Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email KEVINLEUNG@CUHK.EDU.HK _publ_contact_author_name 'Prof Wing-Por Leung' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name W.-P.Leung H.Cheng H.L.Hou H.-W.Li T.C.W.Mak Q.-C.Yang data_p-1 _database_code_CSD 198206 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H33 N3 Pb Si2' _chemical_formula_weight 662.93 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' Pb Pb -3.3944 10.1111 '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 8.5695(12) _cell_length_b 11.7207(16) _cell_length_c 13.8504(19) _cell_angle_alpha 84.487(2) _cell_angle_beta 83.495(3) _cell_angle_gamma 87.398(3) _cell_volume 1375.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 6.242 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5795 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9250 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.02 _reflns_number_total 6468 _reflns_number_gt 5799 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART CCD DIFFRACTOMETER' _computing_cell_refinement 'BRUKER SMART CCD DIFFRACTOMETER' _computing_data_reduction 'BRUKER SMART CCD DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6468 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0588 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 Pb1 Pb -0.039011(14) 0.024371(10) 0.144754(8) 0.03144(5) Uani 1 1 d . . . Si1 Si 0.33773(12) 0.12058(9) 0.20500(8) 0.0407(2) Uani 1 1 d . . . Si2 Si 0.09034(11) -0.23867(8) 0.23898(7) 0.0349(2) Uani 1 1 d . . . N1 N -0.1381(3) 0.1399(2) 0.26621(19) 0.0320(6) Uani 1 1 d . . . N2 N 0.1689(3) 0.1361(2) 0.1473(2) 0.0356(6) Uani 1 1 d . . . N3 N -0.0310(3) -0.1201(2) 0.26890(19) 0.0329(6) Uani 1 1 d . . . C1 C -0.2175(4) 0.1001(3) 0.3518(2) 0.0337(7) Uani 1 1 d . . . C2 C -0.2961(5) 0.1781(3) 0.4130(3) 0.0434(8) Uani 1 1 d . . . H2A H -0.3524 0.1521 0.4717 0.052 Uiso 1 1 calc R . . C3 C -0.2885(5) 0.2940(3) 0.3845(3) 0.0460(9) Uani 1 1 d . . . H3A H -0.3418 0.3464 0.4239 0.055 Uiso 1 1 calc R . . C4 C -0.2026(4) 0.3328(3) 0.2983(3) 0.0429(8) Uani 1 1 d . . . H4A H -0.1965 0.4110 0.2796 0.051 Uiso 1 1 calc R . . C5 C -0.1254(4) 0.2534(3) 0.2397(3) 0.0337(7) Uani 1 1 d . . . C6 C -0.0279(4) 0.2921(3) 0.1498(3) 0.0381(8) Uani 1 1 d . . . H6A H -0.0647 0.3564 0.1132 0.046 Uiso 1 1 calc R . . C7 C 0.1109(4) 0.2433(3) 0.1147(2) 0.0328(7) Uani 1 1 d . . . C8 C 0.2075(4) 0.3073(3) 0.0310(3) 0.0370(7) Uani 1 1 d . . . C9 C 0.2157(5) 0.4277(3) 0.0220(3) 0.0492(9) Uani 1 1 d . . . H9A H 0.1564 0.4704 0.0672 0.059 Uiso 1 1 calc R . . C10 C 0.3107(5) 