0027(8) 0.0065(8) -0.0024(8) C9 0.0250(10) 0.0240(11) 0.0214(10) 0.0078(9) 0.0071(8) 0.0056(8) C10 0.0298(11) 0.0288(12) 0.0286(11) 0.0036(10) 0.0103(9) 0.0041(9) C11 0.0429(13) 0.0307(13) 0.0315(12) -0.0004(10) 0.0101(10) 0.0096(10) C12 0.0479(14) 0.0431(15) 0.0375(14) 0.0092(12) 0.0229(12) 0.0217(12) C13 0.0335(12) 0.0458(15) 0.0444(14) 0.0128(12) 0.0213(11) 0.0137(11) C14 0.0267(11) 0.0308(12) 0.0347(12) 0.0083(10) 0.0114(9) 0.0036(9) C15 0.0204(9) 0.0215(10) 0.0270(11) 0.0062(9) 0.0101(8) -0.0008(8) C16 0.0279(11) 0.0257(12) 0.0343(12) 0.0012(10) 0.0091(9) -0.0015(9) C17 0.0319(12) 0.0231(12) 0.0528(15) 0.0018(11) 0.0134(11) 0.0024(9) C18 0.0271(11) 0.0284(12) 0.0534(15) 0.0157(12) 0.0142(11) 0.0070(9) C19 0.0354(12) 0.0439(15) 0.0312(13) 0.0136(11) 0.0081(10) 0.0106(11) C20 0.0343(12) 0.0311(12) 0.0263(11) 0.0044(10) 0.0081(9) 0.0069(9) C21 0.0217(10) 0.0262(11) 0.0209(10) 0.0025(9) 0.0062(8) -0.0016(8) C22 0.0270(10) 0.0255(11) 0.0190(10) 0.0049(9) 0.0047(8) -0.0003(8) C23 0.0340(12) 0.0290(12) 0.0371(13) 0.0018(10) 0.0169(10) -0.0019(9) C24 0.0407(13) 0.0356(14) 0.0385(13) 0.0054(11) 0.0185(11) -0.0069(11) C25 0.0519(15) 0.0269(12) 0.0317(13) 0.0041(10) 0.0125(11) -0.0060(11) C26 0.0622(17) 0.0301(14) 0.0577(17) 0.0050(13) 0.0344(14) 0.0063(12) C27 0.0460(14) 0.0322(13) 0.0485(15) 0.0066(12) 0.0283(12) 0.0022(11) C28 0.0299(11) 0.0249(11) 0.0206(10) 0.0043(9) 0.0090(9) -0.0035(9) C29 0.0420(13) 0.0311(13) 0.0262(12) 0.0023(10) 0.0029(10) 0.0010(10) C30 0.0636(17) 0.0352(14) 0.0256(12) -0.0049(11) 0.0065(12) -0.0003(12) C31 0.0651(17) 0.0285(13) 0.0342(14) -0.0027(11) 0.0236(13) -0.0011(12) C32 0.0428(13) 0.0333(13) 0.0405(14) 0.0025(11) 0.0218(11) 0.0032(11) C33 0.0313(11) 0.0339(13) 0.0260(11) 0.0009(10) 0.0100(9) -0.0010(9) C34 0.113(14) 0.056(11) 0.058(11) -0.009(8) 0.025(10) -0.031(8) C34A 0.038(8) 0.044(8) 0.070(11) -0.005(7) 0.013(6) -0.005(6) C35 0.071(11) 0.070(11) 0.080(12) -0.033(8) -0.002(8) -0.031(7) C35A 0.049(9) 0.037(8) 0.056(10) -0.010(7) 0.007(7) 0.001(6) C36 0.074(11) 0.057(11) 0.057(11) -0.022(7) 0.028(8) -0.036(8) C36A 0.043(8) 0.033(7) 0.033(7) 0.014(4) 0.007(5) 0.024(5) _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 Si2 2.008(3) . ? Cl1A Si1 2.0128(17) . ? Cl2 Si2 1.997(3) . ? Cl2A Si1 2.011(2) . ? Cl3 Si2 2.024(4) . ? Cl3A Si1 2.001(2) . ? Si1 N1 1.7392(17) . ? Si1 C34 1.860(7) . ? Si1 C35 1.862(7) . ? Si1 C36 1.865(7) . ? Si2 N1 1.7472(17) . ? Si2 C36A 1.854(7) . ? Si2 C34A 1.860(7) . ? Si2 C35A 1.864(7) . ? N1 C1 1.467(2) . ? C1 C2 1.405(3) . ? C1 C6 1.407(3) . ? C2 C3 1.393(3) . ? C2 C8 1.526(3) . ? C3 C4 1.385(3) . ? C4 C5 1.382(3) . ? C4 C7 1.507(3) . ? C5 C6 1.392(3) . ? C6 C21 1.531(3) . ? C8 C9 1.523(3) . ? C8 C15 1.529(3) . ? C9 C14 1.387(3) . ? C9 C10 1.393(3) . ? C10 C11 1.381(3) . ? C11 C12 1.378(3) . ? C12 C13 1.377(4) . ? C13 C14 1.386(3) . ? C15 C16 1.385(3) . ? C15 C20 1.393(3) . ? C16 C17 1.385(3) . ? C17 C18 1.375(4) . ? C18 C19 1.379(4) . ? C19 C20 1.393(3) . ? C21 C28 1.522(3) . ? C21 C22 1.532(3) . ? C22 C27 1.380(3) . ? C22 C23 1.384(3) . ? C23 C24 1.390(3) . ? C24 C25 1.367(4) . ? C25 C26 1.376(3) . ? C26 C27 1.387(3) . ? C28 C33 1.385(3) . ? C28 C29 1.393(3) . ? C29 C30 1.380(4) . ? C30 C31 1.376(4) . ? C31 C32 1.383(4) . ? C32 C33 1.389(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C34 111.9(6) . . ? N1 Si1 C35 109.3(6) . . ? C34 Si1 C35 107.6(9) . . ? N1 Si1 C36 114.4(7) . . ? C34 Si1 C36 106.7(9) . . ? C35 Si1 C36 106.5(9) . . ? N1 Si1 Cl3A 113.04(12) . . ? C34 Si1 Cl3A 107.0(6) . . ? C35 Si1 Cl3A 107.8(7) . . ? C36 Si1 Cl3A 1.5(8) . . ? N1 Si1 Cl2A 111.04(10) . . ? C34 Si1 Cl2A 107.7(7) . . ? C35 Si1 Cl2A 2.1(7) . . ? C36 Si1 Cl2A 104.6(6) . . ? Cl3A Si1 Cl2A 105.87(13) . . ? N1 Si1 Cl1A 110.29(11) . . ? C34 Si1 Cl1A 1.6(7) . . ? C35 Si1 Cl1A 108.8(7) . . ? C36 Si1 Cl1A 107.3(6) . . ? Cl3A Si1 Cl1A 107.51(12) . . ? Cl2A Si1 Cl1A 108.89(12) . . ? N1 Si2 C36A 108.8(6) . . ? N1 Si2 C34A 110.5(8) . . ? C36A Si2 C34A 110.0(10) . . ? N1 Si2 C35A 113.3(6) . . ? C36A Si2 C35A 109.8(9) . . ? C34A Si2 C35A 104.4(9) . . ? N1 Si2 Cl2 114.03(16) . . ? C36A Si2 Cl2 108.7(6) . . ? C34A Si2 Cl2 104.7(7) . . ? C35A Si2 Cl2 1.1(9) . . ? N1 Si2 Cl1 111.0(2) . . ? C36A Si2 Cl1 107.8(7) . . ? C34A Si2 Cl1 2.3(9) . . ? C35A Si2 Cl1 106.1(7) . . ? Cl2 Si2 Cl1 106.4(2) . . ? N1 Si2 Cl3 109.54(18) . . ? C36A Si2 Cl3 0.8(8) . . ? C34A Si2 Cl3 109.9(7) . . ? C35A Si2 Cl3 109.1(7) . . ? Cl2 Si2 Cl3 108.0(3) . . ? Cl1 Si2 Cl3 107.7(3) . . ? C1 N1 Si1 121.86(13) . . ? C1 N1 Si2 117.48(13) . . ? Si1 N1 Si2 120.64(9) . . ? C2 C1 C6 119.49(17) . . ? C2 C1 N1 120.55(16) . . ? C6 C1 N1 119.92(17) . . ? C3 C2 C1 118.82(17) . . ? C3 C2 C8 118.23(17) . . ? C1 C2 C8 122.94(17) . . ? C4 C3 C2 122.55(18) . . ? C5 C4 C3 117.56(17) . . ? C5 C4 C7 120.97(18) . . ? C3 C4 C7 121.46(18) . . ? C4 C5 C6 122.42(18) . . ? C5 C6 C1 119.02(18) . . ? C5 C6 C21 118.05(17) . . ? C1 C6 C21 122.86(17) . . ? C9 C8 C2 113.72(16) . . ? C9 C8 C15 111.84(16) . . ? C2 C8 C15 111.64(15) . . ? C14 C9 C10 118.3(2) . . ? C14 C9 C8 118.16(19) . . ? C10 C9 C8 123.46(18) . . ? C11 C10 C9 120.6(2) . . ? C12 C11 C10 120.5(2) . . ? C13 C12 C11 119.6(2) . . ? C12 C13 C14 120.2(2) . . ? C13 C14 C9 120.8(2) . . ? C16 C15 C20 118.3(2) . . ? C16 C15 C8 119.13(18) . . ? C20 C15 C8 122.60(19) . . ? C15 C16 C17 121.2(2) . . ? C18 C17 C16 120.3(2) . . ? C17 C18 C19 119.3(2) . . ? C18 C19 C20 120.6(2) . . ? C15 C20 C19 120.2(2) . . ? C28 C21 C6 111.29(17) . . ? C28 C21 C22 113.88(16) . . ? C6 C21 C22 110.91(17) . . ? C27 C22 C23 117.7(2) . . ? C27 C22 C21 118.96(18) . . ? C23 C22 C21 123.3(2) . . ? C22 C23 C24 120.9(2) . . ? C25 C24 C23 120.6(2) . . ? C24 C25 C26 119.5(2) . . ? C25 C26 C27 119.8(2) . . ? C22 C27 C26 121.6(2) . . ? C33 C28 C29 117.7(2) . . ? C33 C28 C21 123.24(19) . . ? C29 C28 C21 119.0(2) . . ? C30 C29 C28 121.1(2) . . ? C31 C30 C29 120.5(2) . . ? C30 C31 C32 119.3(2) . . ? C31 C32 C33 120.1(2) . . ? C28 C33 C32 121.2(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.322 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.047 # Attachment '- compound13.CIF' data_compound13 _database_code_depnum_ccdc_archive 'CCDC 822601' #TrackingRef '- compound13.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H40 Cl3 N Si2' _chemical_formula_weight 769.32 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4843(7) _cell_length_b 12.8042(8) _cell_length_c 14.8588(9) _cell_angle_alpha 82.135(5) _cell_angle_beta 85.347(5) _cell_angle_gamma 80.847(5) _cell_volume 1947.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 0.332 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.959 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 12610 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0942 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6849 _reflns_number_gt 4998 _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^)+(0.0622P)^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 6849 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1424 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.04337(9) 0.33259(7) 0.22233(6) 0.0229(2) Uani 1 1 d . . . Si1 Si 0.20596(10) 0.22800(7) 0.19687(6) 0.0161(2) Uani 1 1 d . . . N1 N 0.3465(3) 0.2625(2) 0.22336(16) 0.0133(6) Uani 1 1 d . . . C1 C 0.4172(3) 0.2001(2) 0.2990(2) 0.0132(7) Uani 1 1 d . . . Cl2 Cl 0.20726(9) 0.21679(7) 0.06119(5) 0.0224(2) Uani 1 1 d . . . Si2 Si 0.41883(10) 0.36783(7) 0.15681(6) 0.0159(2) Uani 1 1 d . . . C2 C 0.3855(3) 0.2240(2) 0.3885(2) 0.0146(7) Uani 1 1 d . . . Cl3 Cl 0.17768(9) 0.08607(7) 0.26758(5) 0.0213(2) Uani 1 1 d . . . C3 C 0.4702(4) 0.1791(3) 0.4545(2) 0.0179(8) Uani 1 1 d . . . H3 H 0.4513 0.1972 0.5146 0.022 Uiso 1 1 calc R . . C4 C 0.5819(4) 0.1085(3) 0.4372(2) 0.0175(8) Uani 1 1 d . . . C5 C 0.6023(3) 0.0767(3) 0.3506(2) 0.0157(8) Uani 1 1 d . . . H5 H 0.6739 0.0238 0.3387 0.019 Uiso 1 1 calc R . . C6 C 0.5214(3) 0.1200(2) 0.2810(2) 0.0139(7) Uani 1 1 d . . . C7 C 0.6760(4) 0.0661(3) 0.5097(2) 0.0222(8) Uani 1 1 d . . . H7A H 0.6887 0.1241 0.5432 0.033 Uiso 1 1 calc R . . H7B H 0.7590 0.0364 0.4812 0.033 Uiso 1 1 calc R . . H7C H 0.6414 0.0101 0.5518 0.033 Uiso 1 1 calc R . . C8 C 0.2572(3) 0.2921(2) 0.4138(2) 0.0161(8) Uani 1 1 d . . . H8 H 0.1995 0.2910 0.3636 0.019 Uiso 1 1 calc R . . C9 C 0.1897(3) 0.2413(3) 0.5003(2) 0.0157(8) Uani 1 1 d . . . C10 C 0.2188(4) 0.2583(3) 0.5865(2) 0.0206(8) Uani 1 1 d . . . H10 H 0.2812 0.3029 0.5923 0.025 Uiso 1 1 calc R . . C11 C 0.1578(4) 0.2110(3) 0.6633(2) 0.0254(9) Uani 1 1 d . . . H11 H 0.1795 0.2224 0.7217 0.030 Uiso 1 1 calc R . . C12 C 0.0654(4) 0.1473(3) 0.6565(2) 0.0268(9) Uani 1 1 d . . . H12 H 0.0242 0.1143 0.7098 0.032 Uiso 1 1 calc R . . C13 C 0.0333(4) 0.1320(3) 0.5716(2) 0.0282(9) Uani 1 1 d . . . H13 H -0.0310 0.0890 0.5663 0.034 Uiso 1 1 calc R . . C14 C 0.0947(4) 0.1790(3) 0.4944(2) 0.0209(8) Uani 1 1 d . . . H14 H 0.0714 0.1684 0.4362 0.025 Uiso 1 1 calc R . . C15 C 0.2615(4) 0.4098(3) 0.4192(2) 0.0185(8) Uani 1 1 d . . . C16 C 0.3737(4) 0.4514(3) 0.4230(2) 0.0220(8) Uani 1 1 d . . . H16 H 0.4547 0.4060 0.4226 0.026 Uiso 1 1 calc R . . C17 C 0.3688(4) 0.5606(3) 0.4277(2) 0.0261(9) Uani 1 1 d . . . H17 H 0.4465 0.5893 0.4300 0.031 Uiso 1 1 calc R . . C18 C 0.2511(4) 0.6265(3) 0.4290(2) 0.0289(10) Uani 1 1 d . . . H18 H 0.2480 0.7005 0.4321 0.035 Uiso 1 1 calc R . . C19 C 0.1388(4) 0.5857(3) 0.4259(2) 0.0288(9) Uani 1 1 d . . . H19 H 0.0578 0.6312 0.4270 0.035 Uiso 1 1 calc R . . C20 C 0.1435(4) 0.4773(3) 0.4212(2) 0.0236(9) Uani 1 1 d . . . H20 H 0.0654 0.4491 0.4193 0.028 Uiso 1 1 calc R . . C21 C 0.5466(3) 0.0766(3) 0.1889(2) 0.0156(8) Uani 1 1 d . . . H21 H 0.5078 0.1347 0.1427 0.019 Uiso 1 1 calc R . . C22 C 0.4761(3) -0.0185(3) 0.1859(2) 0.0172(8) Uani 1 1 d . . . C23 C 0.4125(4) -0.0245(3) 0.1087(2) 0.0223(8) Uani 1 1 d . . . H23 H 0.4129 0.0310 0.0592 0.027 Uiso 1 1 calc R . . C24 C 0.3485(4) -0.1101(3) 0.1023(3) 0.0311(10) Uani 1 1 d . . . H24 H 0.3056 -0.1132 0.0491 0.037 Uiso 1 1 calc R . . C25 C 0.3480(4) -0.1900(3) 0.1740(3) 0.0374(11) Uani 1 1 d . . . H25 H 0.3028 -0.2480 0.1709 0.045 Uiso 1 1 calc R . . C26 C 0.4128(4) -0.1867(3) 0.2505(3) 0.0348(11) Uani 1 1 d . . . H26 H 0.4140 -0.2433 0.2992 0.042 Uiso 1 1 calc R . . C27 C 0.4764(4) -0.1007(3) 0.2567(2) 0.0241(9) Uani 1 1 d . . . H27 H 0.5202 -0.0985 0.3098 0.029 Uiso 1 1 calc R . . C28 C 0.6890(4) 0.0534(3) 0.1604(2) 0.0163(8) Uani 1 1 d . . . C29 C 0.7468(4) -0.0441(3) 0.1332(2) 0.0213(8) Uani 1 1 d . . . H29 H 0.6960 -0.0991 0.1323 0.026 Uiso 1 1 calc R . . C30 C 0.8777(4) -0.0614(3) 0.1073(2) 0.0265(9) Uani 1 1 d . . . H30 H 0.9155 -0.1282 0.0889 0.032 Uiso 1 1 calc R . . C31 C 0.9534(4) 0.0166(3) 0.1081(2) 0.0260(9) Uani 1 1 d . . . H31 H 1.0436 0.0033 0.0923 0.031 Uiso 1 1 calc R . . C32 C 0.8969(4) 0.1150(3) 0.1322(2) 0.0261(9) Uani 1 1 d . . . H32 H 0.9473 0.1708 0.1301 0.031 Uiso 1 1 calc R . . C33 C 0.7676(4) 0.1315(3) 0.1590(2) 0.0223(8) Uani 1 1 d . . . H33 H 0.7305 0.1985 0.1773 0.027 Uiso 1 1 calc R . . C34 C 0.5080(4) 0.3263(3) 0.0515(2) 0.0225(8) Uani 1 1 d . . . H34A H 0.5858 0.2759 0.0675 0.034 Uiso 1 1 calc R . . H34B H 0.5330 0.3891 0.0129 0.034 Uiso 1 1 calc R . . H34C H 0.4523 0.2921 0.0185 0.034 Uiso 1 1 calc R . . C35 C 0.2835(4) 0.4753(3) 0.1228(2) 0.0197(8) Uani 1 1 d . . . C36 C 0.2189(4) 0.5402(3) 0.1857(2) 0.0250(9) Uani 1 1 d . . . H36 H 0.2472 0.5307 0.2458 0.030 Uiso 1 1 calc R . . C37 C 0.1152(4) 0.6175(3) 0.1630(3) 0.0377(11) Uani 1 1 d . . . H37 H 0.0733 0.6609 0.2069 0.045 Uiso 1 1 calc R . . C38 C 0.0726(5) 0.6315(3) 0.0758(3) 0.0508(14) Uani 1 1 d . . . H38 H 0.0003 0.6838 0.0601 0.061 Uiso 1 1 calc R . . C39 C 0.1348(5) 0.5697(3) 0.0121(3) 0.0462(13) Uani 1 1 d . . . H39 H 0.1058 0.5797 -0.0479 0.055 Uiso 1 1 calc R . . C40 C 0.2389(4) 0.4935(3) 0.0350(2) 0.0293(10) Uani 1 1 d . . . H40 H 0.2816 0.4520 -0.0099 0.035 Uiso 1 1 calc R . . C41 C 0.5378(4) 0.4223(3) 0.2193(2) 0.0188(8) Uani 1 1 d . . . C42 C 0.6275(4) 0.3635(3) 0.2786(2) 0.0201(8) Uani 1 1 d . . . H42 H 0.6229 0.2901 0.2970 0.024 Uiso 1 1 calc R . . C43 C 0.7231(4) 0.4092(3) 0.3111(2) 0.0260(9) Uani 1 1 d . . . H43 H 0.7824 0.3676 0.3517 0.031 Uiso 1 1 calc R . . C44 C 0.7316(4) 0.5163(3) 0.2839(3) 0.0314(10) Uani 1 1 d . . . H44 H 0.7978 0.5477 0.3050 0.038 Uiso 1 1 calc R . . C45 C 0.6443(4) 0.5765(3) 0.2264(3) 0.0340(10) Uani 1 1 d . . . H45 H 0.6499 0.6498 0.2081 0.041 Uiso 1 1 calc R . . C46 C 0.5479(4) 0.5305(3) 0.1952(2) 0.0234(9) Uani 1 1 d . . . H46 H 0.4872 0.5735 0.1564 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0147(5) 0.0232(5) 0.0302(5) -0.0078(4) -0.0031(4) 0.0036(4) Si1 0.0150(6) 0.0163(5) 0.0166(5) -0.0030(4) -0.0011(4) -0.0001(4) N1 0.0113(17) 0.0121(14) 0.0153(13) -0.0037(11) -0.0001(11) 0.0031(12) C1 0.0088(19) 0.0137(17) 0.0172(16) -0.0010(13) -0.0012(14) -0.0029(15) Cl2 0.0215(6) 0.0272(5) 0.0193(4) -0.0050(4) -0.0044(4) -0.0029(4) Si2 0.0155(6) 0.0155(5) 0.0160(5) -0.0023(4) -0.0003(4) -0.0005(4) C2 0.015(2) 0.0109(17) 0.0181(17) -0.0021(13) -0.0007(14) -0.0015(15) Cl3 0.0207(6) 0.0190(5) 0.0242(4) -0.0020(4) 0.0004(4) -0.0042(4) C3 0.019(2) 0.0173(18) 0.0165(17) -0.0054(14) -0.0001(15) 0.0012(16) C4 0.017(2) 0.0152(17) 0.0188(17) -0.0017(14) -0.0016(15) 0.0008(16) C5 0.011(2) 0.0131(17) 0.0210(17) -0.0050(14) 0.0030(14) 0.0040(15) C6 0.013(2) 0.0118(17) 0.0162(16) -0.0038(13) 0.0029(14) -0.0012(15) C7 0.019(2) 0.025(2) 0.0204(17) -0.0034(15) -0.0032(15) 0.0048(17) C8 0.018(2) 0.0150(18) 0.0138(16) -0.0022(13) -0.0016(14) 0.0037(16) C9 0.009(2) 0.0122(17) 0.0225(18) -0.0042(14) 0.0024(14) 0.0071(15) C10 0.019(2) 0.0203(19) 0.0210(18) -0.0015(15) -0.0034(15) 0.0030(17) C11 0.026(2) 0.026(2) 0.0203(18) -0.0010(15) -0.0006(16) 0.0072(18) C12 0.022(2) 0.024(2) 0.028(2) 0.0050(16) 0.0071(17) 0.0045(18) C13 0.020(2) 0.022(2) 0.042(2) -0.0049(17) 0.0023(18) -0.0029(18) C14 0.019(2) 0.0187(19) 0.0241(18) -0.0063(15) -0.0014(16) 0.0025(17) C15 0.018(2) 0.0171(18) 0.0167(17) -0.0012(14) 0.0030(15) 0.0044(16) C16 0.025(2) 0.0209(19) 0.0184(17) -0.0061(15) 0.0007(15) 0.0041(17) C17 0.031(3) 0.021(2) 0.0262(19) -0.0076(16) 0.0040(17) -0.0036(19) C18 0.040(3) 0.0144(19) 0.030(2) -0.0055(16) 0.0096(18) 0.0015(19) C19 0.029(3) 0.0167(19) 0.034(2) 0.0005(16) 0.0110(18) 0.0078(18) C20 0.024(2) 0.0187(19) 0.0233(18) 