0.4823(4) -0.0529(3) 0.0575(11) Uani 1 1 d . . . H10A H 0.3166 0.5617 -0.0573 0.069 Uiso 1 1 calc R . . C11 C 0.3971(5) 0.4216(4) -0.1213(3) 0.0602(12) Uani 1 1 d . . . H11A H 0.4611 0.4595 -0.1719 0.072 Uiso 1 1 calc R . . C12 C 0.3885(5) 0.3040(4) -0.1145(3) 0.0587(11) Uani 1 1 d . . . H12A H 0.4463 0.2628 -0.1613 0.070 Uiso 1 1 calc R . . C13 C 0.2946(4) 0.2460(3) -0.0388(3) 0.0447(8) Uani 1 1 d . . . H13A H 0.2901 0.1666 -0.0348 0.054 Uiso 1 1 calc R . . C14 C -0.2222(4) -0.0204(3) 0.3819(2) 0.0368(7) Uani 1 1 d . . . H14A H -0.2972 -0.0391 0.4343 0.044 Uiso 1 1 calc R . . C15 C -0.1372(4) -0.1139(3) 0.3482(2) 0.0325(7) Uani 1 1 d . . . C16 C -0.1761(4) -0.2239(3) 0.4104(2) 0.0352(7) Uani 1 1 d . . . C17 C -0.3039(5) -0.2849(3) 0.3946(3) 0.0502(9) Uani 1 1 d . . . H17A H -0.3654 -0.2575 0.3456 0.060 Uiso 1 1 calc R . . C18 C -0.3410(6) -0.3855(4) 0.4503(4) 0.0635(12) Uani 1 1 d . . . H18A H -0.4268 -0.4258 0.4385 0.076 Uiso 1 1 calc R . . C19 C -0.2526(6) -0.4261(4) 0.5225(4) 0.0699(14) Uani 1 1 d . . . H19A H -0.2768 -0.4947 0.5596 0.084 Uiso 1 1 calc R . . C20 C -0.1271(6) -0.3651(4) 0.5406(3) 0.0641(12) Uani 1 1 d . . . H20A H -0.0679 -0.3918 0.5909 0.077 Uiso 1 1 calc R . . C21 C -0.0888(5) -0.2652(3) 0.4847(3) 0.0459(9) Uani 1 1 d . . . H21A H -0.0032 -0.2250 0.4970 0.055 Uiso 1 1 calc R . . C22 C 0.4858(5) 0.0192(5) 0.1478(4) 0.0829(18) Uani 1 1 d . . . H22A H 0.5131 0.0458 0.0806 0.124 Uiso 1 1 calc R . . H22B H 0.4425 -0.0555 0.1519 0.124 Uiso 1 1 calc R . . H22C H 0.5781 0.0148 0.1815 0.124 Uiso 1 1 calc R . . C23 C 0.2897(6) 0.0638(4) 0.3340(3) 0.0664(13) Uani 1 1 d . . . H23A H 0.2143 0.1148 0.3661 0.100 Uiso 1 1 calc R . . H23B H 0.3835 0.0580 0.3663 0.100 Uiso 1 1 calc R . . H23C H 0.2464 -0.0106 0.3365 0.100 Uiso 1 1 calc R . . C24 C 0.4297(7) 0.2595(5) 0.2029(5) 0.097(2) Uani 1 1 d . . . H24A H 0.3553 0.3133 0.2320 0.146 Uiso 1 1 calc R . . H24B H 0.4625 0.2875 0.1366 0.146 Uiso 1 1 calc R . . H24C H 0.5195 0.2502 0.2390 0.146 Uiso 1 1 calc R . . C25 C -0.0048(5) -0.3799(3) 0.2473(3) 0.0556(11) Uani 1 1 d . . . H25A H -0.0924 -0.3731 0.2094 0.083 Uiso 1 1 calc R . . H25B H -0.0408 -0.4028 0.3142 0.083 Uiso 1 1 calc R . . H25C H 0.0700 -0.4363 0.2225 0.083 Uiso 1 1 calc R . . C26 C 0.1702(5) -0.2100(4) 0.1089(3) 0.0533(10) Uani 1 1 d . . . H26A H 0.0850 -0.1996 0.0691 0.080 Uiso 1 1 calc R . . H26B H 0.2367 -0.2737 0.0894 0.080 Uiso 1 1 calc R . . H26C H 0.2301 -0.1418 0.1010 0.080 Uiso 1 1 calc R . . C27 C 0.2589(5) -0.2587(4) 0.3140(3) 0.0530(10) Uani 1 1 d . . . H27A H 0.3110 -0.1875 0.3117 