0.0004(15) 0.0065(16) 0.0032(17) C21 0.015(2) 0.0150(17) 0.0168(16) -0.0015(14) -0.0013(14) -0.0027(15) C22 0.013(2) 0.0159(18) 0.0218(17) -0.0069(14) 0.0051(15) 0.0017(15) C23 0.018(2) 0.0227(19) 0.0264(19) -0.0135(16) 0.0029(16) 0.0015(17) C24 0.026(3) 0.032(2) 0.039(2) -0.0206(19) 0.0052(18) -0.0042(19) C25 0.032(3) 0.027(2) 0.059(3) -0.023(2) 0.008(2) -0.014(2) C26 0.041(3) 0.021(2) 0.040(2) -0.0016(18) 0.014(2) -0.009(2) C27 0.025(2) 0.020(2) 0.0255(19) -0.0066(16) 0.0080(16) -0.0018(17) C28 0.017(2) 0.0188(18) 0.0118(16) -0.0030(14) 0.0009(14) 0.0006(16) C29 0.022(2) 0.024(2) 0.0188(17) -0.0072(15) -0.0011(15) -0.0039(17) C30 0.022(2) 0.030(2) 0.0266(19) -0.0121(17) 0.0011(17) 0.0070(18) C31 0.014(2) 0.043(2) 0.0200(18) -0.0075(17) 0.0002(15) 0.0008(19) C32 0.018(2) 0.036(2) 0.0270(19) -0.0122(17) 0.0011(16) -0.0074(19) C33 0.015(2) 0.026(2) 0.0261(19) -0.0097(16) 0.0041(16) -0.0032(17) C34 0.024(2) 0.0226(19) 0.0211(18) -0.0031(15) 0.0018(16) -0.0056(17) C35 0.022(2) 0.0154(18) 0.0214(18) 0.0016(14) -0.0027(15) -0.0055(16) C36 0.023(2) 0.0186(19) 0.034(2) -0.0007(16) -0.0043(17) -0.0035(18) C37 0.033(3) 0.020(2) 0.061(3) -0.0083(19) -0.013(2) 0.004(2) C38 0.048(3) 0.024(2) 0.080(3) -0.007(2) -0.036(3) 0.013(2) C39 0.056(4) 0.030(2) 0.053(3) 0.004(2) -0.035(3) 0.000(2) C40 0.035(3) 0.023(2) 0.031(2) 0.0001(16) -0.0118(18) -0.006(2) C41 0.018(2) 0.0194(19) 0.0191(17) -0.0045(15) 0.0048(15) -0.0037(16) C42 0.019(2) 0.0182(19) 0.0214(17) -0.0052(15) 0.0026(15) 0.0029(16) C43 0.017(2) 0.033(2) 0.030(2) -0.0131(17) -0.0030(16) 0.0022(18) C44 0.024(3) 0.030(2) 0.044(2) -0.0159(19) -0.0031(19) -0.008(2) C45 0.033(3) 0.025(2) 0.047(2) -0.0094(19) 0.000(2) -0.009(2) C46 0.025(2) 0.0209(19) 0.0234(18) -0.0007(15) -0.0001(16) -0.0030(18) _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 2.0372(13) . ? Si1 N1 1.694(3) . ? Si1 Cl3 2.0230(12) . ? Si1 Cl2 2.0395(11) . ? N1 C1 1.467(4) . ? N1 Si2 1.792(3) . ? C1 C2 1.407(4) . ? C1 C6 1.410(5) . ? Si2 C34 1.853(3) . ? Si2 C35 1.862(4) . ? Si2 C41 1.884(3) . ? C2 C3 1.380(5) . ? C2 C8 1.531(5) . ? C3 C4 1.390(5) . ? C3 H3 0.9500 . ? C4 C5 1.392(4) . ? C4 C7 1.506(5) . ? C5 C6 1.391(5) . ? C5 H5 0.9500 . ? C6 C21 1.534(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C15 1.528(4) . ? C8 C9 1.532(4) . ? C8 H8 1.0000 . ? C9 C14 1.387(5) . ? C9 C10 1.394(4) . ? C10 C11 1.377(5) . ? C10 H10 0.9500 . ? C11 C12 1.380(5) . ? C11 H11 0.9500 . ? C12 C13 1.378(5) . ? C12 H12 0.9500 . ? C13 C14 1.382(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.374(5) . ? C15 C20 1.393(5) . ? C16 C17 1.403(5) . ? C16 H16 0.9500 . ? C17 C18 1.380(6) . ? C17 H17 0.9500 . ? C18 C19 1.368(6) . ? C18 H18 0.9500 . ? C19 C20 1.392(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C28 1.512(5) . ? C21 C22 1.530(4) . ? C21 H21 1.0000 . ? C22 C27 1.382(5) . ? C22 C23 1.390(5) . ? C23 C24 1.390(5) . ? C23 H23 0.9500 . ? C24 C25 1.373(6) . ? C24 H24 0.9500 . ? C25 C26 1.380(6) . ? C25 H25 0.9500 . ? C26 C27 1.391(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.389(5) . ? C28 C29 1.396(5) . ? C29 C30 1.386(5) . ? C29 H29 0.9500 . ? C30 C31 1.373(5) . ? C30 H30 0.9500 . ? C31 C32 1.384(5) . ? C31 H31 0.9500 . ? C32 C33 1.374(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.398(5) . ? C35 C40 1.398(5) . ? C36 C37 1.379(6) . ? C36 H36 0.9500 . ? C37 C38 1.383(6) . ? C37 H37 0.9500 . ? C38 C39 1.374(7) . ? C38 H38 0.9500 . ? C39 C40 1.375(6) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.398(5) . ? C41 C46 1.402(5) . ? C42 C43 1.387(5) . ? C42 H42 0.9500 . ? C43 C44 1.390(5) . ? C43 H43 0.9500 . ? C44 C45 1.372(6) . ? C44 H44 0.9500 . ? C45 C46 1.387(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? 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 Cl3 110.34(10) . . ? N1 Si1 Cl1 115.60(10) . . ? Cl3 Si1 Cl1 106.30(6) . . ? N1 Si1 Cl2 111.03(10) . . ? Cl3 Si1 Cl2 108.78(5) . . ? Cl1 Si1 Cl2 104.41(5) . . ? C1 N1 Si1 119.6(2) . . ? C1 N1 Si2 118.1(2) . . ? Si1 N1 Si2 122.10(15) . . ? C2 C1 C6 120.2(3) . . ? C2 C1 N1 120.0(3) . . ? C6 C1 N1 119.7(3) . . ? N1 Si2 C34 112.82(14) . . ? N1 Si2 C35 106.45(15) . . ? C34 Si2 C35 107.84(16) . . ? N1 Si2 C41 113.67(13) . . ? C34 Si2 C41 106.04(16) . . ? C35 Si2 C41 109.91(15) . . ? C3 C2 C1 118.0(3) . . ? C3 C2 C8 120.5(3) . . ? C1 C2 C8 121.3(3) . . ? C2 C3 C4 123.1(3) . . ? C2 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C3 C4 C5 117.4(3) . . ? C3 C4 C7 121.5(3) . . ? C5 C4 C7 121.1(3) . . ? C6 C5 C4 122.1(3) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C1 118.4(3) . . ? C5 C6 C21 118.8(3) . . ? C1 C6 C21 122.8(3) . . ? 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 . . ? C15 C8 C9 110.7(3) . . ? C15 C8 C2 116.6(3) . . ? C9 C8 C2 111.7(3) . . ? C15 C8 H8 105.7 . . ? C9 C8 H8 105.7 . . ? C2 C8 H8 105.7 . . ? C14 C9 C10 118.2(3) . . ? C14 C9 C8 120.3(3) . . ? C10 C9 C8 121.5(3) . . ? C11 C10 C9 120.5(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.7(3) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 119.4(3) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 120.1(3) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C9 121.1(3) . . ? C13 C14 H14 119.4 . . ? C9 C14 H14 119.4 . . ? C16 C15 C20 119.1(3) . . ? C16 C15 C8 123.9(3) . . ? C20 C15 C8 117.0(3) . . ? C15 C16 C17 120.1(4) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 120.0(4) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C17 120.3(3) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.8(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C15 120.7(4) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? C28 C21 C22 112.5(3) . . ? C28 C21 C6 113.1(3) . . ? C22 C21 C6 111.7(3) . . ? C28 C21 H21 106.3 . . ? C22 C21 H21 106.3 . . ? C6 C21 H21 106.3 . . ? C27 C22 C23 118.6(3) . . ? C27 C22 C21 122.1(3) . . ? C23 C22 C21 119.2(3) . . ? C24 C23 C22 121.3(3) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C25 C24 C23 119.2(4) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 120.2(4) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C22 C27 C26 120.3(4) . . ? C22 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C33 C28 C29 117.2(3) . . ? C33 C28 C21 120.1(3) . . ? C29 C28 C21 122.7(3) . . ? C30 C29 C28 120.5(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C31 C30 C29 120.9(3) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 119.3(4) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C33 C32 C31 119.7(4) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C28 122.3(3) . . ? C32 C33 H33 118.9 . . ? C28 C33 H33 118.9 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 116.7(4) . . ? C36 C35 Si2 120.8(3) . . ? C40 C35 Si2 122.4(3) . . ? C37 C36 C35 121.8(3) . . ? C37 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C36 C37 C38 119.6(4) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C39 C38 C37 120.0(4) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 120.1(4) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C35 121.8(4) . . ? C39 C40 H40 119.1 . . ? C35 C40 H40 119.1 . . ? C42 C41 C46 116.7(3) . . ? C42 C41 Si2 126.5(3) . . ? C46 C41 Si2 116.2(3) . . ? C43 C42 C41 121.8(3) . . ? C43 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C42 C43 C44 119.6(4) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C45 C44 C43 120.0(4) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.0(4) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 121.7(4) . . ? C45 C46 H46 119.1 . . ? C41 C46 H46 119.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.628 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.088 # Attachment '- compound15.CIF' data_compound15 _database_code_depnum_ccdc_archive 'CCDC 822602' #TrackingRef '- compound15.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H37 Cl2 N Si2' _chemical_formula_weight 610.75 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 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 12.5080(7) _cell_length_b 17.0460(10) _cell_length_c 15.5962(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.400(2) _cell_angle_gamma 90.00 _cell_volume 3297.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.295 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9167 _exptl_absorpt_correction_T_max 0.9433 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 43632 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5597 _reflns_number_gt 3900 _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. The atoms of the SiMe3 and SiCl2H fragments were found to be disordered over two sites. This disorder was successfully modelled. The hydride, H1a, was refined with its thermal displacement parameter tied to that of Si(2), and with the Si2-H1a distance constrained with the DFIX command of SHELX-L. The DFIX and DANG commands of SHELX-L were also used to constrain the geometries of the two disordered N(SiMe3)(SiCl2H)sets, giving rise, in total, to the 40 restraints used in the final refinement cycle. A PLATON checks yielded a Level A alert pertaining to an unusually short contact of only 1.77 between H20 (on aromatic carbon C20) and H36F (on partial-occupancy methyl carbon C36A). As C36A only has partial occupancy 0.149(3) and a high Uiso value of 0.27(7)we can have no confidence in the H-positions of C36A. The poor overall quality of the crystal structure arose from the aforementioned disorder and weak diffraction data above a theta value of 23 deg. Despite this, the gross molecular connectivity of the structure is unambiguous and fully consistent with its solution spectroscopic data. ; _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^)+(0.0870P)^2^+9.0081P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5597 _refine_ls_number_parameters 400 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2215 _refine_ls_wR_factor_gt 0.1998 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.083 _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 0.15311(16) 0.14663(11) 0.95440(10) 0.0618(6) Uani 0.851(3) 1 d P A 1 Cl1A Cl 0.2541(13) 0.3056(7) 0.7292(10) 0.105(5) Uiso 0.149(3) 1 d PD A 2 Cl2 Cl 0.38578(14) 0.07473(12) 0.93357(10) 0.0669(6) Uani 0.851(3) 1 d P A 1 Cl2A Cl 0.3756(12) 0.1952(10) 0.6207(10) 0.112(5) Uiso 0.149(3) 1 d PD A 2 Si1 Si 0.28910(13) 0.19211(9) 0.73660(11) 0.0378(4) Uani 0.851(3) 1 d PD A 1 Si1A Si 0.2755(17) 0.1199(13) 0.8755(6) 0.151(9) Uiso 0.149(3) 1 d PD A 2 Si2 Si 0.23097(13) 0.07624(10) 0.87522(9) 0.0375(4) Uani 0.851(3) 1 d PD A 1 Si2A Si 0.2477(16) 0.1893(7) 0.6931(9) 0.139(10) Uiso 0.149(3) 1 d PD A 2 HI2A H 0.1834 0.1874 0.6479 0.167 Uiso 0.149(3) 1 calc PR A 2 N1 N 0.2197(3) 0.1112(2) 0.7682(2) 0.0409(10) Uani 1 1 d D . . C1 C 0.1459(3) 0.0622(2) 0.7110(3) 0.0296(10) Uani 1 1 d . A . C2 C 0.0336(3) 0.0727(2) 0.7059(3) 0.0294(10) Uani 1 1 d . . . C3 C -0.0345(3) 0.0198(3) 0.6573(3) 0.0322(10) Uani 1 1 d . A . H3 H -0.1102 0.0266 0.6546 0.039 Uiso 1 1 calc R . . C4 C 0.0039(3) -0.0419(3) 0.6130(3) 0.0309(10) Uani 1 1 d . . . C5 C 0.1152(4) -0.0492(3) 0.6167(3) 0.0336(10) Uani 1 1 d . A . H5 H 0.1431 -0.0906 0.5854 0.040 Uiso 1 1 calc R . . C6 C 0.1872(3) 0.0013(3) 0.6639(3) 0.0315(10) Uani 1 1 d . . . C7 C -0.0148(4) 0.1423(3) 0.7492(3) 0.0326(10) Uani 1 1 d . A . H7 H 0.0421 0.1604 0.7960 0.039 Uiso 1 1 calc R . . C8 C -0.0707(4) -0.0983(3) 0.5610(3) 0.0401(12) Uani 1 1 d . A . H8A H -0.1358 -0.1054 0.5890 0.060 Uiso 1 1 calc R . . H8B H -0.0344 -0.1490 0.5576 0.060 Uiso 1 1 calc R . . H8C H -0.0905 -0.0774 0.5026 0.060 Uiso 1 1 calc R . . C9 C 0.3085(4) -0.0113(3) 0.6654(3) 0.0350(11) Uani 1 1 d . A . H9 H 0.3423 0.0418 0.6730 0.042 Uiso 1 1 calc R . . C10 C -0.0373(4) 0.2114(3) 0.6877(3) 0.0366(11) Uani 1 1 d . . . C11 C -0.0792(4) 0.2032(3) 0.6011(3) 0.0481(13) Uani 1 1 d . A . H11 H -0.0967 0.1526 0.5779 0.058 Uiso 1 1 calc R . . C12 C -0.0955(5) 0.2692(4) 0.5485(4) 0.0667(18) Uani 1 1 d . . . H12 H -0.1239 0.2636 0.4893 0.080 Uiso 1 1 calc R A . C13 C -0.0703(5) 0.3431(4) 0.5825(5) 0.070(2) Uani 1 1 d . A . H13 H -0.0795 0.3879 0.5461 0.084 Uiso 1 1 calc R . . C14 C -0.0327(5) 0.3516(3) 0.6675(5) 0.0659(18) Uani 1 1 d . . . H14 H -0.0176 0.4024 0.6909 0.079 Uiso 1 1 calc R A . C15 C -0.0163(4) 0.2869(3) 0.7197(4) 0.0486(13) Uani 1 1 d . A . H15 H 0.0100 0.2937 0.7792 0.058 Uiso 1 1 calc R . . C16 C -0.1129(4) 0.1204(3) 0.7943(3) 0.0336(10) Uani 1 1 d . . . C17 C -0.2022(4) 0.1680(3) 0.7918(3) 0.0438(12) Uani 1 1 d . A . H17 H -0.2059 0.2148 0.7585 0.053 Uiso 1 1 calc R . . C18 C -0.2869(4) 0.1486(4) 0.8375(4) 0.0569(15) Uani 1 1 d . . . H18 H -0.3470 0.1829 0.8358 0.068 Uiso 1 1 calc R A . C19 C -0.2850(5) 0.0813(4) 0.8845(4) 0.0613(16) Uani 1 1 d . A . H19 H -0.3441 0.0674 0.9141 0.074 Uiso 1 1 calc R . . C20 C -0.1963(5) 0.0339(4) 0.8884(4) 0.0654(17) Uani 1 1 d . . . H20 H -0.1933 -0.0128 0.9218 0.078 Uiso 1 1 calc R A . C21 C -0.1110(5) 0.0530(3) 0.8442(3) 0.0541(14) Uani 1 1 d . A . H21 H -0.0499 0.0194 0.8481 0.065 Uiso 1 1 calc R . . C22 C 0.3596(4) -0.0606(3) 0.7412(3) 0.0367(11) Uani 1 1 d . . . C23 C 0.3011(4) -0.1139(3) 0.7835(4) 0.0492(13) Uani 1 1 d . A . H23 H 0.2259 -0.1194 0.7663 0.059 Uiso 1 1 calc R . . C24 C 0.3511(5) -0.1588(3) 0.8504(4) 0.0631(16) Uani 1 1 d . . . H24 H 0.3102 -0.1957 0.8781 0.076 Uiso 1 1 calc R A . C25 C 0.4597(5) -0.1506(3) 0.8775(4) 0.0586(15) Uani 1 1 d . A . H25 H 0.4935 -0.1811 0.9243 0.070 Uiso 1 1 calc R . . C26 C 0.5189(5) -0.0977(3) 0.8358(4) 0.0560(15) Uani 1 1 d . . . H26 H 0.5941 -0.0920 0.8535 0.067 Uiso 1 1 calc R A . C27 C 0.4693(4) -0.0536(3) 0.7689(3) 0.0459(13) Uani 1 1 d . A . H27 H 0.5108 -0.0173 0.7407 0.055 Uiso 1 1 calc R . . C28 C 0.3351(4) -0.0421(4) 0.5787(3) 0.0500(14) Uani 1 1 d . . . C29 C 0.3391(5) 0.0098(5) 0.5117(4) 0.073(2) Uani 1 1 d . A . H29 H 0.3291 0.0641 0.5218 0.087 Uiso 1 1 calc R . . C30 C 0.3572(6) -0.0145(6) 0.4296(5) 0.098(2) Uani 1 1 d U . . H30 H 0.3606 0.0224 0.3844 0.118 Uiso 1 1 calc R A . C31 C 0.3693(6) -0.0881(6) 0.4169(6) 0.097(2) Uani 1 1 d U A . H31 H 0.3776 -0.1043 0.3598 0.117 Uiso 1 1 calc R . . C32 C 0.3710(7) -0.1453(6) 0.4788(7) 0.106(3) Uani 1 1 d U . . H32 H 0.3839 -0.1986 0.4653 0.127 Uiso 1 1 calc R A . C33 C 0.3527(2) -0.12247(18) 0.5661(2) 0.079(2) Uani 1 1 d . A . H33 H 0.3528 -0.1596 0.6115 0.095 Uiso 1 1 calc R . . C35 C 0.2269(2) 0.21628(18) 0.6273(2) 0.0483(16) Uani 0.851(3) 1 d PRD A 1 H35A H 0.2336 0.1715 0.5890 0.072 Uiso 0.851(3) 1 calc PR A 1 H35B H 0.2632 0.2619 0.6061 0.072 Uiso 0.851(3) 1 calc PR A 1 H35C H 0.1504 0.2284 0.6281 0.072 Uiso 0.851(3) 1 calc PR A 1 C34 C 0.4358(2) 0.17298(18) 0.7370(2) 0.0605(19) Uani 0.851(3) 1 d PRD A 1 H34A H 0.4608 0.1365 0.7838 0.091 Uiso 0.851(3) 1 calc PR A 1 H34B H 0.4757 0.2224 0.7458 0.091 Uiso 0.851(3) 1 calc PR A 1 H34C H 0.4480 0.1500 0.6815 0.091 Uiso 0.851(3) 1 calc PR A 1 C36 C 0.2799(2) 0.27528(18) 0.8133(2) 0.0608(19) Uani 0.851(3) 1 d PRD A 1 H36A H 0.2053 0.2941 0.8082 0.091 Uiso 0.851(3) 1 calc PR A 1 H36B H 0.3271 0.3180 0.7993 0.091 Uiso 0.851(3) 1 calc PR A 1 H36C H 0.3024 0.2574 0.8725 0.091 Uiso 0.851(3) 1 calc PR A 1 C34A C 0.4232(18) 0.141(3) 0.887(2) 0.14(3) Uiso 0.149(3) 1 d PD A 2 H34D H 0.4600 0.0992 0.8588 0.206 Uiso 0.149(3) 1 calc PR A 2 H34E H 0.4519 0.1433 0.9483 0.206 Uiso 0.149(3) 1 calc PR A 2 H34F H 0.4353 0.1913 0.8593 0.206 Uiso 0.149(3) 1 calc PR A 2 C35A C 0.212(4) 0.201(3) 0.9323(19) 0.16(3) Uiso 0.149(3) 1 d PD A 2 H35D H 0.1337 0.1980 0.9185 0.247 Uiso 0.149(3) 1 calc PR A 2 H35E H 0.2379 0.2515 0.9135 0.247 Uiso 0.149(3) 1 calc PR A 2 H35F H 0.2321 0.1952 0.9949 0.247 Uiso 0.149(3) 1 calc PR A 2 C36A C 0.259(5) 0.028(2) 0.9384(17) 0.27(7) Uiso 0.149(3) 1 d PD A 2 H36D H 0.2785 0.0387 1.0002 0.409 Uiso 0.149(3) 1 calc PR A 2 H36E H 0.3061 -0.0129 0.9201 0.409 Uiso 0.149(3) 1 calc PR A 2 H36F H 0.1838 0.0107 0.9277 0.409 Uiso 0.149(3) 1 calc PR A 2 H1A H 0.193(16) -0.001(4) 0.882(14) 0.327 Uiso 0.851(3) 1 d PD A 1 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 0.0823(13) 0.0717(12) 0.0331(8) -0.0099(8) 0.0139(8) 0.0213(9) Cl2 0.0552(10) 0.0989(15) 0.0420(9) -0.0053(9) -0.0120(7) 0.0089(9) Si1 0.0360(9) 0.0343(9) 0.0430(10) -0.0024(7) 0.0047(8) -0.0066(6) Si2 0.0453(9) 0.0404(10) 0.0261(8) -0.0068(7) 0.0022(6) 0.0014(8) N1 0.037(2) 0.042(2) 0.044(2) -0.0165(19) 0.0055(18) -0.0020(18) C1 0.034(2) 0.025(2) 0.029(2) 0.0002(18) 0.0032(19) -0.0016(18) C2 0.035(2) 0.027(2) 0.027(2) 0.0023(19) 0.0068(18) 0.0034(18) C3 0.029(2) 0.037(3) 0.031(2) 0.001(2) 0.0052(19) -0.0007(19) C4 0.038(3) 0.031(2) 0.024(2) 0.0005(19) 0.0054(19) -0.0009(19) C5 0.037(3) 0.035(3) 0.030(2) -0.005(2) 0.010(2) 0.001(2) C6 0.035(2) 0.029(2) 0.031(2) 0.0002(19) 0.0078(19) -0.0008(19) C7 0.033(2) 0.033(3) 0.032(2) -0.002(2) 0.0048(19) -0.0002(19) C8 0.040(3) 0.044(3) 0.036(3) -0.006(2) 0.004(2) -0.006(2) C9 0.034(2) 0.033(3) 0.039(3) -0.009(2) 0.007(2) 0.0000(19) C10 0.033(2) 0.032(3) 0.047(3) 0.005(2) 0.015(2) 0.006(2) C11 0.054(3) 0.046(3) 0.046(3) 0.006(2) 0.013(3) 0.016(2) C12 0.082(4) 0.075(5) 0.049(3) 0.024(3) 0.028(3) 0.034(4) C13 0.092(5) 0.043(4) 0.085(5) 0.028(3) 0.047(4) 0.022(3) C14 0.077(4) 0.036(3) 0.090(5) 0.015(3) 0.035(4) 0.008(3) C15 0.049(3) 0.033(3) 0.068(4) 0.001(3) 0.022(3) 0.002(2) C16 0.042(3) 0.031(3) 0.030(2) -0.004(2) 0.011(2) -0.002(2) C17 0.035(3) 0.047(3) 0.051(3) 0.003(2) 0.008(2) 0.000(2) C18 0.042(3) 0.071(4) 0.061(4) -0.003(3) 0.018(3) 0.003(3) C19 0.061(4) 0.071(4) 0.057(4) -0.007(3) 0.029(3) -0.016(3) C20 0.095(5) 0.051(4) 0.058(4) 0.013(3) 0.041(3) 0.000(3) C21 0.069(4) 0.048(3) 0.050(3) 0.007(3) 0.025(3) 0.012(3) C22 0.035(3) 0.032(3) 0.043(3) -0.008(2) 0.006(2) 0.0001(19) C23 0.045(3) 0.036(3) 0.064(3) 0.005(3) -0.001(3) -0.002(2) C24 0.057(4) 0.046(3) 0.083(4) 0.018(3) -0.003(3) -0.004(3) C25 0.062(4) 0.048(3) 0.062(4) 0.010(3) -0.009(3) 0.004(3) C26 0.043(3) 0.057(4) 0.065(4) -0.005(3) -0.005(3) 0.001(3) C27 0.039(3) 0.043(3) 0.055(3) -0.003(3) 0.004(2) 0.003(2) C28 0.027(3) 0.078(4) 0.046(3) -0.017(3) 0.008(2) -0.001(2) C29 0.050(4) 0.132(6) 0.039(3) -0.002(4) 0.020(3) 0.011(4) C30 0.075(4) 0.151(6) 0.073(4) -0.006(4) 0.027(3) 0.011(4) C31 0.062(4) 0.145(6) 0.085(5) -0.035(5) 0.009(4) -0.001(4) C32 0.081(4) 0.108(5) 0.130(6) -0.062(5) 0.018(4) 0.004(4) C33 0.072(4) 0.085(5) 0.085(5) -0.054(4) 0.025(4) 0.003(4) C35 0.031(3) 0.031(3) 0.086(5) -0.004(3) 0.020(3) -0.010(2) C34 0.038(4) 0.056(4) 0.087(5) 0.008(4) 0.008(3) -0.006(3) C36 0.072(5) 0.039(4) 0.072(5) -0.017(3) 0.013(4) -0.013(3) _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 Si2 2.055(2) . ? Cl1A Si2A 2.059(5) . ? Cl2 Si2 2.031(2) . ? Cl2A Si2A 2.075(8) . ? Si1 N1 1.735(4) . ? Si1 C35 1.828(4) . ? Si1 C34 1.863(3) . ? Si1 C36 1.868(3) . ? Si1A N1 1.734(7) . ? Si1A C34A 1.868(8) . ? Si1A C35A 1.869(8) . ? Si1A C36A 1.871(8) . ? Si2 N1 1.761(4) . ? Si2 H1A 1.413(9) . ? Si2A N1 1.837(7) . ? Si2A HI2A 1.0000 . ? N1 C1 1.461(5) . ? C1 C6 1.408(6) . ? C1 C2 1.408(6) . ? C2 C3 1.395(6) . ? C2 C7 1.530(6) . ? C3 C4 1.379(6) . ? C3 H3 0.9500 . ? C4 C5 1.392(6) . ? C4 C8 1.502(6) . ? C5 C6 1.387(6) . ? C5 H5 0.9500 . ? C6 C9 1.529(6) . ? C7 C10 1.522(6) . ? C7 C16 1.536(6) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C22 1.524(7) . ? C9 C28 1.527(7) . ? C9 H9 1.0000 . ? C10 C11 1.392(7) . ? C10 C15 1.393(7) . ? C11 C12 1.391(8) . ? C11 H11 0.9500 . ? C12 C13 1.388(9) . ? C12 H12 0.9500 . ? C13 C14 1.356(10) . ? C13 H13 0.9500 . ? C14 C15 1.371(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.377(7) . ? C16 C21 1.385(7) . ? C17 C18 1.391(7) . ? C17 H17 0.9500 . ? C18 C19 1.362(8) . ? C18 H18 0.9500 . ? C19 C20 1.367(8) . ? C19 H19 0.9500 . ? C20 C21 1.381(8) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.384(7) . ? C22 C27 1.389(7) . ? C23 C24 1.377(8) . ? C23 H23 0.9500 . ? C24 C25 1.376(8) . ? C24 H24 0.9500 . ? C25 C26 1.382(8) . ? C25 H25 0.9500 . ? C26 C27 1.369(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.375(9) . ? C28 C33 1.406(6) . ? C29 C30 1.391(9) . ? C29 H29 0.9500 . ? C30 C31 1.283(12) . ? C30 H30 0.9500 . ? C31 C32 1.371(12) . ? C31 H31 0.9500 . ? C32 C33 1.462(9) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C34A H34D 0.9800 . ? C34A H34E 0.9800 . ? C34A H34F 0.9800 . ? C35A H35D 0.9800 . ? C35A H35E 0.9800 . ? C35A H35F 0.9800 . ? C36A H36D 0.9800 . ? C36A H36E 0.9800 . ? C36A H36F 0.9800 . ? C36A H1A 1.23(18) . ? 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 C35 106.01(17) . . ? N1 Si1 C34 112.85(18) . . ? C35 Si1 C34 110.07(17) . . ? N1 Si1 C36 110.33(17) . . ? C35 Si1 C36 111.85(18) . . ? C34 Si1 C36 105.83(16) . . ? N1 Si1A C34A 112.2(6) . . ? N1 Si1A C35A 112.3(6) . . ? C34A Si1A C35A 106.7(5) . . ? N1 Si1A C36A 112.1(6) . . ? C34A Si1A C36A 106.6(5) . . ? C35A Si1A C36A 106.6(5) . . ? N1 Si2 Cl2 112.60(15) . . ? N1 Si2 Cl1 112.71(15) . . ? Cl2 Si2 Cl1 103.68(10) . . ? N1 Si2 H1A 114(9) . . ? Cl2 Si2 H1A 105(9) . . ? Cl1 Si2 H1A 108(8) . . ? N1 Si2A Cl1A 121.8(8) . . ? N1 Si2A Cl2A 127.3(10) . . ? Cl1A Si2A Cl2A 95.5(8) . . ? N1 Si2A HI2A 102.9 . . ? Cl1A Si2A HI2A 102.9 . . ? Cl2A Si2A HI2A 102.9 . . ? C1 N1 Si1A 141.5(7) . . ? C1 N1 Si1 125.5(3) . . ? Si1A N1 Si1 93.0(7) . . ? C1 N1 Si2 110.7(3) . . ? Si1A N1 Si2 30.8(7) . . ? Si1 N1 Si2 123.8(2) . . ? C1 N1 Si2A 100.5(6) . . ? Si1A N1 Si2A 117.8(6) . . ? Si1 N1 Si2A 25.7(6) . . ? Si2 N1 Si2A 148.3(6) . . ? C6 C1 C2 119.7(4) . . ? C6 C1 N1 119.6(4) . . ? C2 C1 N1 120.6(4) . . ? C3 C2 C1 118.9(4) . . ? C3 C2 C7 119.5(4) . . ? C1 C2 C7 121.5(4) . . ? C4 C3 C2 122.5(4) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 117.3(4) . . ? C3 C4 C8 121.8(4) . . ? C5 C4 C8 120.9(4) . . ? C6 C5 C4 123.0(4) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C5 C6 C1 118.5(4) . . ? C5 C6 C9 119.7(4) . . ? C1 C6 C9 121.7(4) . . ? C10 C7 C2 111.9(4) . . ? C10 C7 C16 112.5(4) . . ? C2 C7 C16 113.4(4) . . ? C10 C7 H7 106.1 . . ? C2 C7 H7 106.1 . . ? C16 C7 H7 106.1 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C22 C9 C28 112.4(4) . . ? C22 C9 C6 113.9(4) . . ? C28 C9 C6 111.3(4) . . ? C22 C9 H9 106.2 . . ? C28 C9 H9 106.2 . . ? C6 C9 H9 106.2 . . ? C11 C10 C15 118.0(5) . . ? C11 C10 C7 123.4(4) . . ? C15 C10 C7 118.5(4) . . ? C12 C11 C10 120.0(5) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 120.0(6) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.2(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.1(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C10 121.5(6) . . ? C14 C15 H15 119.2 . . ? C10 C15 H15 119.2 . . ? C17 C16 C21 117.4(4) . . ? C17 C16 C7 122.4(4) . . ? C21 C16 C7 120.1(4) . . ? C16 C17 C18 120.9(5) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 121.0(5) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 118.7(5) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? C19 C20 C21 120.9(5) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C16 121.2(5) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? C23 C22 C27 118.1(5) . . ? C23 C22 C9 122.5(4) . . ? C27 C22 C9 119.5(4) . . ? C24 C23 C22 120.6(5) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 120.7(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.3(5) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 119.9(5) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C22 121.4(5) . . ? C26 C27 H27 119.3 . . ? C22 C27 H27 119.3 . . ? C29 C28 C33 119.9(5) . . ? C29 C28 C9 119.0(5) . . ? C33 C28 C9 121.0(5) . . ? C28 C29 C30 122.3(8) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C31 C30 C29 118.0(9) . . ? C31 C30 H30 121.0 . . ? C29 C30 H30 121.0 . . ? C30 C31 C32 125.3(9) . . ? C30 C31 H31 117.3 . . ? C32 C31 H31 117.3 . . ? C31 C32 C33 118.5(7) . . ? C31 C32 H32 120.8 . . ? C33 C32 H32 120.8 . . ? C28 C33 C32 115.9(5) . . ? C28 C33 H33 122.1 . . ? C32 C33 H33 122.1 . . ? Si1A C34A H34D 109.5 . . ? Si1A C34A H34E 109.5 . . ? H34D C34A H34E 109.5 . . ? Si1A C34A H34F 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? Si1A C35A H35D 109.5 . . ? Si1A C35A H35E 109.5 . . ? H35D C35A H35E 109.5 . . ? Si1A C35A H35F 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? Si1A C36A H36D 109.5 . . ? Si1A C36A H36E 109.5 . . ? H36D C36A H36E 109.5 . . ? Si1A C36A H36F 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 109.5 . . ? Si1A C36A H1A 94(5) . . ? H36D C36A H1A 146.4 . . ? H36E C36A H1A 82.9 . . ? H36F C36A H1A 38.1 . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.396 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.071 # Attachment '- compound3.CIF' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 822603' #TrackingRef '- compound3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H43 N Si' _chemical_formula_weight 697.95 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 20.5915(12) _cell_length_b 10.8266(5) _cell_length_c 17.5359(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.691(5) _cell_angle_gamma 90.00 _cell_volume 3890.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.931 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 17699 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7218 _reflns_number_gt 6033 _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^)+(0.0375P)^2^+2.0232P] 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 7218 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.215800(19) 0.06238(4) -0.00022(2) 0.01684(11) Uani 1 1 d . . . N1 N 0.24702(6) -0.08564(11) 0.00790(7) 0.0173(3) Uani 1 1 d . . . H1 H 0.2578 -0.1206 -0.0344 0.021 Uiso 1 1 calc R . . C1 C 0.25711(7) -0.15705(13) 0.07710(8) 0.0165(3) Uani 1 1 d . . . C2 C 0.20821(7) -0.23737(13) 0.09772(8) 0.0172(3) Uani 1 1 d . . . C3 C 0.21782(7) -0.30226(14) 0.16618(8) 0.0204(3) Uani 1 1 d . . . H3 H 0.1844 -0.3557 0.1802 0.025 Uiso 1 1 calc R . . C4 C 0.27524(7) -0.29106(14) 0.21488(8) 0.0204(3) Uani 1 1 d . . . C5 C 0.32421(7) -0.21680(14) 0.19150(8) 0.0199(3) Uani 1 1 d . . . H5 H 0.3642 -0.2102 0.2233 0.024 Uiso 1 1 calc R . . C6 C 0.31670(7) -0.15151(13) 0.12300(8) 0.0173(3) Uani 1 1 d . . . C7 C 0.28469(8) -0.35968(16) 0.29005(9) 0.0292(4) Uani 1 1 d . . . H7A H 0.2666 -0.3109 0.3300 0.044 Uiso 1 1 calc R . . H7B H 0.3314 -0.3732 0.3042 0.044 Uiso 1 1 calc R . . H7C H 0.2623 -0.4395 0.2848 0.044 Uiso 1 1 calc R . . C8 C 0.14923(7) -0.26121(14) 0.03993(8) 0.0189(3) Uani 1 1 d . . . H8 H 0.1337 -0.1785 0.0204 0.023 Uiso 1 1 calc R . . C9 C 0.17033(7) -0.33174(14) -0.02898(9) 0.0204(3) Uani 1 1 d . . . C10 C 0.13850(8) -0.31236(15) -0.10164(9) 0.0259(4) Uani 1 1 d . . . H10 H 0.1018 -0.2589 -0.1075 0.031 Uiso 1 1 calc R . . C11 C 0.15915(9) -0.36921(17) -0.16545(10) 0.0355(4) Uani 1 1 d . . . H11 H 0.1374 -0.3530 -0.2148 0.043 Uiso 1 1 calc R . . C12 C 0.21111(10) -0.44923(19) -0.15765(11) 0.0444(5) Uani 1 1 d . . . H12 H 0.2257 -0.4879 -0.2015 0.053 Uiso 1 1 calc R . . C13 C 0.24191(10) -0.4730(2) -0.08601(12) 0.0483(6) Uani 1 1 d . . . H13 H 0.2771 -0.5302 -0.0801 0.058 Uiso 1 1 calc R . . C14 C 0.22186(9) -0.41382(17) -0.02243(11) 0.0341(4) Uani 1 1 d . . . H14 H 0.2440 -0.4300 0.0267 0.041 Uiso 1 1 calc R . . C15 C 0.09188(7) -0.32078(15) 0.07440(8) 0.0224(3) Uani 1 1 d . . . C16 C 0.05137(8) -0.24717(17) 0.11380(10) 0.0303(4) Uani 1 1 d . . . H16 H 0.0609 -0.1618 0.1204 0.036 Uiso 1 1 calc R . . C17 C -0.00304(9) -0.2968(2) 0.14372(10) 0.0398(5) Uani 1 1 d . . . H17 H -0.0304 -0.2455 0.1707 0.048 Uiso 1 1 calc R . . C18 C -0.01705(9) -0.4206(2) 0.13410(10) 0.0424(5) Uani 1 1 d . . . H18 H -0.0547 -0.4545 0.1534 0.051 Uiso 1 1 calc R . . C19 C 0.02344(9) -0.4948(2) 0.09671(10) 0.0395(5) Uani 1 1 d . . . H19 H 0.0143 -0.5805 0.0913 0.047 Uiso 1 1 calc R . . C20 C 0.07773(8) -0.44548(16) 0.06669(9) 0.0289(4) Uani 1 1 d . . . H20 H 0.1054 -0.4977 0.0407 0.035 Uiso 1 1 calc R . . C21 C 0.37452(7) -0.08834(14) 0.09203(8) 0.0189(3) Uani 1 1 d . . . H21 H 0.3570 -0.0118 0.0655 0.023 Uiso 1 1 calc R . . C22 C 0.40111(7) -0.16858(14) 0.03044(9) 0.0199(3) Uani 1 1 d . . . C23 C 0.39295(8) -0.29540(15) 0.02712(10) 0.0297(4) Uani 1 1 d . . . H23 H 0.3716 -0.3361 0.0656 0.036 Uiso 1 1 calc R . . C24 C 0.41550(9) -0.36401(16) -0.03165(11) 0.0351(4) Uani 1 1 d . . . H24 H 0.4097 -0.4511 -0.0328 0.042 Uiso 1 1 calc R . . C25 C 0.44628(8) -0.30688(17) -0.08838(10) 0.0320(4) Uani 1 1 d . . . H25 H 0.4608 -0.3537 -0.1293 0.038 Uiso 1 1 calc R . . C26 C 0.45571(8) -0.18099(17) -0.08500(10) 0.0316(4) Uani 1 1 d . . . H26 H 0.4778 -0.1410 -0.1232 0.038 Uiso 1 1 calc R . . C27 C 0.43335(7) -0.11255(15) -0.02654(9) 0.0253(4) Uani 1 1 d . . . H27 H 0.4401 -0.0257 -0.0252 0.030 Uiso 1 1 calc R . . C28 C 0.42565(7) -0.04604(14) 0.15528(9) 0.0225(3) Uani 1 1 d . . . C29 C 0.48612(8) -0.10026(16) 0.16977(10) 0.0307(4) Uani 1 1 d . . . H29 H 0.4975 -0.1681 0.1395 0.037 Uiso 1 1 calc R . . C30 C 0.53072(9) -0.05633(18) 0.22861(12) 0.0411(5) Uani 1 1 d . . . H30 H 0.5723 -0.0944 0.2381 0.049 Uiso 1 1 calc R . . C31 C 0.51485(10) 0.04145(18) 0.27290(11) 0.0419(5) Uani 1 1 d . . . H31 H 0.5454 0.0716 0.3126 0.050 Uiso 1 1 calc R . . C32 C 0.45427(10) 0.09564(18) 0.25938(10) 0.0390(5) Uani 1 1 d . . . H32 H 0.4428 0.1627 0.2903 0.047 Uiso 1 1 calc R . . C33 C 0.41021(9) 0.05252(16) 0.20094(10) 0.0308(4) Uani 1 1 d . . . H33 H 0.3687 0.0909 0.1918 0.037 Uiso 1 1 calc R . . C34 C 0.27777(8) 0.18330(14) 0.03195(9) 0.0211(3) Uani 1 1 d . . . C35 C 0.33671(8) 0.18970(15) -0.00155(9) 0.0255(4) Uani 1 1 d . . . H35 H 0.3446 0.1321 -0.0404 0.031 Uiso 1 1 calc R . . C36 C 0.38353(9) 0.27726(16) 0.02028(10) 0.0340(4) Uani 1 1 d . . . H36 H 0.4231 0.2796 -0.0033 0.041 Uiso 1 1 calc R . . C37 C 0.37251(10) 0.36159(17) 0.07672(11) 0.0393(5) Uani 1 1 d . . . H37 H 0.4049 0.4212 0.0926 0.047 Uiso 1 1 calc R . . C38 C 0.31506(10) 0.35963(16) 0.10993(11) 0.0381(5) Uani 1 1 d . . . H38 H 0.3075 0.4185 0.1483 0.046 Uiso 1 1 calc R . . C39 C 0.26758(9) 0.27134(15) 0.08753(9) 0.0289(4) Uani 1 1 d . . . H39 H 0.2277 0.2712 0.1105 0.035 Uiso 1 1 calc R . . C40 C 0.18945(7) 0.08810(14) -0.10413(8) 0.0192(3) Uani 1 1 d . . . C41 C 0.21585(9) 0.18079(16) -0.14637(10) 0.0318(4) Uani 1 1 d . . . H41 H 0.2484 0.2336 -0.1220 0.038 Uiso 1 1 calc R . . C42 C 0.19567(10) 0.19754(18) -0.22320(10) 0.0404(5) Uani 1 1 d . . . H42 H 0.2148 0.2610 -0.2510 0.048 Uiso 1 1 calc R . . C43 C 0.14818(9) 0.12320(16) -0.25979(9) 0.0317(4) Uani 1 1 d . . . H43 H 0.1345 0.1353 -0.3126 0.038 Uiso 1 1 calc R . . C44 C 0.12073(8) 0.03138(16) -0.21948(9) 0.0262(4) Uani 1 1 d . . . H44 H 0.0879 -0.0204 -0.2442 0.031 Uiso 1 1 calc R . . C45 C 0.14131(8) 0.01473(15) -0.14246(9) 0.0241(3) Uani 1 1 d . . . H45 H 0.1219 -0.0488 -0.1150 0.029 Uiso 1 1 calc R . . C46 C 0.14464(7) 0.08145(14) 0.05747(9) 0.0212(3) Uani 1 1 d . . . C47 C 0.08455(8) 0.12317(19) 0.02429(10) 0.0366(4) Uani 1 1 d . . . H47 H 0.0791 0.1399 -0.0291 0.044 Uiso 1 1 calc R . . C48 C 0.03246(9) 0.1409(2) 0.06737(11) 0.0450(5) Uani 1 1 d . . . H48 H -0.0082 0.1686 0.0431 0.054 Uiso 1 1 calc R . . C49 C 0.03920(9) 0.11890(18) 0.14468(10) 0.0342(4) Uani 1 1 d . . . H49 H 0.0035 0.1320 0.1742 0.041 Uiso 1 1 calc R . . C50 C 0.09812(9) 0.07761(16) 0.17909(10) 0.0307(4) Uani 1 1 d . . . H50 H 0.1033 0.0624 0.2327 0.037 Uiso 1 1 calc R . . C51 C 0.14982(8) 0.05818(15) 0.13593(9) 0.0263(4) Uani 1 1 d . . . H51 H 0.1899 0.0281 0.1604 0.032 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 0.0196(2) 0.0171(2) 0.0137(2) 0.00085(16) 0.00102(15) 0.00069(16) N1 0.0216(6) 0.0186(6) 0.0118(6) 0.0005(5) 0.0029(5) -0.0001(5) C1 0.0209(7) 0.0145(7) 0.0142(7) 0.0003(6) 0.0021(6) 0.0023(6) C2 0.0181(7) 0.0180(7) 0.0158(7) -0.0014(6) 0.0024(6) 0.0004(6) C3 0.0204(8) 0.0220(8) 0.0193(8) 0.0020(6) 0.0039(6) -0.0032(6) C4 0.0228(8) 0.0218(8) 0.0166(8) 0.0033(6) 0.0017(6) 0.0005(6) C5 0.0187(7) 0.0215(8) 0.0186(8) 0.0011(6) -0.0023(6) -0.0003(6) C6 0.0183(7) 0.0150(7) 0.0188(7) -0.0018(6) 0.0023(6) 0.0002(6) C7 0.0277(9) 0.0363(10) 0.0227(8) 0.0107(7) -0.0011(7) -0.0051(7) C8 0.0192(8) 0.0198(8) 0.0172(7) 0.0027(6) -0.0005(6) -0.0008(6) C9 0.0196(8) 0.0198(8) 0.0216(8) -0.0014(6) 0.0010(6) -0.0071(6) C10 0.0298(9) 0.0235(8) 0.0241(8) 0.0001(7) 0.0007(7) -0.0046(7) C11 0.0490(11) 0.0350(10) 0.0220(9) -0.0046(8) 0.0013(8) -0.0128(9) C12 0.0449(11) 0.0506(12) 0.0388(11) -0.0269(10) 0.0108(9) -0.0081(10) C13 0.0372(11) 0.0503(13) 0.0554(13) -0.0293(11) -0.0050(10) 0.0106(10) C14 0.0322(9) 0.0332(10) 0.0347(10) -0.0124(8) -0.0078(8) 0.0061(8) C15 0.0191(8) 0.0307(9) 0.0162(8) 0.0052(7) -0.0037(6) -0.0040(7) C16 0.0265(9) 0.0378(10) 0.0270(9) 0.0066(8) 0.0040(7) 0.0012(8) C17 0.0268(9) 0.0646(14) 0.0289(10) 0.0099(9) 0.0077(7) 0.0037(9) C18 0.0280(10) 0.0732(15) 0.0255(10) 0.0125(10) 0.0004(8) -0.0207(10) C19 0.0439(11) 0.0500(12) 0.0231(9) 0.0070(9) -0.0039(8) -0.0270(10) C20 0.0325(9) 0.0351(10) 0.0183(8) 0.0022(7) -0.0015(7) -0.0104(8) C21 0.0190(7) 0.0166(7) 0.0206(8) 0.0035(6) -0.0003(6) -0.0010(6) C22 0.0145(7) 0.0225(8) 0.0222(8) 0.0024(6) -0.0008(6) -0.0018(6) C23 0.0334(9) 0.0242(9) 0.0333(9) 0.0016(7) 0.0126(8) -0.0038(7) C24 0.0390(10) 0.0230(9) 0.0457(11) -0.0045(8) 0.0155(9) -0.0039(8) C25 0.0278(9) 0.0363(10) 0.0332(10) -0.0065(8) 0.0096(7) 0.0019(8) C26 0.0279(9) 0.0371(10) 0.0318(10) 0.0051(8) 0.0125(7) -0.0012(8) C27 0.0219(8) 0.0232(8) 0.0315(9) 0.0036(7) 0.0053(7) -0.0034(7) C28 0.0238(8) 0.0200(8) 0.0231(8) 0.0071(7) -0.0010(6) -0.0075(6) C29 0.0294(9) 0.0241(9) 0.0365(10) 0.0055(8) -0.0064(7) -0.0038(7) C30 0.0327(10) 0.0363(11) 0.0500(12) 0.0143(9) -0.0179(9) -0.0070(8) C31 0.0539(12) 0.0333(10) 0.0339(10) 0.0088(9) -0.0183(9) -0.0225(9) C32 0.0528(12) 0.0325(10) 0.0302(10) -0.0021(8) -0.0031(9) -0.0154(9) C33 0.0326(9) 0.0281(9) 0.0314(9) -0.0008(8) 0.0011(7) -0.0076(7) C34 0.0256(8) 0.0164(8) 0.0203(8) 0.0034(6) -0.0028(6) 0.0014(6) C35 0.0277(9) 0.0211(8) 0.0269(9) 0.0046(7) -0.0011(7) -0.0023(7) C36 0.0317(10) 0.0302(10) 0.0385(10) 0.0103(8) -0.0043(8) -0.0061(8) C37 0.0442(11) 0.0275(10) 0.0422(11) 0.0063(8) -0.0155(9) -0.0138(8) C38 0.0561(12) 0.0229(9) 0.0321(10) -0.0048(8) -0.0109(9) -0.0021(9) C39 0.0381(10) 0.0236(9) 0.0239(9) -0.0001(7) -0.0026(7) 0.0010(7) C40 0.0238(8) 0.0178(7) 0.0162(7) 0.0002(6) 0.0025(6) 0.0038(6) C41 0.0442(11) 0.0258(9) 0.0237(9) 0.0043(7) -0.0045(8) -0.0109(8) C42 0.0606(13) 0.0364(11) 0.0231(9) 0.0114(8) -0.0011(9) -0.0162(10) C43 0.0436(10) 0.0345(10) 0.0158(8) 0.0039(7) -0.0038(7) 0.0015(8) C44 0.0264(8) 0.0297(9) 0.0217(8) -0.0020(7) -0.0018(7) -0.0012(7) C45 0.0273(8) 0.0240(8) 0.0210(8) 0.0035(7) 0.0018(7) -0.0021(7) C46 0.0226(8) 0.0215(8) 0.0194(8) -0.0020(6) 0.0018(6) 0.0021(6) C47 0.0305(9) 0.0608(13) 0.0182(8) -0.0011(8) 0.0005(7) 0.0153(9) C48 0.0259(9) 0.0782(15) 0.0304(10) -0.0078(10) -0.0001(8) 0.0194(10) C49 0.0280(9) 0.0465(11) 0.0295(10) -0.0084(8) 0.0104(7) 0.0016(8) C50 0.0393(10) 0.0338(10) 0.0205(8) 0.0013(7) 0.0101(7) 0.0058(8) C51 0.0277(9) 0.0305(9) 0.0207(8) 0.0006(7) 0.0027(7) 0.0085(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 1.7273(13) . ? Si1 C40 1.8698(15) . ? Si1 C46 1.8728(16) . ? Si1 C34 1.8756(16) . ? N1 C1 1.4364(18) . ? N1 H1 0.8800 . ? C1 C6 1.400(2) . ? C1 C2 1.405(2) . ? C2 C3 1.388(2) . ? C2 C8 1.525(2) . ? C3 C4 1.393(2) . ? C3 H3 0.9500 . ? C4 C5 1.383(2) . ? C4 C7 1.509(2) . ? C5 C6 1.389(2) . ? C5 H5 0.9500 . ? C6 C21 1.519(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C15 1.522(2) . ? C8 C9 1.528(2) . ? C8 H8 1.0000 . ? C9 C14 1.380(2) . ? C9 C10 1.390(2) . ? C10 C11 1.381(2) . ? C10 H10 0.9500 . ? C11 C12 1.373(3) . ? C11 H11 0.9500 . ? C12 C13 1.374(3) . ? C12 H12 0.9500 . ? C13 C14 1.384(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.385(2) . ? C15 C16 1.387(2) . ? C16 C17 1.391(2) . ? C16 H16 0.9500 . ? C17 C18 1.378(3) . ? C17 H17 0.9500 . ? C18 C19 1.371(3) . ? C18 H18 0.9500 . ? C19 C20 1.389(2) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C28 1.522(2) . ? C21 C22 1.529(2) . ? C21 H21 1.0000 . ? C22 C23 1.384(2) . ? C22 C27 1.392(2) . ? C23 C24 1.387(2) . ? C23 H23 0.9500 . ? C24 C25 1.378(2) . ? C24 H24 0.9500 . ? C25 C26 1.377(3) . ? C25 H25 0.9500 . ? C26 C27 1.380(2) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.377(2) . ? C28 C33 1.390(2) . ? C29 C30 1.395(2) . ? C29 H29 0.9500 . ? C30 C31 1.371(3) . ? C30 H30 0.9500 . ? C31 C32 1.378(3) . ? C31 H31 0.9500 . ? C32 C33 1.381(2) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.394(2) . ? C34 C35 1.402(2) . ? C35 C36 1.379(2) . ? C35 H35 0.9500 . ? C36 C37 1.382(3) . ? C36 H36 0.9500 . ? C37 C38 1.370(3) . ? C37 H37 0.9500 . ? C38 C39 1.396(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.390(2) . ? C40 C45 1.391(2) . ? C41 C42 1.382(2) . ? C41 H41 0.9500 . ? C42 C43 1.375(3) . ? C42 H42 0.9500 . ? C43 C44 1.374(2) . ? C43 H43 0.9500 . ? C44 C45 1.387(2) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.390(2) . ? C46 C51 1.392(2) . ? C47 C48 1.385(2) . ? C47 H47 0.9500 . ? C48 C49 1.370(3) . ? C48 H48 0.9500 . ? C49 C50 1.375(2) . ? C49 H49 0.9500 . ? C50 C51 1.382(2) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? 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 C40 106.75(6) . . ? N1 Si1 C46 111.26(6) . . ? C40 Si1 C46 110.06(7) . . ? N1 Si1 C34 112.72(6) . . ? C40 Si1 C34 108.19(7) . . ? C46 Si1 C34 107.82(7) . . ? C1 N1 Si1 126.19(10) . . ? C1 N1 H1 116.9 . . ? Si1 N1 H1 116.9 . . ? C6 C1 C2 119.21(13) . . ? C6 C1 N1 120.51(13) . . ? C2 C1 N1 120.22(12) . . ? C3 C2 C1 119.45(13) . . ? C3 C2 C8 121.66(13) . . ? C1 C2 C8 118.55(13) . . ? C2 C3 C4 121.70(14) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 117.91(14) . . ? C5 C4 C7 120.70(13) . . ? C3 C4 C7 121.38(14) . . ? C4 C5 C6 122.01(13) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 119.44(13) . . ? C5 C6 C21 120.93(13) . . ? C1 C6 C21 119.13(13) . . ? 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 . . ? C15 C8 C2 113.96(12) . . ? C15 C8 C9 113.26(12) . . ? C2 C8 C9 109.87(12) . . ? C15 C8 H8 106.4 . . ? C2 C8 H8 106.4 . . ? C9 C8 H8 106.4 . . ? C14 C9 C10 117.53(15) . . ? C14 C9 C8 122.17(14) . . ? C10 C9 C8 120.28(14) . . ? C11 C10 C9 121.37(16) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C12 C11 C10 120.01(17) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 119.58(17) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C14 120.15(18) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C9 C14 C13 121.30(17) . . ? C9 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C20 C15 C16 118.54(15) . . ? C20 C15 C8 122.56(15) . . ? C16 C15 C8 118.89(15) . . ? C15 C16 C17 120.85(18) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 119.74(19) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 119.91(17) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.46(19) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C15 C20 C19 120.47(18) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C6 C21 C28 112.64(12) . . ? C6 C21 C22 110.18(12) . . ? C28 C21 C22 114.54(12) . . ? C6 C21 H21 106.3 . . ? C28 C21 H21 106.3 . . ? C22 C21 H21 106.3 . . ? C23 C22 C27 117.82(15) . . ? C23 C22 C21 122.88(14) . . ? C27 C22 C21 119.28(14) . . ? C22 C23 C24 120.95(16) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 120.51(16) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 119.09(16) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C25 C26 C27 120.48(16) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 121.13(15) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? C29 C28 C33 118.38(15) . . ? C29 C28 C21 123.62(15) . . ? C33 C28 C21 118.01(14) . . ? C28 C29 C30 120.53(18) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 120.36(18) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 119.60(17) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C31 C32 C33 120.05(19) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 121.07(17) . . ? C32 C33 H33 119.5 . . ? C28 C33 H33 119.5 . . ? C39 C34 C35 117.13(15) . . ? C39 C34 Si1 122.85(13) . . ? C35 C34 Si1 120.00(12) . . ? C36 C35 C34 121.89(16) . . ? C36 C35 H35 119.1 . . ? C34 C35 H35 119.1 . . ? C35 C36 C37 119.54(18) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 120.30(17) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 120.10(17) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C34 C39 C38 121.01(17) . . ? C34 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C41 C40 C45 116.92(14) . . ? C41 C40 Si1 122.41(12) . . ? C45 C40 Si1 120.67(11) . . ? C42 C41 C40 121.25(16) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C43 C42 C41 120.61(16) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C44 C43 C42 119.56(15) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C45 119.59(15) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C44 C45 C40 122.06(15) . . ? C44 C45 H45 119.0 . . ? C40 C45 H45 119.0 . . ? C47 C46 C51 116.77(15) . . ? C47 C46 Si1 121.43(12) . . ? C51 C46 Si1 121.77(12) . . ? C48 C47 C46 121.47(16) . . ? C48 C47 H47 119.3 . . ? C46 C47 H47 119.3 . . ? C49 C48 C47 120.52(17) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C48 C49 C50 119.29(16) . . ? C48 C49 H49 120.4 . . ? C50 C49 H49 120.4 . . ? C49 C50 C51 120.21(16) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C50 C51 C46 121.73(15) . . ? C50 C51 H51 119.1 . . ? C46 C51 H51 119.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.408 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.040 # Attachment '- compound4.CIF' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 822604' #TrackingRef '- compound4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 Cl Ge N Si' _chemical_formula_weight 618.79 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' Ge Ge 0.1547 1.8001 '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 9.839(2) _cell_length_b 18.298(4) _cell_length_c 19.291(4) _cell_angle_alpha 104.22(3) _cell_angle_beta 98.69(3) _cell_angle_gamma 104.60(3) _cell_volume 3172.