0.080 Uiso 1 1 calc R . . H27B H 0.3316 -0.3160 0.2885 0.080 Uiso 1 1 calc R . . H27C H 0.2208 -0.2829 0.3803 0.080 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 0.03564(8) 0.03058(7) 0.02724(7) -0.00022(4) -0.00159(5) -0.00170(5) Si1 0.0379(5) 0.0434(5) 0.0402(5) 0.0034(4) -0.0076(4) -0.0015(4) Si2 0.0383(5) 0.0301(4) 0.0349(5) -0.0018(4) 0.0002(4) 0.0014(4) N1 0.0317(14) 0.0307(13) 0.0326(14) -0.0036(11) 0.0011(11) 0.0005(11) N2 0.0298(14) 0.0312(14) 0.0422(16) 0.0078(12) 0.0012(12) 0.0005(11) N3 0.0353(15) 0.0304(14) 0.0311(14) 0.0005(11) 0.0018(11) -0.0010(11) C1 0.0314(17) 0.0359(17) 0.0337(17) -0.0038(13) -0.0026(13) -0.0008(14) C2 0.048(2) 0.046(2) 0.0342(18) -0.0062(15) 0.0048(16) 0.0019(17) C3 0.050(2) 0.0395(19) 0.048(2) -0.0180(17) 0.0016(17) 0.0059(17) C4 0.045(2) 0.0305(17) 0.054(2) -0.0082(16) -0.0052(17) -0.0003(15) C5 0.0293(16) 0.0315(16) 0.0405(18) -0.0016(14) -0.0058(14) -0.0002(13) C6 0.0395(19) 0.0295(16) 0.0421(19) 0.0055(14) 0.0001(15) 0.0014(14) C7 0.0340(17) 0.0310(16) 0.0324(16) 0.0031(13) -0.0034(13) -0.0023(13) C8 0.0328(17) 0.0372(18) 0.0385(18) 0.0089(14) -0.0016(14) -0.0048(14) C9 0.050(2) 0.0358(19) 0.057(2) 0.0053(17) 0.0059(19) -0.0037(17) C10 0.055(3) 0.043(2) 0.069(3) 0.018(2) 0.000(2) -0.0092(19) C11 0.047(2) 0.066(3) 0.059(3) 0.025(2) 0.005(2) -0.007(2) C12 0.054(3) 0.070(3) 0.044(2) 0.010(2) 0.0119(19) 0.008(2) C13 0.044(2) 0.043(2) 0.044(2) 0.0036(16) 0.0037(16) 0.0014(16) C14 0.0403(19) 0.0348(17) 0.0324(17) 0.0013(13) 0.0062(14) -0.0032(15) C15 0.0349(17) 0.0318(16) 0.0300(16) 0.0015(13) -0.0026(13) -0.0038(13) C16 0.0381(18) 0.0305(16) 0.0333(17) 0.0011(13) 0.0068(14) 0.0009(14) C17 0.045(2) 0.047(2) 0.056(2) 0.0079(18) -0.0041(18) -0.0064(18) C18 0.058(3) 0.049(2) 0.080(3) 0.005(2) 0.007(2) -0.021(2) C19 0.081(3) 0.043(2) 0.076(3) 0.023(2) 0.012(3) -0.011(2) C20 0.083(3) 0.054(3) 0.050(3) 0.017(2) -0.006(2) 0.005(2) C21 0.054(2) 0.042(2) 0.040(2) 0.0039(16) -0.0039(17) -0.0012(17) C22 0.049(3) 0.117(5) 0.082(4) -0.019(4) -0.009(3) 0.028(3) C23 0.085(4) 0.069(3) 0.045(2) 0.006(2) -0.015(2) -0.005(3) C24 0.107(5) 0.078(4) 0.116(5) 0.033(3) -0.070(4) -0.047(3) C25 0.063(3) 0.036(2) 0.068(3) -0.0103(19) 0.001(2) -0.0072(19) C26 0.059(3) 0.055(2) 0.042(2) -0.0017(18) 0.0059(18) 0.012(2) C27 0.045(2) 0.060(3) 0.052(2) -0.0032(19) -0.0011(18) 0.0104(19) _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 N2 2.264(3) . ? Pb1 N3 2.299(3) . ? Pb1 N1 2.322(3) . ? Si1 N2 1.725(3) . ? Si1 C24 1.837(5) . ? Si1 C23 1.853(5) . ? Si1 C22 1.862(5) . ? Si2 N3 1.751(3) . ? Si2 C26 1.858(4) . ? Si2 C27 1.866(4) . ? Si2 C25 1.866(4) . ? N1 C1 1.351(4) . ? N1 C5 1.352(4) . ? N2 C7 1.383(4) . ? N3 C15 1.350(4) . ? C1 C2 1.403(5) . ? C1 C14 1.436(5) . ? C2 C3 1.380(5) . ? C3 C4 1.379(5) . ? C4 C5 1.390(5) . ? C5 C6 1.465(5) . ? C6 C7 1.356(5) . ? C7 C8 1.504(4) . ? C8 C13 1.388(5) . ? C8 C9 1.410(5) . ? C9 C10 1.370(5) . ? C10 C11 1.369(6) . ? C11 C12 1.377(6) . ? C12 C13 1.390(5) . ? C14 C15 1.377(5) . ? C15 C16 1.510(4) . ? C16 C21 1.377(5) . ? C16 C17 1.383(5) . ? C17 C18 1.375(6) . ? C18 C19 1.360(7) . ? C19 C20 1.377(7) . ? C20 C21 1.372(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 N2 Pb1 N3 108.04(10) . . ? N2 Pb1 N1 79.81(10) . . ? N3 Pb1 N1 85.62(9) . . ? N2 Si1 C24 110.6(2) . . ? N2 Si1 C23 109.89(19) . . ? C24 Si1 C23 108.3(3) . . ? N2 Si1 C22 112.67(19) . . ? C24 Si1 C22 108.0(3) . . ? C23 Si1 C22 107.2(2) . . ? N3 Si2 C26 106.91(16) . . ? N3 Si2 C27 111.95(16) . . ? C26 Si2 C27 108.3(2) . . ? N3 Si2 C25 116.94(17) . . ? C26 Si2 C25 105.4(2) . . ? C27 Si2 C25 106.9(2) . . ? C1 N1 C5 121.8(3) . . ? C1 N1 Pb1 124.0(2) . . ? C5 N1 Pb1 113.9(2) . . ? C7 N2 Si1 121.2(2) . . ? C7 N2 Pb1 102.4(2) . . ? Si1 N2 Pb1 133.83(15) . . ? C15 N3 Si2 126.9(2) . . ? C15 N3 Pb1 117.5(2) . . ? Si2 N3 Pb1 114.43(13) . . ? N1 C1 C2 119.5(3) . . ? N1 C1 C14 121.3(3) . . ? C2 C1 C14 119.2(3) . . ? C3 C2 C1 119.0(3) . . ? C4 C3 C2 120.6(3) . . ? C3 C4 C5 119.0(3) . . ? N1 C5 C4 120.1(3) . . ? N1 C5 C6 119.7(3) . . ? C4 C5 C6 120.2(3) . . ? C7 C6 C5 126.3(3) . . ? C6 C7 N2 125.1(3) . . ? C6 C7 C8 118.2(3) . . ? N2 C7 C8 116.7(3) . . ? C13 C8 C9 118.6(3) . . ? C13 C8 C7 119.2(3) . . ? C9 C8 C7 122.2(3) . . ? C10 C9 C8 120.3(4) . . ? C11 C10 C9 120.9(4) . . ? C10 C11 C12 119.5(4) . . ? C11 C12 C13 121.0(4) . . ? C8 C13 C12 119.7(4) . . ? C15 C14 C1 132.5(3) . . ? N3 C15 C14 129.8(3) . . ? N3 C15 C16 117.7(3) . . ? C14 C15 C16 112.5(3) . . ? C21 C16 C17 118.4(3) . . ? C21 C16 C15 121.7(3) . . ? C17 C16 C15 119.9(3) . . ? C18 C17 C16 120.8(4) . . ? C19 C18 C17 120.2(4) . . ? C18 C19 C20 119.7(4) . . ? C21 C20 C19 120.3(4) . . ? C20 C21 C16 120.6(4) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.279 _refine_diff_density_min -1.078 _refine_diff_density_rms 0.093 data_p-1_b _database_code_CSD 198207 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H41 N3 Pb Si2' _chemical_formula_weight 622.96 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' Pb Pb -3.3944 10.1111 '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 9.751(2) _cell_length_b 12.115(2) _cell_length_c 12.609(3) _cell_angle_alpha 103.36(3) _cell_angle_beta 100.73(3) _cell_angle_gamma 100.66(3) _cell_volume 1382.