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 1.113 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.763 _exptl_absorpt_correction_T_max 0.872 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 21013 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11121 _reflns_number_gt 7502 _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. Two crystallographically independent molecules were refined in the asymmetric unit. There are no significant geometric differences between them. ; _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^)+(0.0454P)^2^+1.6896P] 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 11121 _refine_ls_number_parameters 729 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Ge1 Ge 0.67777(4) 0.78622(2) 0.09310(2) 0.03308(12) Uani 1 1 d . . . Cl1 Cl 0.88115(11) 0.76071(6) 0.13704(6) 0.0520(3) Uani 1 1 d . . . Si1 Si 0.77331(10) 0.69614(6) -0.05296(6) 0.0330(3) Uani 1 1 d . . . N1 N 0.6622(3) 0.74315(15) -0.00648(14) 0.0243(6) Uani 1 1 d . . . C1 C 0.5361(3) 0.75235(18) -0.05001(17) 0.0235(8) Uani 1 1 d . . . Ge2 Ge 0.58314(4) 0.71257(2) 0.39597(2) 0.03677(12) Uani 1 1 d . . . Cl2 Cl 0.74237(14) 0.65330(8) 0.35581(7) 0.0753(4) Uani 1 1 d . . . Si2 Si 0.80902(10) 0.72323(6) 0.54637(6) 0.0378(3) Uani 1 1 d . . . N2 N 0.6592(3) 0.73972(15) 0.49645(14) 0.0250(6) Uani 1 1 d . . . C2 C 0.4026(3) 0.69339(18) -0.06809(17) 0.0225(7) Uani 1 1 d . . . C3 C 0.2858(3) 0.70147(19) -0.11252(19) 0.0286(8) Uani 1 1 d . . . H3 H 0.1963 0.6608 -0.1260 0.034 Uiso 1 1 calc R . . C4 C 0.2950(3) 0.7665(2) -0.13792(19) 0.0316(8) Uani 1 1 d . . . C5 C 0.4265(3) 0.8260(2) -0.11637(18) 0.0292(8) Uani 1 1 d . . . H5 H 0.4335 0.8722 -0.1316 0.035 Uiso 1 1 calc R . . C6 C 0.5479(3) 0.82029(18) -0.07342(17) 0.0229(7) Uani 1 1 d . . . C7 C 0.1680(4) 0.7725(2) -0.1888(2) 0.0494(11) Uani 1 1 d . . . H7A H 0.1734 0.7517 -0.2399 0.074 Uiso 1 1 calc R . . H7B H 0.1702 0.8280 -0.1788 0.074 Uiso 1 1 calc R . . H7C H 0.0780 0.7417 -0.1806 0.074 Uiso 1 1 calc R . . C8 C 0.3877(3) 0.62395(18) -0.03622(18) 0.0263(8) Uani 1 1 d . . . H8 H 0.4784 0.6089 -0.0374 0.032 Uiso 1 1 calc R . . C9 C 0.3802(3) 0.64850(18) 0.04435(19) 0.0279(8) Uani 1 1 d . . . C10 C 0.4542(4) 0.6205(2) 0.0944(2) 0.0361(9) Uani 1 1 d . . . H10 H 0.5114 0.5879 0.0783 0.043 Uiso 1 1 calc R . . C11 C 0.4453(4) 0.6398(2) 0.1673(2) 0.0458(10) Uani 1 1 d . . . H11 H 0.4963 0.6202 0.2008 0.055 Uiso 1 1 calc R . . C12 C 0.3630(4) 0.6870(2) 0.1914(2) 0.0442(10) Uani 1 1 d . . . H12 H 0.3555 0.6996 0.2412 0.053 Uiso 1 1 calc R . . C13 C 0.2909(4) 0.7162(2) 0.1422(2) 0.0384(9) Uani 1 1 d . . . H13 H 0.2349 0.7495 0.1586 0.046 Uiso 1 1 calc R . . C14 C 0.2998(4) 0.69732(19) 0.0698(2) 0.0326(9) Uani 1 1 d . . . H14 H 0.2503 0.7180 0.0368 0.039 Uiso 1 1 calc R . . C15 C 0.2632(3) 0.55007(18) -0.08141(18) 0.0250(8) Uani 1 1 d . . . C16 C 0.1247(3) 0.53544(19) -0.06879(19) 0.0301(8) Uani 1 1 d . . . H16 H 0.1046 0.5726 -0.0309 0.036 Uiso 1 1 calc R . . C17 C 0.0158(4) 0.4676(2) -0.11063(19) 0.0330(9) Uani 1 1 d . . . H17 H -0.0784 0.4585 -0.1016 0.040 Uiso 1 1 calc R . . C18 C 0.0444(4) 0.4132(2) -0.16556(19) 0.0349(9) Uani 1 1 d . . . H18 H -0.0300 0.3664 -0.1939 0.042 Uiso 1 1 calc R . . C19 C 0.1800(4) 0.4267(2) -0.1794(2) 0.0383(9) Uani 1 1 d . . . H19 H 0.1994 0.3895 -0.2175 0.046 Uiso 1 1 calc R . . C20 C 0.2884(4) 0.49484(19) -0.13759(19) 0.0309(8) Uani 1 1 d . . . H20 H 0.3818 0.5040 -0.1476 0.037 Uiso 1 1 calc R . . C21 C 0.6926(3) 0.88545(18) -0.05041(17) 0.0255(8) Uani 1 1 d . . . H21 H 0.7675 0.8584 -0.0596 0.031 Uiso 1 1 calc R . . C22 C 0.7307(3) 0.92809(18) 0.03138(18) 0.0240(8) Uani 1 1 d . . . C23 C 0.8705(3) 0.94780(19) 0.07251(19) 0.0301(8) Uani 1 1 d . . . H23 H 0.9430 0.9349 0.0489 0.036 Uiso 1 1 calc R . . C24 C 0.9059(4) 0.9857(2) 0.1470(2) 0.0393(10) Uani 1 1 d . . . H24 H 1.0020 0.9985 0.1742 0.047 Uiso 1 1 calc R . . C25 C 0.8016(4) 1.0051(2) 0.1820(2) 0.0387(9) Uani 1 1 d . . . H25 H 0.8254 1.0308 0.2334 0.046 Uiso 1 1 calc R . . C26 C 0.6623(4) 0.9868(2) 0.1417(2) 0.0363(9) Uani 1 1 d . . . H26 H 0.5904 1.0006 0.1653 0.044 Uiso 1 1 calc R . . C27 C 0.6274(3) 0.94873(19) 0.06760(19) 0.0292(8) Uani 1 1 d . . . H27 H 0.5313 0.9363 0.0406 0.035 Uiso 1 1 calc R . . C28 C 0.7022(3) 0.9425(2) -0.09726(19) 0.0289(8) Uani 1 1 d . . . C29 C 0.7241(3) 1.0229(2) -0.0676(2) 0.0334(9) Uani 1 1 d . . . H29 H 0.7347 1.0444 -0.0163 0.040 Uiso 1 1 calc R . . C30 C 0.7308(4) 1.0724(2) -0.1121(2) 0.0455(11) Uani 1 1 d . . . H30 H 0.7462 1.1273 -0.0908 0.055 Uiso 1 1 calc R . . C31 C 0.7154(4) 1.0431(3) -0.1861(3) 0.0507(12) Uani 1 1 d . . . H31 H 0.7189 1.0772 -0.2163 0.061 Uiso 1 1 calc R . . C32 C 0.6945(4) 0.9632(3) -0.2167(2) 0.0504(12) Uani 1 1 d . . . H32 H 0.6845 0.9424 -0.2681 0.060 Uiso 1 1 calc R . . C33 C 0.6881(4) 0.9131(2) -0.1726(2) 0.0390(9) Uani 1 1 d . . . H33 H 0.6740 0.8583 -0.1941 0.047 Uiso 1 1 calc R . . C34 C 0.7759(4) 0.6037(2) -0.0297(2) 0.0518(11) Uani 1 1 d . . . H34A H 0.8055 0.6155 0.0237 0.078 Uiso 1 1 calc R . . H34B H 0.8443 0.5815 -0.0531 0.078 Uiso 1 1 calc R . . H34C H 0.6793 0.5654 -0.0475 0.078 Uiso 1 1 calc R . . C35 C 0.6986(4) 0.6700(3) -0.1533(2) 0.0545(12) Uani 1 1 d . . . H35A H 0.6024 0.6316 -0.1664 0.082 Uiso 1 1 calc R . . H35B H 0.7622 0.6470 -0.1802 0.082 Uiso 1 1 calc R . . H35C H 0.6919 0.7178 -0.1663 0.082 Uiso 1 1 calc R . . C36 C 0.9617(4) 0.7626(2) -0.0326(2) 0.0500(11) Uani 1 1 d . . . H36A H 0.9627 0.8062 -0.0537 0.075 Uiso 1 1 calc R . . H36B H 1.0226 0.7326 -0.0540 0.075 Uiso 1 1 calc R . . H36C H 0.9990 0.7839 0.0207 0.075 Uiso 1 1 calc R . . C37 C 0.5750(3) 0.78096(18) 0.53637(17) 0.0228(7) Uani 1 1 d . . . C38 C 0.4584(3) 0.73851(18) 0.55923(17) 0.0233(7) Uani 1 1 d . . . C39 C 0.3809(3) 0.78003(19) 0.59905(17) 0.0254(8) Uani 1 1 d . . . H39 H 0.3041 0.7516 0.6157 0.031 Uiso 1 1 calc R . . C40 C 0.4115(3) 0.86126(19) 0.61529(18) 0.0257(8) Uani 1 1 d . . . C41 C 0.5248(3) 0.90152(18) 0.59054(17) 0.0232(7) Uani 1 1 d . . . H41 H 0.5458 0.9571 0.6001 0.028 Uiso 1 1 calc R . . C42 C 0.6079(3) 0.86342(18) 0.55246(17) 0.0232(7) Uani 1 1 d . . . C43 C 0.3277(4) 0.9050(2) 0.6602(2) 0.0381(9) Uani 1 1 d . . . H43A H 0.2839 0.9343 0.6320 0.057 Uiso 1 1 calc R . . H43B H 0.3930 0.9420 0.7057 0.057 Uiso 1 1 calc R . . H43C H 0.2519 0.8670 0.6721 0.057 Uiso 1 1 calc R . . C44 C 0.4167(3) 0.64831(18) 0.53715(18) 0.0259(8) Uani 1 1 d . . . H44 H 0.5090 0.6345 0.5434 0.031 Uiso 1 1 calc R . . C45 C 0.3436(3) 0.61368(19) 0.45592(19) 0.0282(8) Uani 1 1 d . . . C46 C 0.3857(4) 0.5558(2) 0.4106(2) 0.0381(9) Uani 1 1 d . . . H46 H 0.4592 0.5371 0.4312 0.046 Uiso 1 1 calc R . . C47 C 0.3234(5) 0.5248(2) 0.3363(2) 0.0510(11) Uani 1 1 d . . . H47 H 0.3549 0.4858 0.3062 0.061 Uiso 1 1 calc R . . C48 C 0.2150(5) 0.5509(3) 0.3060(2) 0.0547(12) Uani 1 1 d . . . H48 H 0.1707 0.5294 0.2552 0.066 Uiso 1 1 calc R . . C49 C 0.1713(4) 0.6083(2) 0.3500(2) 0.0463(10) Uani 1 1 d . . . H49 H 0.0967 0.6263 0.3293 0.056 Uiso 1 1 calc R . . C50 C 0.2355(4) 0.6396(2) 0.4238(2) 0.0346(9) Uani 1 1 d . . . H50 H 0.2055 0.6796 0.4533 0.042 Uiso 1 1 calc R . . C51 C 0.3299(3) 0.61260(18) 0.58741(18) 0.0260(8) Uani 1 1 d . . . C52 C 0.1812(4) 0.5811(2) 0.5693(2) 0.0341(9) Uani 1 1 d . . . H52 H 0.1279 0.5799 0.5234 0.041 Uiso 1 1 calc R . . C53 C 0.1097(4) 0.5515(2) 0.6178(2) 0.0379(9) Uani 1 1 d . . . H53 H 0.0077 0.5298 0.6046 0.045 Uiso 1 1 calc R . . C54 C 0.1831(4) 0.5527(2) 0.6840(2) 0.0461(10) Uani 1 1 d . . . H54 H 0.1331 0.5322 0.7168 0.055 Uiso 1 1 calc R . . C55 C 0.3298(5) 0.5841(3) 0.7026(2) 0.0688(15) Uani 1 1 d . . . H55 H 0.3824 0.5858 0.7488 0.083 Uiso 1 1 calc R . . C56 C 0.4019(4) 0.6133(3) 0.6542(2) 0.0563(12) Uani 1 1 d . . . H56 H 0.5041 0.6345 0.6677 0.068 Uiso 1 1 calc R . . C57 C 0.7292(3) 0.90845(18) 0.52324(17) 0.0234(7) Uani 1 1 d . . . H57 H 0.8086 0.8839 0.5286 0.028 Uiso 1 1 calc R . . C58 C 0.6796(3) 0.89658(18) 0.44193(18) 0.0240(8) Uani 1 1 d . . . C59 C 0.7687(4) 0.8829(2) 0.3935(2) 0.0346(9) Uani 1 1 d . . . H59 H 0.8636 0.8824 0.4118 0.041 Uiso 1 1 calc R . . C60 C 0.7200(4) 0.8699(2) 0.3188(2) 0.0441(10) Uani 1 1 d . . . H60 H 0.7818 0.8603 0.2865 0.053 Uiso 1 1 calc R . . C61 C 0.5835(4) 0.87086(19) 0.2910(2) 0.0351(9) Uani 1 1 d . . . H61 H 0.5509 0.8622 0.2399 0.042 Uiso 1 1 calc R . . C62 C 0.4946(4) 0.8845(2) 0.3381(2) 0.0333(9) Uani 1 1 d . . . H62 H 0.4002 0.8855 0.3195 0.040 Uiso 1 1 calc R . . C63 C 0.5425(3) 0.89673(19) 0.41229(19) 0.0305(8) Uani 1 1 d . . . H63 H 0.4793 0.9055 0.4440 0.037 Uiso 1 1 calc R . . C64 C 0.7924(3) 0.99564(19) 0.56896(18) 0.0255(8) Uani 1 1 d . . . C65 C 0.8686(3) 1.0136(2) 0.64103(19) 0.0334(9) Uani 1 1 d . . . H65 H 0.8840 0.9720 0.6594 0.040 Uiso 1 1 calc R . . C66 C 0.9225(4) 1.0910(2) 0.6865(2) 0.0425(10) Uani 1 1 d . . . H66 H 0.9731 1.1019 0.7357 0.051 Uiso 1 1 calc R . . C67 C 0.9026(4) 1.1517(2) 0.6603(2) 0.0434(10) Uani 1 1 d . . . H67 H 0.9395 1.2048 0.6912 0.052 Uiso 1 1 calc R . . C68 C 0.8283(4) 1.1353(2) 0.5885(2) 0.0411(10) Uani 1 1 d . . . H68 H 0.8141 1.1771 0.5700 0.049 Uiso 1 1 calc R . . C69 C 0.7745(3) 1.0574(2) 0.5434(2) 0.0319(9) Uani 1 1 d . . . H69 H 0.7246 1.0467 0.4941 0.038 Uiso 1 1 calc R . . C70 C 0.8208(4) 0.7672(3) 0.6459(2) 0.0563(12) Uani 1 1 d . . . H70A H 0.8369 0.8243 0.6566 0.084 Uiso 1 1 calc R . . H70B H 0.9012 0.7574 0.6751 0.084 Uiso 1 1 calc R . . H70C H 0.7306 0.7429 0.6584 0.084 Uiso 1 1 calc R . . C71 C 0.9798(4) 0.7728(3) 0.5245(3) 0.0643(14) Uani 1 1 d . . . H71A H 0.9721 0.7545 0.4715 0.096 Uiso 1 1 calc R . . H71B H 1.0600 0.7599 0.5504 0.096 Uiso 1 1 calc R . . H71C H 0.9973 0.8302 0.5401 0.096 Uiso 1 1 calc R . . C72 C 0.7900(4) 0.6163(2) 0.5289(3) 0.0604(13) Uani 1 1 d . . . H72A H 0.7093 0.5916 0.5480 0.091 Uiso 1 1 calc R . . H72B H 0.8791 0.6100 0.5536 0.091 Uiso 1 1 calc R . . H72C H 0.7716 0.5910 0.4760 0.091 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 Ge1 0.0399(2) 0.0313(2) 0.0268(2) 0.00640(18) 0.00359(18) 0.01306(17) Cl1 0.0552(6) 0.0488(6) 0.0421(6) 0.0043(5) -0.0143(5) 0.0227(5) Si1 0.0260(5) 0.0352(6) 0.0345(6) 0.0018(5) 0.0026(4) 0.0143(4) N1 0.0237(14) 0.0255(15) 0.0223(15) 0.0051(12) 0.0022(12) 0.0088(11) C1 0.0223(17) 0.0277(19) 0.0204(18) 0.0037(15) 0.0028(14) 0.0119(14) Ge2 0.0469(2) 0.0354(2) 0.0278(2) 0.00652(18) 0.01198(19) 0.01270(18) Cl2 0.1048(10) 0.0858(9) 0.0592(8) 0.0155(7) 0.0478(7) 0.0588(8) Si2 0.0302(5) 0.0427(6) 0.0490(7) 0.0203(5) 0.0113(5) 0.0180(5) N2 0.0280(15) 0.0266(15) 0.0239(16) 0.0061(13) 0.0122(12) 0.0121(12) C2 0.0228(17) 0.0232(18) 0.0235(19) 0.0095(15) 0.0061(15) 0.0078(14) C3 0.0237(18) 0.030(2) 0.032(2) 0.0124(16) 0.0052(16) 0.0051(14) C4 0.0249(18) 0.035(2) 0.036(2) 0.0153(18) 0.0038(16) 0.0093(15) C5 0.0293(19) 0.033(2) 0.033(2) 0.0188(17) 0.0099(16) 0.0121(16) C6 0.0212(17) 0.0246(18) 0.0245(19) 0.0071(15) 0.0067(15) 0.0089(14) C7 0.032(2) 0.056(3) 0.061(3) 0.034(2) -0.006(2) 0.0083(18) C8 0.0221(17) 0.0264(18) 0.030(2) 0.0093(16) 0.0039(15) 0.0072(14) C9 0.0256(18) 0.0220(18) 0.031(2) 0.0090(16) 0.0004(16) -0.0004(14) C10 0.040(2) 0.030(2) 0.034(2) 0.0130(18) 0.0004(18) 0.0053(16) C11 0.055(3) 0.042(2) 0.035(3) 0.017(2) -0.002(2) 0.005(2) C12 0.053(2) 0.039(2) 0.026(2) 0.0065(19) 0.0053(19) -0.006(2) C13 0.043(2) 0.027(2) 0.038(2) 0.0061(18) 0.0077(19) 0.0027(17) C14 0.034(2) 0.0264(19) 0.033(2) 0.0083(17) 0.0034(17) 0.0043(15) C15 0.0279(18) 0.0235(18) 0.025(2) 0.0117(16) 0.0019(15) 0.0081(14) C16 0.031(2) 0.029(2) 0.029(2) 0.0048(16) 0.0046(16) 0.0108(15) C17 0.0274(19) 0.033(2) 0.034(2) 0.0092(18) 0.0016(16) 0.0057(16) C18 0.039(2) 0.029(2) 0.029(2) 0.0070(17) -0.0016(17) 0.0031(16) C19 0.049(2) 0.033(2) 0.031(2) 0.0035(18) 0.0095(18) 0.0162(18) C20 0.034(2) 0.030(2) 0.032(2) 0.0108(17) 0.0115(17) 0.0118(16) C21 0.0199(17) 0.0286(19) 0.028(2) 0.0078(16) 0.0050(15) 0.0081(14) C22 0.0272(18) 0.0200(17) 0.029(2) 0.0127(15) 0.0085(16) 0.0075(14) C23 0.0258(19) 0.032(2) 0.033(2) 0.0079(17) 0.0075(16) 0.0121(15) C24 0.029(2) 0.044(2) 0.035(2) 0.0039(19) -0.0033(17) 0.0084(17) C25 0.046(2) 0.036(2) 0.029(2) 0.0003(17) 0.0050(19) 0.0145(18) C26 0.041(2) 0.036(2) 0.037(2) 0.0095(18) 0.0148(19) 0.0173(17) C27 0.0248(18) 0.030(2) 0.032(2) 0.0087(17) 0.0054(16) 0.0089(15) C28 0.0164(17) 0.039(2) 0.031(2) 0.0163(18) 0.0039(15) 0.0025(14) C29 0.0247(18) 0.037(2) 0.040(2) 0.0169(19) 0.0050(16) 0.0085(15) C30 0.032(2) 0.051(3) 0.060(3) 0.033(2) 0.007(2) 0.0099(18) C31 0.029(2) 0.072(3) 0.065(3) 0.048(3) 0.012(2) 0.011(2) C32 0.027(2) 0.090(4) 0.034(2) 0.033(3) 0.0044(18) 0.005(2) C33 0.030(2) 0.047(2) 0.037(2) 0.014(2) 0.0083(17) 0.0029(17) C34 0.052(3) 0.041(2) 0.062(3) 0.006(2) 0.008(2) 0.025(2) C35 0.051(3) 0.072(3) 0.038(3) -0.001(2) 0.013(2) 0.028(2) C36 0.030(2) 0.056(3) 0.061(3) 0.007(2) 0.015(2) 0.0141(18) C37 0.0232(17) 0.0288(19) 0.0176(18) 0.0063(15) 0.0026(14) 0.0114(14) C38 0.0239(17) 0.0227(18) 0.0217(19) 0.0082(15) 0.0009(15) 0.0053(14) C39 0.0227(17) 0.031(2) 0.0251(19) 0.0089(16) 0.0101(15) 0.0086(14) C40 0.0235(18) 0.029(2) 0.0238(19) 0.0048(16) 0.0058(15) 0.0097(14) C41 0.0263(17) 0.0192(17) 0.0219(19) 0.0035(14) 0.0051(15) 0.0057(14) C42 0.0215(17) 0.0265(19) 0.0201(18) 0.0074(15) 0.0032(14) 0.0050(14) C43 0.039(2) 0.031(2) 0.044(2) 0.0039(18) 0.0194(18) 0.0114(16) C44 0.0267(18) 0.0276(19) 0.027(2) 0.0116(16) 0.0075(15) 0.0106(14) C45 0.0325(19) 0.0218(18) 0.029(2) 0.0092(16) 0.0105(16) 0.0012(15) C46 0.046(2) 0.028(2) 0.037(2) 0.0081(18) 0.0108(19) 0.0064(17) C47 0.068(3) 0.035(2) 0.037(3) -0.002(2) 0.016(2) 0.003(2) C48 0.062(3) 0.052(3) 0.030(2) 0.008(2) 0.000(2) -0.007(2) C49 0.045(2) 0.048(3) 0.038(3) 0.020(2) 0.003(2) -0.0005(19) C50 0.038(2) 0.031(2) 0.033(2) 0.0131(17) 0.0066(18) 0.0047(16) C51 0.0294(19) 0.0204(18) 0.029(2) 0.0092(15) 0.0059(16) 0.0085(14) C52 0.033(2) 0.036(2) 0.035(2) 0.0190(18) 0.0068(17) 0.0055(16) C53 0.030(2) 0.035(2) 0.047(3) 0.0163(19) 0.0086(19) 0.0031(16) C54 0.044(2) 0.058(3) 0.039(3) 0.028(2) 0.010(2) 0.007(2) C55 0.047(3) 0.109(4) 0.048(3) 0.052(3) -0.003(2) -0.001(3) C56 0.030(2) 0.086(3) 0.052(3) 0.040(3) 0.002(2) 0.001(2) C57 0.0215(17) 0.0266(18) 0.0235(19) 0.0078(15) 0.0057(14) 0.0086(14) C58 0.0286(18) 0.0192(17) 0.0231(19) 0.0051(15) 0.0084(15) 0.0047(14) C59 0.0249(19) 0.047(2) 0.031(2) 0.0092(18) 0.0108(16) 0.0075(16) C60 0.042(2) 0.058(3) 0.031(2) 0.009(2) 0.0180(19) 0.0103(19) C61 0.040(2) 0.030(2) 0.028(2) 0.0061(17) 0.0044(18) 0.0010(16) C62 0.032(2) 0.037(2) 0.032(2) 0.0140(17) 0.0028(17) 0.0100(16) C63 0.0308(19) 0.036(2) 0.029(2) 0.0106(17) 0.0103(16) 0.0131(16) C64 0.0181(17) 0.0267(19) 0.030(2) 0.0077(16) 0.0095(15) 0.0030(14) C65 0.0286(19) 0.037(2) 0.031(2) 0.0108(18) 0.0084(17) 0.0019(16) C66 0.033(2) 0.048(3) 0.032(2) 0.003(2) 0.0105(18) -0.0042(18) C67 0.035(2) 0.035(2) 0.042(3) -0.008(2) 0.0152(19) -0.0052(17) C68 0.036(2) 0.028(2) 0.063(3) 0.015(2) 0.026(2) 0.0076(16) C69 0.0276(19) 0.033(2) 0.035(2) 0.0089(18) 0.0114(16) 0.0084(15) C70 0.055(3) 0.076(3) 0.042(3) 0.022(2) -0.002(2) 0.029(2) C71 0.031(2) 0.080(3) 0.096(4) 0.045(3) 0.017(2) 0.022(2) C72 0.056(3) 0.059(3) 0.084(4) 0.033(3) 0.020(2) 0.036(2) _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 Ge1 N1 1.855(3) . ? Ge1 Cl1 2.2566(12) . ? Si1 N1 1.769(3) . ? Si1 C34 1.858(4) . ? Si1 C35 1.859(4) . ? Si1 C36 1.865(4) . ? N1 C1 1.460(4) . ? C1 C2 1.405(4) . ? C1 C6 1.408(4) . ? Ge2 N2 1.862(3) . ? Ge2 Cl2 2.2452(13) . ? Si2 N2 1.769(3) . ? Si2 C72 1.857(4) . ? Si2 C71 1.859(4) . ? Si2 C70 1.864(4) . ? N2 C37 1.439(4) . ? C2 C3 1.388(4) . ? C2 