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour RED _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 6.200 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.875 _exptl_absorpt_correction_T_max 1.073 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RAXIS-IIC RIGAKU' _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4114 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4114 _reflns_number_gt 3774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAXIS-IIC RIGAKU' _computing_cell_refinement 'BIOTEX RIGAKU' _computing_data_reduction 'BIOTEX RIGAKU' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1742P)^2^+1.6688P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0129(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4114 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.2156 _refine_ls_wR_factor_gt 0.2011 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.604 _refine_ls_shift/su_mean 0.099 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 0.489181(19) 0.354746(15) 0.228489(14) 0.06455(6) Uani 1 1 d . . . Si1 Si 0.73844(18) 0.38911(15) 0.08417(12) 0.0739(5) Uani 1 1 d . . . Si2 Si 0.66782(19) 0.13241(14) 0.29413(14) 0.0760(5) Uani 1 1 d . . . N1 N 0.5980(4) 0.4101(4) 0.4209(3) 0.0599(12) Uani 1 1 d . . . N2 N 0.7058(5) 0.4590(4) 0.2095(3) 0.0646(13) Uani 1 1 d . . . N3 N 0.5105(5) 0.1768(4) 0.2563(4) 0.0708(14) Uani 1 1 d . . . C1 C 0.7163(6) 0.4982(4) 0.4666(4) 0.0663(16) Uani 1 1 d . . . C2 C 0.7787(7) 0.5214(5) 0.5843(4) 0.0768(19) Uani 1 1 d . . . H2A H 0.8595 0.5822 0.6199 0.092 Uiso 1 1 calc R . . C3 C 0.7152(7) 0.4504(5) 0.6449(4) 0.0767(18) Uani 1 1 d . . . H3A H 0.7537 0.4650 0.7214 0.092 Uiso 1 1 calc R . . C4 C 0.5973(7) 0.3598(5) 0.5919(5) 0.0806(19) Uani 1 1 d . . . H4A H 0.5567 0.3141 0.6332 0.097 Uiso 1 1 calc R . . C5 C 0.5386(6) 0.3357(5) 0.4801(4) 0.0715(17) Uani 1 1 d . . . C6 C 0.7693(5) 0.5723(5) 0.4082(4) 0.0644(15) Uani 1 1 d . . . H6A H 0.8177 0.6465 0.4540 0.077 Uiso 1 1 calc R . . C7 C 0.7657(7) 0.5599(5) 0.2955(4) 0.0722(17) Uani 1 1 d . . . C8 C 0.8365(6) 0.6693(5) 0.2646(5) 0.0758(18) Uani 1 1 d . . . C9 C 0.8869(10) 0.7816(6) 0.3638(6) 0.108(3) Uani 1 1 d . . . H9A H 0.8076 0.7948 0.3961 0.161 Uiso 1 1 calc R . . H9B H 0.9220 0.8470 0.3373 0.161 Uiso 1 1 calc R . . H9C H 0.9624 0.7727 0.4197 0.161 Uiso 1 1 calc R . . C10 C 0.9699(8) 0.6529(6) 0.2155(6) 0.102(3) Uani 1 1 d . . . H10A H 0.9427 0.5838 0.1533 0.153 Uiso 1 1 calc R . . H10B H 1.0448 0.6451 0.2726 0.153 Uiso 1 1 calc R . . H10C H 1.0041 0.7196 0.1904 0.153 Uiso 1 1 calc R . . C11 C 0.7234(8) 0.6955(6) 0.1787(6) 0.094(2) Uani 1 1 d . . . H11A H 0.6422 0.7058 0.2095 0.142 Uiso 1 1 calc R . . H11B H 0.6931 0.6315 0.1117 0.142 Uiso 1 1 calc R . . H11C H 0.7637 0.7655 0.1610 0.142 Uiso 1 1 calc R . . C12 C 0.5927(9) 0.2504(6) 0.0164(4) 0.103(3) Uani 1 1 d . . . H12A H 0.5008 0.2694 0.0032 0.155 Uiso 1 1 calc R . . H12B H 0.5940 0.2003 0.0653 0.155 Uiso 1 1 calc R . . H12C H 0.6093 0.2111 -0.0537 0.155 Uiso 1 1 calc R . . C13 C 0.9156(8) 0.3402(7) 0.1062(7) 0.112(3) Uani 1 1 d . . . H13A H 0.9214 0.3027 0.1657 0.168 Uiso 1 1 calc R . . H13B H 0.9950 0.4070 0.1259 0.168 Uiso 1 1 calc R . . H13C H 0.9189 0.2863 0.0382 0.168 Uiso 1 1 calc R . . C14 C 0.4187(7) 0.2417(5) 0.4180(5) 0.0767(18) Uani 1 1 d . . . H14A H 0.3418 0.2298 0.4514 0.092 Uiso 1 1 calc R . . C15 C 0.4042(6) 0.1685(5) 0.3169(4) 0.0703(17) Uani 1 1 d . . . C16 C 0.2649(8) 0.0724(7) 0.2562(5) 0.097(3) Uani 1 1 d . . . C17 C 0.1493(7) 0.0671(7) 0.3260(7) 0.116(3) Uani 1 1 d . . . H17A H 0.1233 0.1408 0.3423 0.173 Uiso 1 1 calc R . . H17B H 0.1874 0.0507 0.3950 0.173 Uiso 1 1 calc R . . H17C H 0.0658 0.0065 0.2839 0.173 Uiso 1 1 calc R . . C18 C 0.3018(10) -0.0510(7) 0.2326(11) 0.170(5) Uani 1 1 d . . . H18A H 0.3725 -0.0520 0.1889 0.255 Uiso 1 1 calc R . . H18B H 0.2163 -0.1102 0.1920 0.255 Uiso 1 1 calc R . . H18C H 0.3389 -0.0659 0.3026 0.255 Uiso 1 1 calc R . . C19 C 0.2109(9) 0.0927(11) 0.1441(8) 0.183(4) Uani 1 1 d . . . H19A H 0.1880 0.1676 0.1554 0.274 Uiso 1 1 calc R . . H19B H 0.1264 0.0328 0.1029 0.274 Uiso 1 1 calc R . . H19C H 0.2839 0.0906 0.1026 0.274 Uiso 1 1 calc R . . C20 C 0.7270(10) 0.4631(7) -0.0335(6) 0.114(3) Uani 1 1 d . . . H20A H 0.6384 0.4876 -0.0445 0.171 Uiso 1 1 calc R . . H20B H 0.7302 0.4091 -0.1014 0.171 Uiso 1 1 calc R . . H20C H 0.8064 0.5299 -0.0139 0.171 Uiso 1 1 calc R . . C21 C 0.6447(9) 0.0406(6) 0.4014(7) 0.154(3) Uani 1 1 d . . . H21A H 0.6237 0.0872 0.4663 0.231 Uiso 1 1 calc R . . H21B H 0.7319 0.0170 0.4236 0.231 Uiso 1 1 calc R . . H21C H 0.5671 -0.0274 0.3669 0.231 Uiso 1 1 calc R . . C22 C 0.8317(7) 0.2556(6) 0.3580(6) 0.085(2) Uani 1 1 d . . . H22A H 0.8446 0.3012 0.3062 0.128 Uiso 1 1 calc R . . H22B H 0.9144 0.2245 0.3746 0.128 Uiso 1 1 calc R . . H22C H 0.8199 0.3040 0.4260 0.128 Uiso 1 1 calc R . . C23 C 0.7086(8) 0.0354(6) 0.1693(6) 0.103(2) Uani 1 1 d . . . H23A H 0.7209 0.0776 0.1147 0.154 Uiso 1 1 calc R . . H23B H 0.6303 -0.0324 0.1365 0.154 Uiso 1 1 calc R . . H23C H 0.7951 0.0117 0.1933 0.154 