C8 1.527(4) . ? C3 C4 1.382(5) . ? C4 C5 1.392(4) . ? C4 C7 1.513(5) . ? C5 C6 1.389(4) . ? C6 C21 1.530(4) . ? C8 C9 1.527(5) . ? C8 C15 1.533(4) . ? C9 C14 1.386(5) . ? C9 C10 1.393(5) . ? C10 C11 1.386(5) . ? C11 C12 1.374(5) . ? C12 C13 1.387(5) . ? C13 C14 1.376(5) . ? C15 C20 1.388(5) . ? C15 C16 1.391(4) . ? C16 C17 1.384(4) . ? C17 C18 1.380(5) . ? C18 C19 1.373(5) . ? C19 C20 1.384(5) . ? C21 C22 1.519(4) . ? C21 C28 1.534(5) . ? C22 C23 1.390(4) . ? C22 C27 1.393(4) . ? C23 C24 1.380(5) . ? C24 C25 1.382(5) . ? C25 C26 1.384(5) . ? C26 C27 1.374(5) . ? C28 C29 1.389(5) . ? C28 C33 1.392(5) . ? C29 C30 1.389(5) . ? C30 C31 1.367(6) . ? C31 C32 1.384(6) . ? C32 C33 1.393(5) . ? C37 C42 1.404(4) . ? C37 C38 1.409(4) . ? C38 C39 1.389(4) . ? C38 C44 1.528(4) . ? C39 C40 1.384(4) . ? C40 C41 1.390(4) . ? C40 C43 1.509(4) . ? C41 C42 1.382(4) . ? C42 C57 1.535(4) . ? C44 C45 1.522(5) . ? C44 C51 1.542(5) . ? C45 C46 1.391(5) . ? C45 C50 1.393(5) . ? C46 C47 1.383(5) . ? C47 C48 1.384(6) . ? C48 C49 1.381(6) . ? C49 C50 1.378(5) . ? C51 C56 1.368(5) . ? C51 C52 1.384(4) . ? C52 C53 1.386(5) . ? C53 C54 1.360(5) . ? C54 C55 1.366(5) . ? C55 C56 1.384(6) . ? C57 C58 1.514(4) . ? C57 C64 1.534(4) . ? C58 C63 1.384(4) . ? C58 C59 1.395(5) . ? C59 C60 1.389(5) . ? C60 C61 1.375(5) . ? C61 C62 1.375(5) . ? C62 C63 1.381(5) . ? C64 C69 1.379(5) . ? C64 C65 1.393(5) . ? C65 C66 1.389(5) . ? C66 C67 1.374(5) . ? C67 C68 1.387(5) . ? C68 C69 1.392(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ge1 Cl1 98.85(9) . . ? N1 Si1 C34 111.49(17) . . ? N1 Si1 C35 108.10(15) . . ? C34 Si1 C35 108.3(2) . . ? N1 Si1 C36 111.93(15) . . ? C34 Si1 C36 109.33(19) . . ? C35 Si1 C36 107.6(2) . . ? C1 N1 Si1 118.5(2) . . ? C1 N1 Ge1 110.95(19) . . ? Si1 N1 Ge1 130.54(15) . . ? C2 C1 C6 120.0(3) . . ? C2 C1 N1 119.8(3) . . ? C6 C1 N1 120.2(3) . . ? N2 Ge2 Cl2 98.54(9) . . ? N2 Si2 C72 112.24(17) . . ? N2 Si2 C71 111.23(17) . . ? C72 Si2 C71 109.1(2) . . ? N2 Si2 C70 107.58(16) . . ? C72 Si2 C70 108.4(2) . . ? C71 Si2 C70 108.1(2) . . ? C37 N2 Si2 118.7(2) . . ? C37 N2 Ge2 109.89(19) . . ? Si2 N2 Ge2 131.39(15) . . ? C3 C2 C1 118.8(3) . . ? C3 C2 C8 121.6(3) . . ? C1 C2 C8 119.5(3) . . ? C4 C3 C2 122.4(3) . . ? C3 C4 C5 117.8(3) . . ? C3 C4 C7 121.5(3) . . ? C5 C4 C7 120.7(3) . . ? C6 C5 C4 122.3(3) . . ? C5 C6 C1 118.6(3) . . ? C5 C6 C21 122.2(3) . . ? C1 C6 C21 119.2(3) . . ? C9 C8 C2 111.3(3) . . ? C9 C8 C15 111.8(3) . . ? C2 C8 C15 113.8(3) . . ? C14 C9 C10 118.2(3) . . ? C14 C9 C8 122.1(3) . . ? C10 C9 C8 119.7(3) . . ? C11 C10 C9 120.9(4) . . ? C12 C11 C10 120.2(4) . . ? C11 C12 C13 119.3(4) . . ? C14 C13 C12 120.6(4) . . ? C13 C14 C9 120.8(3) . . ? C20 C15 C16 117.9(3) . . ? C20 C15 C8 119.1(3) . . ? C16 C15 C8 122.9(3) . . ? C17 C16 C15 121.0(3) . . ? C18 C17 C16 119.8(3) . . ? C19 C18 C17 120.2(3) . . ? C18 C19 C20 119.7(3) . . ? C19 C20 C15 121.3(3) . . ? C22 C21 C6 111.7(3) . . ? C22 C21 C28 112.6(3) . . ? C6 C21 C28 112.9(3) . . ? C23 C22 C27 117.8(3) . . ? C23 C22 C21 120.7(3) . . ? C27 C22 C21 121.4(3) . . ? C24 C23 C22 121.2(3) . . ? C23 C24 C25 120.0(3) . . ? C24 C25 C26 119.5(3) . . ? C27 C26 C25 120.3(3) . . ? C26 C27 C22 121.2(3) . . ? C29 C28 C33 118.1(3) . . ? C29 C28 C21 122.6(3) . . ? C33 C28 C21 119.3(3) . . ? C30 C29 C28 120.8(4) . . ? C31 C30 C29 120.8(4) . . ? C30 C31 C32 119.4(4) . . ? C31 C32 C33 120.3(4) . . ? C28 C33 C32 120.6(4) . . ? C42 C37 C38 119.7(3) . . ? C42 C37 N2 120.4(3) . . ? C38 C37 N2 120.0(3) . . ? C39 C38 C37 118.7(3) . . ? C39 C38 C44 121.8(3) . . ? C37 C38 C44 119.4(3) . . ? C40 C39 C38 122.4(3) . . ? C39 C40 C41 117.7(3) . . ? C39 C40 C43 121.2(3) . . ? C41 C40 C43 121.1(3) . . ? C42 C41 C40 122.3(3) . . ? C41 C42 C37 119.2(3) . . ? C41 C42 C57 121.5(3) . . ? C37 C42 C57 119.2(3) . . ? C45 C44 C38 110.1(3) . . ? C45 C44 C51 113.7(3) . . ? C38 C44 C51 113.1(3) . . ? C46 C45 C50 117.5(3) . . ? C46 C45 C44 120.6(3) . . ? C50 C45 C44 121.9(3) . . ? C47 C46 C45 121.7(4) . . ? C46 C47 C48 119.5(4) . . ? C49 C48 C47 119.8(4) . . ? C50 C49 C48 120.2(4) . . ? C49 C50 C45 121.2(4) . . ? C56 C51 C52 117.8(3) . . ? C56 C51 C44 118.9(3) . . ? C52 C51 C44 123.3(3) . . ? C51 C52 C53 120.2(3) . . ? C54 C53 C52 121.2(3) . . ? C53 C54 C55 119.0(4) . . ? C54 C55 C56 120.2(4) . . ? C51 C56 C55 121.6(4) . . ? C58 C57 C64 113.6(3) . . ? C58 C57 C42 110.6(2) . . ? C64 C57 C42 112.1(3) . . ? C63 C58 C59 117.2(3) . . ? C63 C58 C57 121.3(3) . . ? C59 C58 C57 121.4(3) . . ? C60 C59 C58 120.7(3) . . ? C61 C60 C59 120.8(3) . . ? C60 C61 C62 119.2(3) . . ? C61 C62 C63 120.0(3) . . ? C62 C63 C58 122.1(3) . . ? C69 C64 C65 117.9(3) . . ? C69 C64 C57 123.6(3) . . ? C65 C64 C57 118.4(3) . . ? C66 C65 C64 121.3(4) . . ? C67 C66 C65 119.9(4) . . ? C66 C67 C68 119.7(3) . . ? C67 C68 C69 119.8(4) . . ? C64 C69 C68 121.3(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.383 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.066 # Attachment '- compound7.CIF' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 822605' #TrackingRef '- compound7.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 Cl N Si Sn' _chemical_formula_weight 664.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Sn Sn -0.6537 1.4246 '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 9.799(2) _cell_length_b 18.329(4) _cell_length_c 19.472(4) _cell_angle_alpha 103.50(3) _cell_angle_beta 98.96(3) _cell_angle_gamma 104.63(3) _cell_volume 3203.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 21201 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11268 _reflns_number_gt 7479 _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. Two crystallographically independent molecules were refined in the asymmetric unit.There are no significant geometric differences between them. ; _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^)+(0.0516P)^2^+1.3980P] 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 11268 _refine_ls_number_parameters 729 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Sn1 Sn 0.68095(4) 0.787807(18) 0.099294(16) 0.03324(11) Uani 1 1 d . . . Cl1 Cl 0.90888(15) 0.76287(8) 0.14003(7) 0.0530(4) Uani 1 1 d . . . Si1 Si 0.77338(14) 0.69509(8) -0.05539(7) 0.0337(3) Uani 1 1 d . . . N1 N 0.6619(4) 0.74132(19) -0.01095(18) 0.0254(8) Uani 1 1 d . . . C1 C 0.5360(4) 0.7498(2) -0.0533(2) 0.0222(10) Uani 1 1 d . . . Sn2 Sn 0.57779(4) 0.712560(18) 0.390399(16) 0.03671(12) Uani 1 1 d . . . Cl2 Cl 0.7614(2) 0.65421(11) 0.35461(9) 0.0869(6) Uani 1 1 d . . . Si2 Si 0.81138(14) 0.72499(8) 0.55028(8) 0.0376(3) Uani 1 1 d . . . N2 N 0.6634(4) 0.74188(19) 0.50129(17) 0.0242(8) Uani 1 1 d . . . C2 C 0.4016(4) 0.6920(2) -0.0719(2) 0.0228(10) Uani 1 1 d . . . C3 C 0.2834(5) 0.6998(2) -0.1159(2) 0.0253(10) Uani 1 1 d . . . H3 H 0.1938 0.6591 -0.1293 0.030 Uiso 1 1 calc R . . C4 C 0.2924(5) 0.7652(3) -0.1405(2) 0.0293(11) Uani 1 1 d . . . C5 C 0.4242(5) 0.8250(2) -0.1180(2) 0.0286(11) Uani 1 1 d . . . H5 H 0.4306 0.8718 -0.1321 0.034 Uiso 1 1 calc R . . C6 C 0.5464(4) 0.8186(2) -0.0760(2) 0.0230(10) Uani 1 1 d . . . C7 C 0.1657(5) 0.7716(3) -0.1913(3) 0.0456(14) Uani 1 1 d . . . H7A H 0.1671 0.7472 -0.2416 0.068 Uiso 1 1 calc R . . H7B H 0.1726 0.8272 -0.1848 0.068 Uiso 1 1 calc R . . H7C H 0.0750 0.7446 -0.1807 0.068 Uiso 1 1 calc R . . C8 C 0.3875(5) 0.6220(2) -0.0404(2) 0.0248(10) Uani 1 1 d . . . H8 H 0.4779 0.6064 -0.0424 0.030 Uiso 1 1 calc R . . C9 C 0.3834(4) 0.6468(2) 0.0395(2) 0.0254(10) Uani 1 1 d . . . C10 C 0.4581(5) 0.6193(2) 0.0895(3) 0.0352(12) Uani 1 1 d . . . H10 H 0.5140 0.5861 0.0735 0.042 Uiso 1 1 calc R . . C11 C 0.4533(6) 0.6389(3) 0.1619(3) 0.0431(13) Uani 1 1 d . . . H11 H 0.5061 0.6199 0.1953 0.052 Uiso 1 1 calc R . . C12 C 0.3709(5) 0.6862(3) 0.1848(3) 0.0401(13) Uani 1 1 d . . . H12 H 0.3659 0.6992 0.2344 0.048 Uiso 1 1 calc R . . C13 C 0.2955(5) 0.7152(3) 0.1375(2) 0.0339(12) Uani 1 1 d . . . H13 H 0.2394 0.7481 0.1540 0.041 Uiso 1 1 calc R . . C14 C 0.3026(5) 0.6954(2) 0.0649(2) 0.0299(11) Uani 1 1 d . . . H14 H 0.2512 0.7155 0.0321 0.036 Uiso 1 1 calc R . . C15 C 0.2606(5) 0.5493(2) -0.0833(2) 0.0250(10) Uani 1 1 d . . . C16 C 0.1230(5) 0.5357(2) -0.0699(2) 0.0278(11) Uani 1 1 d . . . H16 H 0.1049 0.5729 -0.0322 0.033 Uiso 1 1 calc R . . C17 C 0.0105(5) 0.4685(2) -0.1104(2) 0.0333(11) Uani 1 1 d . . . H17 H -0.0831 0.4597 -0.1004 0.040 Uiso 1 1 calc R . . C18 C 0.0375(5) 0.4147(3) -0.1658(2) 0.0359(12) Uani 1 1 d . . . H18 H -0.0382 0.3686 -0.1937 0.043 Uiso 1 1 calc R . . C19 C 0.1712(5) 0.4275(3) -0.1802(2) 0.0360(12) Uani 1 1 d . . . H19 H 0.1880 0.3904 -0.2184 0.043 Uiso 1 1 calc R . . C20 C 0.2839(5) 0.4942(2) -0.1396(2) 0.0312(11) Uani 1 1 d . . . H20 H 0.3770 0.5023 -0.1503 0.037 Uiso 1 1 calc R . . C21 C 0.6909(4) 0.8847(2) -0.0524(2) 0.0248(10) Uani 1 1 d . . . H21 H 0.7673 0.8585 -0.0607 0.030 Uiso 1 1 calc R . . C22 C 0.7261(4) 0.9254(2) 0.0289(2) 0.0243(10) Uani 1 1 d . . . C23 C 0.8660(5) 0.9441(2) 0.0704(2) 0.0308(11) Uani 1 1 d . . . H23 H 0.9396 0.9313 0.0479 0.037 Uiso 1 1 calc R . . C24 C 0.8994(5) 0.9816(3) 0.1450(2) 0.0370(12) Uani 1 1 d . . . H24 H 0.9947 0.9934 0.1731 0.044 Uiso 1 1 calc R . . C25 C 0.7938(5) 1.0012(3) 0.1773(2) 0.0362(12) Uani 1 1 d . . . H25 H 0.8162 1.0266 0.2279 0.043 Uiso 1 1 calc R . . C26 C 0.6543(5) 0.9840(2) 0.1364(2) 0.0317(11) Uani 1 1 d . . . H26 H 0.5817 0.9982 0.1589 0.038 Uiso 1 1 calc R . . C27 C 0.6212(5) 0.9464(2) 0.0630(2) 0.0311(11) Uani 1 1 d . . . H27 H 0.5255 0.9346 0.0354 0.037 Uiso 1 1 calc R . . C28 C 0.7022(4) 0.9427(2) -0.0976(2) 0.0264(10) Uani 1 1 d . . . C29 C 0.7283(5) 1.0227(3) -0.0680(3) 0.0322(11) Uani 1 1 d . . . H29 H 0.7398 1.0434 -0.0173 0.039 Uiso 1 1 calc R . . C30 C 0.7378(5) 1.0734(3) -0.1118(3) 0.0396(12) Uani 1 1 d . . . H30 H 0.7562 1.1281 -0.0904 0.048 Uiso 1 1 calc R . . C31 C 0.7211(5) 1.0453(3) -0.1847(3) 0.0487(14) Uani 1 1 d . . . H31 H 0.7259 1.0800 -0.2143 0.058 Uiso 1 1 calc R . . C32 C 0.6969(5) 0.9654(3) -0.2156(3) 0.0490(15) Uani 1 1 d . . . H32 H 0.6859 0.9453 -0.2664 0.059 Uiso 1 1 calc R . . C33 C 0.6889(5) 0.9151(3) -0.1720(2) 0.0375(12) Uani 1 1 d . . . H33 H 0.6740 0.8607 -0.1934 0.045 Uiso 1 1 calc R . . C34 C 0.7803(6) 0.6051(3) -0.0290(3) 0.0519(15) Uani 1 1 d . . . H34A H 0.8069 0.6178 0.0240 0.078 Uiso 1 1 calc R . . H34B H 0.8526 0.5844 -0.0496 0.078 Uiso 1 1 calc R . . H34C H 0.6850 0.5654 -0.0473 0.078 Uiso 1 1 calc R . . C35 C 0.6997(6) 0.6672(3) -0.1555(2) 0.0565(16) Uani 1 1 d . . . H35A H 0.6048 0.6273 -0.1685 0.085 Uiso 1 1 calc R . . H35B H 0.7663 0.6460 -0.1809 0.085 Uiso 1 1 calc R . . H35C H 0.6893 0.7138 -0.1697 0.085 Uiso 1 1 calc R . . C36 C 0.9598(5) 0.7612(3) -0.0371(3) 0.0478(14) Uani 1 1 d . . . H36A H 0.9593 0.8035 -0.0600 0.072 Uiso 1 1 calc R . . H36B H 1.0217 0.7313 -0.0570 0.072 Uiso 1 1 calc R . . H36C H 0.9975 0.7840 0.0154 0.072 Uiso 1 1 calc R . . C37 C 0.5781(4) 0.7819(2) 0.5403(2) 0.0217(10) Uani 1 1 d . . . C38 C 0.4603(4) 0.7400(2) 0.5625(2) 0.0222(10) Uani 1 1 d . . . C39 C 0.3820(5) 0.7803(2) 0.6016(2) 0.0276(11) Uani 1 1 d . . . H39 H 0.3047 0.7516 0.6179 0.033 Uiso 1 1 calc R . . C40 C 0.4134(5) 0.8616(2) 0.6177(2) 0.0266(10) Uani 1 1 d . . . C41 C 0.5264(4) 0.9017(2) 0.5926(2) 0.0229(10) Uani 1 1 d . . . H41 H 0.5469 0.9570 0.6015 0.028 Uiso 1 1 calc R . . C42 C 0.6099(4) 0.8645(2) 0.5552(2) 0.0218(10) Uani 1 1 d . . . C43 C 0.3294(5) 0.9044(2) 0.6624(2) 0.0362(12) Uani 1 1 d . . . H43A H 0.2687 0.9248 0.6315 0.054 Uiso 1 1 calc R . . H43B H 0.3971 0.9483 0.7019 0.054 Uiso 1 1 calc R . . H43C H 0.2679 0.8680 0.6827 0.054 Uiso 1 1 calc R . . C44 C 0.4183(5) 0.6498(2) 0.5409(2) 0.0263(10) Uani 1 1 d . . . H44 H 0.5112 0.6362 0.5479 0.032 Uiso 1 1 calc R . . C45 C 0.3472(5) 0.6159(2) 0.4599(2) 0.0272(11) Uani 1 1 d . . . C46 C 0.3922(5) 0.5591(3) 0.4160(2) 0.0366(12) Uani 1 1 d . . . H46 H 0.4666 0.5408 0.4368 0.044 Uiso 1 1 calc R . . C47 C 0.3291(6) 0.5289(3) 0.3422(3) 0.0479(15) Uani 1 1 d . . . H47 H 0.3606 0.4902 0.3127 0.058 Uiso 1 1 calc R . . C48 C 0.2211(6) 0.5550(3) 0.3118(3) 0.0511(15) Uani 1 1 d . . . H48 H 0.1788 0.5344 0.2613 0.061 Uiso 1 1 calc R . . C49 C 0.1738(6) 0.6106(3) 0.3537(3) 0.0447(13) Uani 1 1 d . . . H49 H 0.0983 0.6279 0.3326 0.054 Uiso 1 1 calc R . . C50 C 0.2374(5) 0.6411(3) 0.4270(2) 0.0359(12) Uani 1 1 d . . . H50 H 0.2056 0.6801 0.4558 0.043 Uiso 1 1 calc R . . C51 C 0.3307(5) 0.6138(2) 0.5895(2) 0.0291(11) Uani 1 1 d . . . C52 C 0.1822(5) 0.5799(3) 0.5705(2) 0.0329(11) Uani 1 1 d . . . H52 H 0.1299 0.5776 0.5243 0.039 Uiso 1 1 calc R . . C53 C 0.1081(5) 0.5492(3) 0.6172(3) 0.0364(12) Uani 1 1 d . . . H53 H 0.0061 0.5255 0.6024 0.044 Uiso 1 1 calc R . . C54 C 0.1799(6) 0.5524(3) 0.6842(3) 0.0473(14) Uani 1 1 d . . . H54 H 0.1291 0.5312 0.7163 0.057 Uiso 1 1 calc R . . C55 C 0.3278(6) 0.5871(4) 0.7044(3) 0.0685(19) Uani 1 1 d . . . H55 H 0.3789 0.5905 0.7513 0.082 Uiso 1 1 calc R . . C56 C 0.4027(6) 0.6170(3) 0.6580(3) 0.0550(15) Uani 1 1 d . . . H56 H 0.5048 0.6400 0.6729 0.066 Uiso 1 1 calc R . . C57 C 0.7306(4) 0.9093(2) 0.5259(2) 0.0222(10) Uani 1 1 d . . . H57 H 0.8108 0.8850 0.5315 0.027 Uiso 1 1 calc R . . C58 C 0.6799(4) 0.8975(2) 0.4451(2) 0.0231(10) Uani 1 1 d . . . C59 C 0.7681(5) 0.8837(3) 0.3976(2) 0.0328(11) Uani 1 1 d . . . H59 H 0.8633 0.8830 0.4160 0.039 Uiso 1 1 calc R . . C60 C 0.7197(5) 0.8707(3) 0.3234(2) 0.0399(13) Uani 1 1 d . . . H60 H 0.7814 0.8608 0.2916 0.048 Uiso 1 1 calc R . . C61 C 0.5817(5) 0.8724(3) 0.2960(2) 0.0353(12) Uani 1 1 d . . . H61 H 0.5486 0.8641 0.2455 0.042 Uiso 1 1 calc R . . C62 C 0.4933(5) 0.8861(2) 0.3425(2) 0.0332(11) Uani 1 1 d . . . H62 H 0.3987 0.8875 0.3241 0.040 Uiso 1 1 calc R . . C63 C 0.5412(5) 0.8981(2) 0.4166(2) 0.0281(10) Uani 1 1 d . . . H63 H 0.4783 0.9067 0.4480 0.034 Uiso 1 1 calc R . . C64 C 0.7941(4) 0.9962(2) 0.5694(2) 0.0255(10) Uani 1 1 d . . . C65 C 0.8699(5) 1.0148(3) 0.6421(2) 0.0333(11) Uani 1 1 d . . . H65 H 0.8834 0.9736 0.6616 0.040 Uiso 1 1 calc R . . C66 C 0.9244(5) 1.0911(3) 0.6850(3) 0.0409(13) Uani 1 1 d . . . H66 H 0.9760 1.1020 0.7336 0.049 Uiso 1 1 calc R . . C67 C 0.9052(5) 1.1522(3) 0.6585(3) 0.0431(14) Uani 1 1 d . . . H67 H 0.9414 1.2050 0.6887 0.052 Uiso 1 1 calc R . . C68 C 0.8329(5) 1.1353(3) 0.5877(3) 0.0415(13) Uani 1 1 d . . . H68 H 0.8203 1.1768 0.5685 0.050 Uiso 1 1 calc R . . C69 C 0.7777(5) 1.0576(2) 0.5435(2) 0.0301(11) Uani 1 1 d . . . H69 H 0.7279 1.0471 0.4947 0.036 Uiso 1 1 calc R . . C70 C 0.8257(6) 0.7669(4) 0.6491(3) 0.0608(16) Uani 1 1 d . . . H70A H 0.8445 0.8240 0.6603 0.091 Uiso 1 1 calc R . . H70B H 0.9054 0.7554 0.6773 0.091 Uiso 1 1 calc R . . H70C H 0.7348 0.7434 0.6615 0.091 Uiso 1 1 calc R . . C71 C 0.9824(5) 0.7739(4) 0.5290(3) 0.0656(17) Uani 1 1 d . . . H71A H 0.9739 0.7570 0.4765 0.098 Uiso 1 1 calc R . . H71B H 1.0621 0.7595 0.5538 0.098 Uiso 1 1 calc R . . H71C H 1.0018 0.8311 0.5453 0.098 Uiso 1 1 calc R . . C72 C 0.7943(6) 0.6186(3) 0.5320(3) 0.0622(17) Uani 1 1 d . . . H72A H 0.7138 0.5928 0.5508 0.093 Uiso 1 1 calc R . . H72B H 0.8844 0.6122 0.5560 0.093 Uiso 1 1 calc R . . H72C H 0.7755 0.5945 0.4796 0.093 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 Sn1 0.0393(2) 0.03107(19) 0.02647(19) 0.00515(14) 0.00411(15) 0.01049(15) Cl1 0.0557(9) 0.0492(8) 0.0441(8) 0.0021(6) -0.0145(7) 0.0245(7) Si1 0.0273(7) 0.0377(7) 0.0322(7) 0.0002(6) 0.0019(6) 0.0149(6) N1 0.025(2) 0.0242(19) 0.0259(19) 0.0066(16) 0.0015(16) 0.0095(16) C1 0.025(2) 0.027(2) 0.014(2) 0.0036(18) 0.0039(18) 0.0103(19) Sn2 0.0498(2) 0.03204(19) 0.02592(19) 0.00491(15) 0.01071(16) 0.01006(16) Cl2 0.1224(16) 0.1031(13) 0.0666(11) 0.0172(10) 0.0543(11) 0.0747(12) Si2 0.0307(8) 0.0429(8) 0.0479(9) 0.0208(7) 0.0116(7) 0.0174(6) N2 0.026(2) 0.0272(19) 0.0227(19) 0.0073(16) 0.0101(16) 0.0107(16) C2 0.025(2) 0.024(2) 0.017(2) 0.0040(18) 0.0060(19) 0.0058(19) C3 0.021(2) 0.030(2) 0.021(2) 0.005(2) 0.0025(19) 0.005(2) C4 0.025(3) 0.038(3) 0.031(3) 0.015(2) 0.008(2) 0.013(2) C5 0.028(3) 0.029(2) 0.036(3) 0.015(2) 0.010(2) 0.012(2) C6 0.021(2) 0.029(2) 0.019(2) 0.0049(19) 0.0072(19) 0.0073(19) C7 0.031(3) 0.047(3) 0.059(3) 0.030(3) -0.003(3) 0.006(2) C8 0.022(2) 0.026(2) 0.026(2) 0.0064(19) 0.0029(19) 0.0081(19) C9 0.024(2) 0.018(2) 0.028(2) 0.0051(19) -0.003(2) 0.0037(19) C10 0.037(3) 0.024(2) 0.040(3) 0.009(2) 0.002(2) 0.005(2) C11 0.053(3) 0.039(3) 0.032(3) 0.013(2) -0.003(3) 0.009(3) C12 0.044(3) 0.036(3) 0.027(3) 0.005(2) 0.002(2) -0.004(3) C13 0.039(3) 0.028(2) 0.031(3) 0.005(2) 0.010(2) 0.005(2) C14 0.032(3) 0.026(2) 0.028(3) 0.008(2) -0.002(2) 0.007(2) C15 0.028(3) 0.023(2) 0.025(2) 0.0098(19) 0.003(2) 0.009(2) C16 0.028(3) 0.023(2) 0.027(2) 0.0013(19) 0.003(2) 0.005(2) C17 0.030(3) 0.032(3) 0.035(3) 0.009(2) 0.004(2) 0.006(2) C18 0.037(3) 0.031(3) 0.029(3) 0.005(2) -0.005(2) 0.003(2) C19 0.050(3) 0.031(3) 0.025(3) 0.003(2) 0.010(2) 0.011(2) C20 0.035(3) 0.030(2) 0.030(3) 0.008(2) 0.011(2) 0.010(2) C21 0.020(2) 0.032(2) 0.024(2) 0.008(2) 0.0076(19) 0.010(2) C22 0.024(3) 0.020(2) 0.029(2) 0.0080(19) 0.007(2) 0.0042(19) C23 0.027(3) 0.032(2) 0.033(3) 0.008(2) 0.006(2) 0.011(2) C24 0.031(3) 0.035(3) 0.036(3) 0.004(2) -0.003(2) 0.007(2) C25 0.043(3) 0.030(3) 0.029(3) 0.001(2) 0.004(2) 0.009(2) C26 0.037(3) 0.027(2) 0.034(3) 0.008(2) 0.015(2) 0.013(2) C27 0.028(3) 0.032(3) 0.034(3) 0.010(2) 0.004(2) 0.009(2) C28 0.015(2) 0.036(3) 0.028(3) 0.014(2) 0.0056(19) 0.003(2) C29 0.023(3) 0.038(3) 0.037(3) 0.013(2) 0.003(2) 0.011(2) C30 0.030(3) 0.041(3) 0.050(3) 0.024(3) 0.003(2) 0.007(2) C31 0.029(3) 0.064(4) 0.066(4) 0.046(3) 0.011(3) 0.012(3) C32 0.027(3) 0.082(4) 0.031(3) 0.021(3) 0.006(2) 0.000(3) C33 0.028(3) 0.046(3) 0.036(3) 0.014(2) 0.007(2) 0.005(2) C34 0.048(3) 0.038(3) 0.065(4) 0.001(3) 0.004(3) 0.024(3) C35 0.050(4) 0.085(4) 0.032(3) -0.001(3) 0.010(3) 0.033(3) C36 0.027(3) 0.058(3) 0.052(3) 0.005(3) 0.012(2) 0.011(3) C37 0.020(2) 0.028(2) 0.016(2) 0.0036(18) -0.0001(18) 0.0091(19) C38 0.025(2) 0.021(2) 0.018(2) 0.0041(18) -0.0004(19) 0.0062(19) C39 0.026(3) 0.031(3) 0.026(2) 0.011(2) 0.009(2) 0.005(2) C40 0.025(3) 0.028(2) 0.026(2) 0.003(2) 0.008(2) 0.010(2) C41 0.023(2) 0.021(2) 0.021(2) 0.0021(18) 0.0016(19) 0.0055(19) C42 0.020(2) 0.027(2) 0.016(2) 0.0021(18) 0.0041(18) 0.0067(19) C43 0.035(3) 0.027(2) 0.045(3) 0.002(2) 0.022(2) 0.008(2) C44 0.026(2) 0.025(2) 0.029(2) 0.008(2) 0.009(2) 0.009(2) C45 0.029(3) 0.025(2) 0.025(2) 0.009(2) 0.008(2) 0.002(2) C46 0.048(3) 0.028(3) 0.035(3) 0.009(2) 0.016(2) 0.011(2) C47 0.068(4) 0.029(3) 0.039(3) 0.001(2) 0.022(3) 0.001(3) C48 0.065(4) 0.042(3) 0.030(3) 0.008(3) 0.005(3) -0.006(3) C49 0.046(3) 0.041(3) 0.037(3) 0.013(3) 0.001(3) -0.001(3) C50 0.038(3) 0.030(3) 0.033(3) 0.008(2) 0.007(2) -0.001(2) C51 0.031(3) 0.025(2) 0.029(3) 0.007(2) 0.006(2) 0.006(2) C52 0.030(3) 0.039(3) 0.028(3) 0.014(2) 0.004(2) 0.006(2) C53 0.029(3) 0.031(3) 0.043(3) 0.014(2) 0.003(2) -0.001(2) C54 0.046(3) 0.060(3) 0.042(3) 0.029(3) 0.014(3) 0.010(3) C55 0.048(4) 0.109(5) 0.046(3) 0.048(4) 0.002(3) -0.001(4) C56 0.037(3) 0.084(4) 0.045(3) 0.040(3) 0.006(3) 0.003(3) C57 0.019(2) 0.022(2) 0.023(2) 0.0039(19) 0.0041(19) 0.0051(18) C58 0.024(2) 0.016(2) 0.027(2) 0.0039(18) 0.008(2) 0.0031(18) C59 0.025(3) 0.038(3) 0.034(3) 0.006(2) 0.013(2) 0.008(2) C60 0.037(3) 0.050(3) 0.031(3) 0.008(2) 0.017(2) 0.009(2) C61 0.045(3) 0.033(3) 0.022(2) 0.005(2) 0.007(2) 0.004(2) C62 0.033(3) 0.029(2) 0.035(3) 0.011(2) 0.000(2) 0.008(2) C63 0.031(3) 0.030(2) 0.027(3) 0.009(2) 0.013(2) 0.011(2) C64 0.020(2) 0.027(2) 0.029(3) 0.006(2) 0.010(2) 0.0055(19) C65 0.029(3) 0.037(3) 0.030(3) 0.008(2) 0.009(2) 0.002(2) C66 0.030(3) 0.044(3) 0.035(3) -0.003(3) 0.009(2) -0.001(2) C67 0.031(3) 0.035(3) 0.049(3) -0.006(3) 0.017(3) -0.004(2) C68 0.035(3) 0.031(3) 0.064(4) 0.013(3) 0.024(3) 0.010(2) C69 0.028(3) 0.027(2) 0.033(3) 0.004(2) 0.012(2) 0.005(2) C70 0.055(4) 0.090(4) 0.042(3) 0.025(3) 0.003(3) 0.030(3) C71 0.031(3) 0.080(4) 0.095(5) 0.040(4) 0.014(3) 0.019(3) C72 0.056(4) 0.056(4) 0.095(5) 0.041(3) 0.020(3) 0.033(3) _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 Sn1 N1 2.076(3) . ? Sn1 Cl1 2.4412(15) . ? Si1 N1 1.755(4) . ? Si1 C36 1.847(5) . ? Si1 C34 1.853(5) . ? Si1 C35 1.869(5) . ? N1 C1 1.437(5) . ? C1 C2 1.398(6) . ? C1 C6 1.416(6) . ? Sn2 N2 2.079(3) . ? Sn2 Cl2 2.4253(17) . ? Si2 N2 1.744(4) . ? Si2 C71 1.848(6) . ? Si2 C72 1.858(5) . ? Si2 C70 1.866(5) . ? N2 C37 1.435(5) . ? C2 C3 1.389(6) . ? C2 C8 1.533(6) . ? C3 C4 1.378(6) . ? C4 C5 1.395(6) . ? C4 C7 1.511(6) . ? C5 C6 1.388(6) . ? C6 C21 1.534(6) . ? C8 C9 1.525(6) . ? C8 C15 1.530(6) . ? C9 C10 1.390(6) . ? C9 C14 1.393(6) . ? C10 C11 1.383(6) . ? C11 C12 1.374(7) . ? C12 C13 1.376(6) . ? C13 C14 1.391(6) . ? C15 C16 1.385(6) . ? C15 C20 1.397(6) . ? C16 C17 1.394(6) . ? C17 C18 1.389(6) . ? C18 C19 1.356(6) . ? C19 C20 1.390(6) . ? C21 C28 1.525(6) . ? C21 C22 1.527(5) . ? C22 C23 1.392(6) . ? C22 C27 1.392(6) . ? C23 C24 1.401(6) . ? C24 C25 1.371(6) . ? C25 C26 1.389(6) . ? C26 C27 1.381(6) . ? C28 C29 1.386(6) . ? C28 C33 1.393(6) . ? C29 C30 1.395(6) . ? C30 C31 1.361(7) . ? C31 C32 1.390(7) . ? C32 C33 1.387(7) . ? C37 C38 1.405(6) . ? C37 C42 1.415(5) . ? C38 C39 1.386(6) . ? C38 C44 1.536(5) . ? C39 C40 1.391(6) . ? C40 C41 1.389(6) . ? C40 C43 1.509(6) . ? C41 C42 1.378(6) . ? C42 C57 1.529(6) . ? C44 C51 1.526(6) . ? C44 C45 1.529(6) . ? C45 C46 1.394(6) . ? C45 C50 1.398(6) . ? C46 C47 1.391(7) . ? C47 C48 1.376(7) . ? C48 C49 1.373(7) . ? C49 C50 1.383(6) . ? C51 C52 1.382(6) . ? C51 C56 1.390(6) . ? C52 C53 1.381(6) . ? C53 C54 1.364(6) . ? C54 C55 1.378(7) . ? C55 C56 1.375(7) . ? C57 C58 1.521(6) . ? C57 C64 1.532(5) . ? C58 C59 1.384(6) . ? C58 C63 1.389(6) . ? C59 C60 1.392(6) . ? C60 C61 1.385(7) . ? C61 C62 1.373(6) . ? C62 C63 1.391(6) . ? C64 C69 1.370(6) . ? C64 C65 1.409(6) . ? C65 C66 1.370(6) . ? C66 C67 1.380(7) . ? C67 C68 1.373(7) . ? C68 C69 1.398(6) . ? 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 Sn1 Cl1 96.49(10) . . ? N1 Si1 C36 112.1(2) . . ? N1 Si1 C34 111.4(2) . . ? C36 Si1 C34 108.9(2) . . ? N1 Si1 C35 108.9(2) . . ? C36 Si1 C35 106.6(3) . . ? C34 Si1 C35 108.7(3) . . ? C1 N1 Si1 119.2(3) . . ? C1 N1 Sn1 111.4(3) . . ? Si1 N1 Sn1 129.42(19) . . ? C2 C1 C6 118.7(4) . . ? C2 C1 N1 121.5(4) . . ? C6 C1 N1 119.8(4) . . ? N2 Sn2 Cl2 95.41(11) . . ? N2 Si2 C71 111.4(2) . . ? N2 Si2 C72 112.4(2) . . ? C71 Si2 C72 107.8(3) . . ? N2 Si2 C70 108.7(2) . . ? C71 Si2 C70 107.8(3) . . ? C72 Si2 C70 108.6(3) . . ? C37 N2 Si2 118.8(3) . . ? C37 N2 Sn2 109.7(2) . . ? Si2 N2 Sn2 131.51(19) . . ? C3 C2 C1 120.3(4) . . ? C3 C2 C8 121.3(4) . . ? C1 C2 C8 118.3(4) . . ? C4 C3 C2 121.7(4) . . ? C3 C4 C5 117.7(4) . . ? C3 C4 C7 121.5(4) . . ? C5 C4 C7 120.7(4) . . ? C6 C5 C4 122.4(4) . . ? C5 C6 C1 118.9(4) . . ? C5 C6 C21 121.7(4) . . ? C1 C6 C21 119.4(4) . . ? C9 C8 C15 111.6(3) . . ? C9 C8 C2 110.5(3) . . ? C15 C8 C2 114.1(3) . . ? C10 C9 C14 117.4(4) . . ? C10 C9 C8 120.5(4) . . ? C14 C9 C8 122.1(4) . . ? C11 C10 C9 121.9(5) . . ? C12 C11 C10 118.9(5) . . ? C11 C12 C13 121.3(5) . . ? C12 C13 C14 118.9(5) . . ? C13 C14 C9 121.4(4) . . ? C16 C15 C20 118.2(4) . . ? C16 C15 C8 123.4(4) . . ? C20 C15 C8 118.4(4) . . ? C15 C16 C17 121.4(4) . . ? C18 C17 C16 119.0(4) . . ? C19 C18 C17 120.4(4) . . ? C18 C19 C20 120.8(4) . . ? C19 C20 C15 120.2(4) . . ? C28 C21 C22 112.6(3) . . ? C28 C21 C6 113.9(3) . . ? C22 C21 C6 111.2(3) . . ? C23 C22 C27 118.4(4) . . ? C23 C22 C21 120.3(4) . . ? C27 C22 C21 121.3(4) . . ? C22 C23 C24 120.7(4) . . ? C25 C24 C23 119.7(4) . . ? C24 C25 C26 120.3(4) . . ? C27 C26 C25 119.9(4) . . ? C26 C27 C22 121.0(4) . . ? C29 C28 C33 117.6(4) . . ? C29 C28 C21 123.2(4) . . ? C33 C28 C21 119.1(4) . . ? C28 C29 C30 120.9(4) . . ? C31 C30 C29 120.8(5) . . ? C30 C31 C32 119.4(5) . . ? C33 C32 C31 119.9(5) . . ? C32 C33 C28 121.3(5) . . ? C38 C37 C42 119.0(4) . . ? C38 C37 N2 121.0(4) . . ? C42 C37 N2 120.0(4) . . ? C39 C38 C37 119.8(4) . . ? C39 C38 C44 121.3(4) . . ? C37 C38 C44 118.9(4) . . ? C38 C39 C40 121.8(4) . . ? C41 C40 C39 117.5(4) . . ? C41 C40 C43 121.6(4) . . ? C39 C40 C43 120.8(4) . . ? C42 C41 C40 122.8(4) . . ? C41 C42 C37 119.0(4) . . ? C41 C42 C57 121.9(4) . . ? C37 C42 C57 119.0(4) . . ? C51 C44 C45 114.0(3) . . ? C51 C44 C38 113.2(3) . . ? C45 C44 C38 110.1(3) . . ? C46 C45 C50 117.7(4) . . ? C46 C45 C44 120.4(4) . . ? C50 C45 C44 121.9(4) . . ? C47 C46 C45 120.6(5) . . ? C48 C47 C46 120.0(5) . . ? C49 C48 C47 120.8(5) . . ? C48 C49 C50 119.3(5) . . ? C49 C50 C45 121.7(5) . . ? C52 C51 C56 117.4(4) . . ? C52 C51 C44 124.0(4) . . ? C56 C51 C44 118.6(4) . . ? C53 C52 C51 121.5(4) . . ? C54 C53 C52 120.6(5) . . ? C53 C54 C55 118.6(5) . . ? C56 C55 C54 121.2(5) . . ? C55 C56 C51 120.7(5) . . ? C58 C57 C42 110.6(3) . . ? C58 C57 C64 112.9(3) . . ? C42 C57 C64 112.7(3) . . ? C59 C58 C63 118.1(4) . . ? C59 C58 C57 121.3(4) . . ? C63 C58 C57 120.6(4) . . ? C58 C59 C60 121.1(4) . . ? C61 C60 C59 120.0(4) . . ? C62 C61 C60 119.3(4) . . ? C61 C62 C63 120.5(4) . . ? C58 C63 C62 120.9(4) . . ? C69 C64 C65 117.2(4) . . ? C69 C64 C57 124.4(4) . . ? C65 C64 C57 118.3(4) . . ? C66 C65 C64 121.4(5) . . ? C65 C66 C67 120.7(5) . . ? C68 C67 C66 118.6(4) . . ? C67 C68 C69 120.8(5) . . ? C64 C69 C68 121.1(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.082 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.093 # Attachment '- compound9.CIF' data_compound9 _database_code_depnum_ccdc_archive 'CCDC 822606' #TrackingRef '- compound9.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H57 Cl N O1.50 Si Sn' _chemical_formula_weight 962.27 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' Sn Sn -0.6537 1.4246 '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' _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 13.4198(3) _cell_length_b 14.0960(3) _cell_length_c 14.4193(3) _cell_angle_alpha 66.512(2) _cell_angle_beta 81.228(2) _cell_angle_gamma 86.827(2) _cell_volume 2472.33(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 998 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.851 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _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 16094 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9670 _reflns_number_gt 8515 _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. One full molecule of diethyl ether of crystallisation was located and its C and O atoms refined anisotropically without restraints. Another molecule of diethyl ether with its atomic sites set at 50% occupancy was refined with isotropic thermal parameters for its C and O atoms The DFIX and DANG commands of SHELX-L were used to constrain the geometry of this molecule. The largest peak in the final difference map of the refinement (1.96 ang./A3) is located close to Sn(1). ; _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^)+(0.0565P)^2^+2.6405P] 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 9670 _refine_ls_number_parameters 567 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.080 _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 Sn1 Sn 0.704160(16) 0.838790(17) 0.725540(17) 0.01995(9) Uani 1 1 d . . . Cl1 Cl 0.77457(7) 0.71025(7) 0.65998(7) 0.0273(2) Uani 1 1 d . . . Si1 Si 0.86314(6) 0.69412(7) 0.90615(7) 0.01544(19) Uani 1 1 d . . . O1 O 1.4323(2) 0.7004(3) 0.5914(3) 0.0479(8) Uani 1 1 d . . . O2 O 0.8469(5) 1.4537(5) 0.4998(6) 0.068(2) Uiso 0.50 1 d PD . . N1 N 0.78967(18) 0.80106(19) 0.8470(2) 0.0140(5) Uani 1 1 d . . . C1 C 0.7860(2) 0.8848(2) 0.8814(2) 0.0141(6) Uani 1 1 d . . . C2 C 0.8551(2) 0.9676(2) 0.8328(2) 0.0163(6) Uani 1 1 d . . . C3 C 0.8545(2) 1.0449(2) 0.8704(2) 0.0168(6) Uani 1 1 d . . . H3 H 0.9030 1.0992 0.8390 0.020 Uiso 1 1 calc R . . C4 C 0.7850(2) 1.0447(2) 0.9524(2) 0.0171(6) Uani 1 1 d . . . C5 C 0.7134(2) 0.9659(2) 0.9954(2) 0.0167(6) Uani 1 1 d . . . H5 H 0.6639 0.9659 1.0501 0.020 Uiso 1 1 calc R . . C6 C 0.7121(2) 0.8869(2) 0.9607(2) 0.0156(6) Uani 1 1 d . . . C7 C 0.7862(3) 1.1310(3) 0.9891(3) 0.0249(8) Uani 1 1 d . . . H7A H 0.7271 1.1245 1.0405 0.037 Uiso 1 1 calc R . . H7B H 0.7845 1.1978 0.9313 0.037 Uiso 1 1 calc R . . H7C H 0.8477 1.1267 1.0195 0.037 Uiso 1 1 calc R . . C8 C 0.9218(2) 0.9768(2) 0.7338(2) 0.0162(6) Uani 1 1 d . . . H8 H 0.9443 0.9052 0.7429 0.019 Uiso 1 1 calc R . . C9 C 1.0170(2) 1.0415(3) 0.7093(2) 0.0176(7) Uani 1 1 d . . . C10 C 1.0957(3) 0.9982(3) 0.7651(3) 0.0253(8) Uani 1 1 d . . . H10 H 1.0885 0.9304 0.8173 0.030 Uiso 1 1 calc R . . C11 C 1.1851(3) 1.0532(3) 0.7452(3) 0.0314(9) Uani 1 1 d . . . H11 H 1.2378 1.0234 0.7848 0.038 Uiso 1 1 calc R . . C12 C 1.1973(3) 1.1505(3) 0.6687(3) 0.0330(9) Uani 1 1 d . . . H12 H 1.2588 1.1872 0.6545 0.040 Uiso 1 1 calc R . . C13 C 1.1204(3) 1.1944(3) 0.6130(3) 0.0316(9) Uani 1 1 d . . . H13 H 1.1289 1.2618 0.5603 0.038 Uiso 1 1 calc R . . C14 C 1.0293(3) 1.1407(3) 0.6330(3) 0.0248(8) Uani 1 1 d . . . H14 H 0.9762 1.1719 0.5944 0.030 Uiso 1 1 calc R . . C15 C 0.8579(2) 1.0136(2) 0.6475(2) 0.0168(6) Uani 1 1 d . . . C16 C 0.8723(2) 0.9730(3) 0.5727(3) 0.0213(7) Uani 1 1 d . . . H16 H 0.9245 0.9243 0.5742 0.026 Uiso 1 1 calc R . . C17 C 0.8116(3) 1.0022(3) 0.4961(3) 0.0254(8) Uani 1 1 d . . . H17 H 0.8222 0.9733 0.4460 0.030 Uiso 1 1 calc R . . C18 C 0.7360(3) 1.0731(3) 0.4926(3) 0.0278(8) Uani 1 1 d . . . H18 H 0.6936 1.0922 0.4410 0.033 Uiso 1 1 calc R . . C19 C 0.7215(3) 1.1168(3) 0.5646(3) 0.0275(8) Uani 1 1 d . . . H19 H 0.6704 1.1671 0.5612 0.033 Uiso 1 1 calc R . . C20 C 0.7818(3) 1.0871(3) 0.6413(3) 0.0230(7) Uani 1 1 d . . . H20 H 0.7713 1.1170 0.6905 0.028 Uiso 1 1 calc R . . C21 C 0.6255(2) 0.8083(2) 1.0004(2) 0.0171(6) Uani 1 1 d . . . H21 H 0.6564 0.7416 1.0019 0.021 Uiso 1 1 calc R . . C22 C 0.5748(2) 0.7857(2) 1.1095(3) 0.0178(7) Uani 1 1 d . . . C23 C 0.4717(3) 0.7992(3) 1.1325(3) 0.0243(7) Uani 1 1 d . . . H23 H 0.4316 0.8285 1.0790 0.029 Uiso 1 1 calc R . . C24 C 0.4273(3) 0.7696(3) 1.2341(3) 0.0322(9) Uani 1 1 d . . . H24 H 0.3569 0.7786 1.2492 0.039 Uiso 1 1 calc R . . C25 C 0.4837(3) 0.7278(3) 1.3118(3) 0.0318(9) Uani 1 1 d . . . H25 H 0.4526 0.7079 1.3806 0.038 Uiso 1 1 calc R . . C26 C 0.5863(3) 0.7143(3) 1.2905(3) 0.0279(8) Uani 1 1 d . . . H26 H 0.6259 0.6849 1.3444 0.033 Uiso 1 1 calc R . . C27 C 0.6312(3) 0.7444(3) 1.1890(3) 0.0228(7) Uani 1 1 d . . . H27 H 0.7018 0.7363 1.1744 0.027 Uiso 1 1 calc R . . C28 C 0.5521(2) 0.8374(3) 0.9235(3) 0.0183(7) Uani 1 1 d . . . C29 C 0.5303(2) 0.9407(3) 0.8666(3) 0.0205(7) Uani 1 1 d . . . H29 H 0.5603 0.9938 0.8781 0.025 Uiso 1 1 calc R . . C30 C 0.4654(3) 0.9675(3) 0.7934(3) 0.0278(8) Uani 1 1 d . . . H30 H 0.4505 1.0382 0.7566 0.033 Uiso 1 1 calc R . . C31 C 0.4225(3) 0.8910(3) 0.7744(3) 0.0300(8) Uani 1 1 d . . . H31 H 0.3799 0.9089 0.7231 0.036 Uiso 1 1 calc R . . C32 C 0.4424(3) 0.7883(3) 0.8309(3) 0.0293(8) Uani 1 1 d . . . H32 H 0.4124 0.7357 0.8187 0.035 Uiso 1 1 calc R . . C33 C 0.5057(2) 0.7610(3) 0.9053(3) 0.0247(8) Uani 1 1 d . . . H33 H 0.5176 0.6901 0.9441 0.030 Uiso 1 1 calc R . . C34 C 0.9979(2) 0.7061(2) 0.8427(3) 0.0183(7) Uani 1 1 d . . . C35 C 1.0787(2) 0.6930(3) 0.8970(3) 0.0228(7) Uani 1 1 d . . . H35 H 1.0653 0.6786 0.9679 0.027 Uiso 1 1 calc R . . C36 C 1.1780(3) 0.7004(3) 0.8506(3) 0.0281(8) Uani 1 1 d . . . H36 H 1.2313 0.6914 0.8897 0.034 Uiso 1 1 calc R . . C37 C 1.1993(3) 0.7208(3) 0.7480(3) 0.0287(8) Uani 1 1 d . . . H37 H 1.2672 0.7260 0.7159 0.034 Uiso 1 1 calc R . . C38 C 1.1204(3) 0.7337(3) 0.6918(3) 0.0276(8) Uani 1 1 d . . . H38 H 1.1345 0.7480 0.6209 0.033 Uiso 1 1 calc R . . C39 C 1.0215(3) 0.7258(3) 0.7386(3) 0.0245(7) Uani 1 1 d . . . H39 H 0.9685 0.7340 0.6994 0.029 Uiso 1 1 calc R . . C40 C 0.8057(2) 0.5771(2) 0.9037(3) 0.0178(7) Uani 1 1 d . . . C41 C 0.8604(3) 0.5107(3) 0.8648(3) 0.0221(7) Uani 1 1 d . . . H41 H 0.9309 0.5210 0.8437 0.027 Uiso 1 1 calc R . . C42 C 0.8133(3) 0.4294(3) 0.8566(3) 0.0309(9) Uani 1 1 d . . . H42 H 0.8518 0.3851 0.8296 0.037 Uiso 1 1 calc R . . C43 C 0.7114(3) 0.4128(3) 0.8871(3) 0.0352(9) Uani 1 1 d . . . H43 H 0.6791 0.3585 0.8796 0.042 Uiso 1 1 calc R . . C44 C 0.6564(3) 0.4751(3) 0.9285(4) 0.0374(10) Uani 1 1 d . . . H44 H 0.5861 0.4632 0.9507 0.045 Uiso 1 1 calc R . . C45 C 0.7033(3) 0.5555(3) 0.9379(3) 0.0292(8) Uani 1 1 d . . . H45 H 0.6647 0.5968 0.9684 0.035 Uiso 1 1 calc R . . C46 C 0.8691(2) 0.6747(3) 1.0421(3) 0.0183(7) Uani 1 1 d . . . C47 C 0.8426(3) 0.5794(3) 1.1222(3) 0.0250(7) Uani 1 1 d . . . H47 H 0.8161 0.5263 1.1079 0.030 Uiso 1 1 calc R . . C48 C 0.8543(3) 0.5606(3) 1.2226(3) 0.0325(9) Uani 1 1 d . . . H48 H 0.8369 0.4949 1.2757 0.039 Uiso 1 1 calc R . . C49 C 0.8910(3) 0.6376(3) 1.2445(3) 0.0315(8) Uani 1 1 d . . . H49 H 0.8977 0.6254 1.3130 0.038 Uiso 1 1 calc R . . C50 C 0.9181(3) 0.7328(3) 1.1667(3) 0.0245(7) Uani 1 1 d . . . H50 H 0.9439 0.7856 1.1819 0.029 Uiso 1 1 calc R . . C51 C 0.9076(2) 0.7510(3) 1.0670(3) 0.0215(7) Uani 1 1 d . . . H51 H 0.9267 0.8165 1.0142 0.026 Uiso 1 1 calc R . . C52 C 1.4403(5) 0.5413(4) 0.7457(4) 0.0621(15) Uani 1 1 d . . . H52A H 1.5105 0.5549 0.7482 0.093 Uiso 1 1 calc R . . H52B H 1.4292 0.4664 0.7715 0.093 Uiso 1 1 calc R . . H52C H 1.3951 0.5698 0.7881 0.093 Uiso 1 1 calc R . . C53 C 1.4190(4) 0.5914(4) 0.6370(4) 0.0583(14) Uani 1 1 d . . . H53A H 1.4640 0.5606 0.5953 0.070 Uiso 1 1 calc R . . H53B H 1.3487 0.5751 0.6352 0.070 Uiso 1 1 calc R . . C54 C 1.5350(3) 0.7321(4) 0.5706(4) 0.0462(12) Uani 1 1 d . . . H54A H 1.5749 0.6969 0.5301 0.055 Uiso 1 1 calc R . . H54B H 1.5627 0.7123 0.6356 0.055 Uiso 1 1 calc R . . C55 C 1.5431(3) 0.8454(4) 0.5133(4) 0.0474(12) Uani 1 1 d . . . H55A H 1.5118 0.8653 0.4512 0.071 Uiso 1 1 calc R . . H55B H 1.6144 0.8659 0.4948 0.071 Uiso 1 1 calc R . . H55C H 1.5086 0.8801 0.5560 0.071 Uiso 1 1 calc R . . C56 C 0.6907(7) 1.5164(9) 0.5603(10) 0.079(4) Uiso 0.50 1 d PD . . H56A H 0.7268 1.5789 0.5507 0.119 Uiso 0.50 1 calc PR . . H56B H 0.6378 1.4996 0.6194 0.119 Uiso 0.50 1 calc PR . . H56C H 0.6602 1.5282 0.4991 0.119 Uiso 0.50 1 calc PR . . C57 C 0.7643(6) 1.4268(7) 0.5785(7) 0.068(3) Uiso 0.50 1 d PD . . H57A H 0.7884 1.4088 0.6450 0.082 Uiso 0.50 1 calc PR . . H57B H 0.7295 1.3655 0.5811 0.082 Uiso 0.50 1 calc PR . . C58 C 0.9221(7) 1.3800(7) 0.5049(9) 0.081(4) Uiso 0.50 1 d PD . . H58A H 0.8939 1.3204 0.4975 0.097 Uiso 0.50 1 calc PR . . H58B H 0.9451 1.3546 0.5728 0.097 Uiso 0.50 1 calc PR . . C59 C 1.0108(7) 1.4238(10) 0.4229(9) 0.083(4) Uiso 0.50 1 d PD . . H59A H 1.0624 1.4473 0.4505 0.125 Uiso 0.50 1 calc PR . . H59B H 0.9887 1.4824 0.3654 0.125 Uiso 0.50 1 calc PR . . H59C H 1.0392 1.3703 0.3995 0.125 Uiso 0.50 1 calc PR . . 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 Sn1 0.01856(13) 0.02448(15) 0.01758(14) -0.00924(11) -0.00027(10) -0.00524(9) Cl1 0.0343(5) 0.0286(5) 0.0229(5) -0.0137(4) -0.0051(4) -0.0019(4) Si1 0.0160(4) 0.0147(4) 0.0150(4) -0.0062(4) 0.0020(3) -0.0050(3) O1 0.0310(15) 0.063(2) 0.047(2) -0.0171(17) -0.0048(14) -0.0154(14) N1 0.0141(12) 0.0149(13) 0.0132(13) -0.0061(11) 0.0004(10) -0.0034(10) C1 0.0158(14) 0.0154(15) 0.0121(15) -0.0059(13) -0.0032(12) -0.0013(12) C2 0.0158(14) 0.0179(16) 0.0132(16) -0.0042(13) 0.0002(12) -0.0040(12) C3 0.0189(15) 0.0149(15) 0.0146(16) -0.0036(13) -0.0004(13) -0.0066(12) C4 0.0226(15) 0.0148(15) 0.0136(16) -0.0044(13) -0.0045(13) -0.0022(12) C5 0.0170(14) 0.0206(16) 0.0127(16) -0.0085(13) 0.0029(12) -0.0013(12) C6 0.0157(14) 0.0151(15) 0.0130(16) -0.0032(13) 0.0012(12) -0.0039(12) C7 0.0305(18) 0.0218(18) 0.0246(19) -0.0129(16) 0.0027(15) -0.0079(14) C8 0.0186(15) 0.0149(15) 0.0129(16) -0.0043(13) 0.0030(13) -0.0060(12) C9 0.0195(15) 0.0212(17) 0.0128(16) -0.0095(14) 0.0062(13) -0.0072(13) C10 0.0217(16) 0.0279(19) 0.0247(19) -0.0094(16) 0.0007(15) -0.0055(14) C11 0.0233(18) 0.045(2) 0.032(2) -0.0220(19) -0.0011(16) -0.0057(17) C12 0.0276(19) 0.049(2) 0.033(2) -0.030(2) 0.0094(17) -0.0197(17) C13 0.043(2) 0.029(2) 0.0219(19) -0.0122(17) 0.0109(17) -0.0202(17) C14 0.0290(18) 0.0255(18) 0.0192(18) -0.0087(15) 0.0018(15) -0.0091(15) C15 0.0174(15) 0.0170(16) 0.0141(16) -0.0049(13) 0.0035(12) -0.0084(12) C16 0.0217(16) 0.0215(17) 0.0177(17) -0.0072(14) 0.0078(13) -0.0089(13) C17 0.0297(18) 0.033(2) 0.0127(17) -0.0097(15) 0.0054(14) -0.0134(15) C18 0.0310(19) 0.031(2) 0.0162(18) -0.0033(15) -0.0045(15) -0.0072(16) C19 0.0280(18) 0.0283(19) 0.0227(19) -0.0065(16) -0.0021(15) -0.0031(15) C20 0.0276(17) 0.0205(17) 0.0219(19) -0.0101(15) -0.0014(15) -0.0011(14) C21 0.0168(15) 0.0168(16) 0.0164(17) -0.0072(13) 0.0054(13) -0.0056(12) C22 0.0207(15) 0.0143(15) 0.0165(17) -0.0064(13) 0.0069(13) -0.0078(12) C23 0.0223(16) 0.0274(19) 0.0239(19) -0.0132(16) 0.0061(14) -0.0055(14) C24 0.0242(18) 0.039(2) 0.033(2) -0.0171(19) 0.0110(16) -0.0071(16) C25 0.038(2) 0.034(2) 0.022(2) -0.0141(17) 0.0142(17) -0.0152(17) C26 0.0345(19) 0.0282(19) 0.0217(19) -0.0115(16) 0.0025(16) -0.0112(16) C27 0.0219(16) 0.0246(18) 0.0209(18) -0.0088(15) 0.0024(14) -0.0063(14) C28 0.0142(14) 0.0219(17) 0.0189(17) -0.0097(14) 0.0042(13) -0.0045(12) C29 0.0194(15) 0.0215(17) 0.0197(18) -0.0079(14) 0.0002(13) -0.0019(13) C30 0.0237(17) 0.035(2) 0.024(2) -0.0121(17) -0.0011(15) 0.0034(15) C31 0.0209(17) 0.051(2) 0.024(2) -0.0213(19) -0.0014(15) -0.0006(16) C32 0.0191(16) 0.041(2) 0.037(2) -0.0256(19) -0.0010(16) -0.0061(16) C33 0.0200(16) 0.0236(18) 0.032(2) -0.0137(16) 0.0014(15) -0.0043(14) C34 0.0167(15) 0.0137(15) 0.0224(18) -0.0065(13) 0.0025(13) -0.0031(12) C35 0.0215(16) 0.0201(17) 0.0239(19) -0.0061(15) -0.0016(14) -0.0007(13) C36 0.0194(16) 0.0249(19) 0.037(2) -0.0083(17) -0.0057(16) -0.0004(14) C37 0.0179(16) 0.0250(19) 0.038(2) -0.0096(17) 0.0035(16) -0.0034(14) C38 0.0258(18) 0.0270(19) 0.025(2) -0.0073(16) 0.0061(15) -0.0067(15) C39 0.0194(16) 0.0244(18) 0.028(2) -0.0095(16) 0.0006(15) -0.0044(14) C40 0.0198(15) 0.0163(16) 0.0173(17) -0.0061(13) -0.0030(13) -0.0025(12) C41 0.0246(17) 0.0182(17) 0.0209(18) -0.0051(14) -0.0020(14) -0.0022(13) C42 0.046(2) 0.0173(18) 0.032(2) -0.0130(16) -0.0049(18) -0.0011(16) C43 0.042(2) 0.0184(19) 0.050(3) -0.0155(18) -0.013(2) -0.0065(16) C44 0.0238(18) 0.025(2) 0.062(3) -0.016(2) -0.0013(19) -0.0099(15) C45 0.0244(17) 0.0219(18) 0.043(2) -0.0172(17) 0.0040(17) -0.0054(14) C46 0.0182(15) 0.0207(16) 0.0160(17) -0.0072(14) -0.0022(13) -0.0001(13) C47 0.0322(18) 0.0192(17) 0.0211(19) -0.0064(15) 0.0005(15) -0.0039(14) C48 0.050(2) 0.0239(19) 0.0173(19) -0.0015(15) -0.0021(17) -0.0048(17) C49 0.043(2) 0.033(2) 0.0177(19) -0.0093(16) -0.0048(17) 0.0013(17) C50 0.0269(17) 0.0277(19) 0.0228(19) -0.0137(16) -0.0043(15) -0.0003(15) C51 0.0221(16) 0.0232(17) 0.0170(17) -0.0055(14) -0.0018(14) -0.0030(13) C52 0.085(4) 0.038(3) 0.064(4) -0.021(3) -0.005(3) -0.011(3) C53 0.055(3) 0.069(4) 0.063(4) -0.039(3) 0.001(3) -0.021(3) C54 0.029(2) 0.072(3) 0.046(3) -0.032(3) 0.000(2) -0.012(2) C55 0.034(2) 0.070(3) 0.033(2) -0.014(2) -0.0026(19) -0.018(2) _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 Sn1 N1 2.114(3) . ? Sn1 Cl1 2.4439(9) . ? Si1 N1 1.743(3) . ? Si1 C40 1.874(3) . ? Si1 C46 1.881(3) . ? Si1 C34 1.882(3) . ? O1 C53 1.419(6) . ? O1 C54 1.423(5) . ? O2 C58 1.397(6) . ? O2 C57 1.407(6) . ? N1 C1 1.447(4) . ? C1 C6 1.403(4) . ? C1 C2 1.409(4) . ? C2 C3 1.396(4) . ? C2 C8 1.526(4) . ? C3 C4 1.389(5) . ? C4 C5 1.389(4) . ? C4 C7 1.510(4) . ? C5 C6 1.393(4) . ? C6 C21 1.531(4) . ? C8 C15 1.521(5) . ? C8 C9 1.526(4) . ? C9 C10 1.390(5) . ? C9 C14 1.391(5) . ? C10 C11 1.394(5) . ? C11 C12 1.374(6) . ? C12 C13 1.370(6) . ? C13 C14 1.405(5) . ? C15 C16 1.395(4) . ? C15 C20 1.401(5) . ? C16 C17 1.389(5) . ? C17 C18 1.376(5) . ? C18 C19 1.389(5) . ? C19 C20 1.385(5) . ? C21 C28 1.514(5) . ? C21 C22 1.528(4) . ? C22 C27 1.383(5) . ? C22 C23 1.394(5) . ? C23 C24 1.396(5) . ? C24 C25 1.364(6) . ? C25 C26 1.384(5) . ? C26 C27 1.396(5) . ? C28 C29 1.398(5) . ? C28 C33 1.402(4) . ? C29 C30 1.393(5) . ? C30 C31 1.386(5) . ? C31 C32 1.383(6) . ? C32 C33 1.391(5) . ? C34 C35 1.394(5) . ? C34 C39 1.401(5) . ? C35 C36 1.386(5) . ? C36 C37 1.376(6) . ? C37 C38 1.391(5) . ? C38 C39 1.383(5) . ? C40 C41 1.395(5) . ? C40 C45 1.395(5) . ? C41 C42 1.393(5) . ? C42 C43 1.375(6) . ? C43 C44 1.372(6) . ? C44 C45 1.388(5) . ? C46 C47 1.399(5) . ? C46 C51 1.407(4) . ? C47 C48 1.397(5) . ? C48 C49 1.379(5) . ? C49 C50 1.386(5) . ? C50 C51 1.385(5) . ? C52 C53 1.507(8) . ? C54 C55 1.478(7) . ? C56 C57 1.521(5) . ? C58 C59 1.506(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 Cl1 98.10(7) . . ? N1 Si1 C40 108.30(13) . . ? N1 Si1 C46 110.99(14) . . ? C40 Si1 C46 109.74(15) . . ? N1 Si1 C34 113.55(14) . . ? C40 Si1 C34 108.44(14) . . ? C46 Si1 C34 105.75(15) . . ? C53 O1 C54 113.5(4) . . ? C58 O2 C57 117.8(6) . . ? C1 N1 Si1 117.5(2) . . ? C1 N1 Sn1 110.10(19) . . ? Si1 N1 Sn1 132.31(14) . . ? C6 C1 C2 119.0(3) . . ? C6 C1 N1 121.0(3) . . ? C2 C1 N1 120.0(3) . . ? C3 C2 C1 119.4(3) . . ? C3 C2 C8 121.2(3) . . ? C1 C2 C8 119.2(3) . . ? C4 C3 C2 121.9(3) . . ? C3 C4 C5 118.0(3) . . ? C3 C4 C7 119.9(3) . . ? C5 C4 C7 122.0(3) . . ? C4 C5 C6 121.8(3) . . ? C5 C6 C1 119.7(3) . . ? C5 C6 C21 120.9(3) . . ? C1 C6 C21 119.1(3) . . ? C15 C8 C9 113.1(3) . . ? C15 C8 C2 109.0(3) . . ? C9 C8 C2 114.2(2) . . ? C10 C9 C14 118.8(3) . . ? C10 C9 C8 118.0(3) . . ? C14 C9 C8 123.2(3) . . ? C9 C10 C11 120.5(4) . . ? C12 C11 C10 120.4(4) . . ? C13 C12 C11 119.8(3) . . ? C12 C13 C14 120.6(4) . . ? C9 C14 C13 119.9(4) . . ? C16 C15 C20 117.7(3) . . ? C16 C15 C8 120.6(3) . . ? C20 C15 C8 121.7(3) . . ? C17 C16 C15 121.3(3) . . ? C18 C17 C16 120.0(3) . . ? C17 C18 C19 120.1(3) . . ? C20 C19 C18 119.9(3) . . ? C19 C20 C15 121.1(3) . . ? C28 C21 C22 113.6(3) . . ? C28 C21 C6 109.7(3) . . ? C22 C21 C6 115.3(3) . . ? C27 C22 C23 118.5(3) . . ? C27 C22 C21 119.4(3) . . ? C23 C22 C21 122.0(3) . . ? C22 C23 C24 120.0(4) . . ? C25 C24 C23 120.8(3) . . ? C24 C25 C26 120.0(3) . . ? C25 C26 C27 119.4(4) . . ? C22 C27 C26 121.3(3) . . ? C29 C28 C33 117.8(3) . . ? C29 C28 C21 121.5(3) . . ? C33 C28 C21 120.7(3) . . ? C30 C29 C28 121.4(3) . . ? C31 C30 C29 120.0(4) . . ? C32 C31 C30 119.4(3) . . ? C31 C32 C33 120.9(3) . . ? C32 C33 C28 120.5(3) . . ? C35 C34 C39 116.9(3) . . ? C35 C34 Si1 122.0(3) . . ? C39 C34 Si1 121.1(2) . . ? C36 C35 C34 122.0(3) . . ? C37 C36 C35 120.1(3) . . ? C36 C37 C38 119.3(3) . . ? C39 C38 C37 120.3(4) . . ? C38 C39 C34 121.4(3) . . ? C41 C40 C45 117.0(3) . . ? C41 C40 Si1 122.8(2) . . ? C45 C40 Si1 120.2(2) . . ? C42 C41 C40 121.1(3) . . ? C43 C42 C41 120.3(3) . . ? C44 C43 C42 119.7(3) . . ? C43 C44 C45 120.1(3) . . ? C44 C45 C40 121.7(3) . . ? C47 C46 C51 117.2(3) . . ? C47 C46 Si1 120.5(2) . . ? C51 C46 Si1 122.1(3) . . ? C48 C47 C46 121.4(3) . . ? C49 C48 C47 119.9(3) . . ? C48 C49 C50 120.1(3) . . ? C51 C50 C49 120.0(3) . . ? C50 C51 C46 121.4(3) . . ? O1 C53 C52 114.5(4) . . ? O1 C54 C55 110.0(4) . . ? O2 C57 C56 110.4(6) . . ? O2 C58 C59 111.7(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.960 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.106