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 0.06685(11) 0.07195(10) 0.05065(9) 0.01628(8) 0.00644(8) 0.01468(8) Si1 0.0773(8) 0.0908(9) 0.0486(6) 0.0167(6) 0.0152(6) 0.0111(7) Si2 0.0860(9) 0.0755(8) 0.0692(8) 0.0203(6) 0.0206(7) 0.0232(7) N1 0.075(2) 0.073(2) 0.0259(14) 0.0092(14) 0.0069(14) 0.0138(18) N2 0.063(2) 0.070(2) 0.0533(19) 0.0150(17) 0.0124(16) 0.0009(18) N3 0.096(3) 0.0545(18) 0.056(2) 0.0098(16) 0.017(2) 0.0135(18) C1 0.081(3) 0.062(2) 0.042(2) 0.003(2) -0.006(2) 0.020(2) C2 0.096(4) 0.077(3) 0.048(2) 0.007(2) 0.010(2) 0.020(3) C3 0.099(3) 0.089(3) 0.046(2) 0.026(2) 0.013(2) 0.029(3) C4 0.113(4) 0.072(3) 0.065(3) 0.022(2) 0.031(3) 0.028(3) C5 0.096(3) 0.070(3) 0.051(2) 0.017(2) 0.022(2) 0.023(2) C6 0.061(2) 0.069(3) 0.057(2) 0.012(2) 0.007(2) 0.012(2) C7 0.094(3) 0.068(3) 0.052(2) 0.018(2) 0.013(2) 0.017(2) C8 0.077(3) 0.080(3) 0.066(3) 0.023(2) 0.012(2) 0.010(2) C9 0.140(6) 0.072(3) 0.098(4) 0.030(3) 0.020(4) -0.004(4) C10 0.108(5) 0.099(4) 0.096(4) 0.031(3) 0.031(3) 0.006(4) C11 0.099(4) 0.089(4) 0.088(4) 0.030(3) 0.003(3) 0.018(3) C12 0.155(6) 0.109(4) 0.031(2) 0.011(3) 0.007(3) 0.021(4) C13 0.084(4) 0.127(6) 0.106(5) 0.004(4) 0.037(3) -0.003(4) C14 0.096(3) 0.078(3) 0.060(3) 0.021(2) 0.022(2) 0.025(2) C15 0.076(3) 0.079(3) 0.058(2) 0.022(2) 0.023(2) 0.011(2) C16 0.093(4) 0.112(5) 0.066(3) 0.010(3) 0.018(3) -0.009(4) C17 0.057(3) 0.127(5) 0.156(6) 0.027(4) 0.046(3) -0.003(3) C18 0.123(5) 0.083(5) 0.270(11) -0.005(6) 0.088(6) -0.030(4) C19 0.098(5) 0.287(9) 0.099(5) 0.064(6) -0.012(4) -0.086(5) C20 0.157(6) 0.108(5) 0.074(3) 0.028(3) 0.040(4) 0.008(5) C21 0.201(5) 0.194(3) 0.162(5) 0.130(3) 0.075(4) 0.148(3) C22 0.070(3) 0.090(4) 0.082(4) 0.012(3) 0.002(3) 0.016(3) C23 0.119(4) 0.098(4) 0.100(4) 0.014(3) 0.035(3) 0.053(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 Pb1 N3 2.302(5) . ? Pb1 N2 2.335(4) . ? Pb1 N1 2.342(3) . ? Pb1 C15 2.800(6) . ? Si1 N2 1.728(5) . ? Si1 C12 1.891(7) . ? Si1 C20 1.899(8) . ? Si1 C13 1.921(9) . ? Si2 N3 1.739(5) . ? Si2 C22 1.874(6) . ? Si2 C23 1.889(8) . ? Si2 C21 1.958(9) . ? N1 C1 1.347(6) . ? N1 C5 1.409(7) . ? N2 C7 1.378(6) . ? N3 C15 1.401(8) . ? C1 C6 1.375(8) . ? C1 C2 1.434(7) . ? C2 C3 1.411(9) . ? C3 C4 1.371(8) . ? C4 C5 1.359(8) . ? C5 C14 1.426(7) . ? C6 C7 1.387(8) . ? C7 C8 1.545(9) . ? C8 C11 1.527(10) . ? C8 C9 1.548(8) . ? C8 C10 1.567(11) . ? C14 C15 1.340(7) . ? C15 C16 1.549(8) . ? C16 C19 1.505(13) . ? C16 C17 1.556(11) . ? C16 C18 1.576(12) . ? 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 N3 Pb1 N2 110.95(17) . . ? N3 Pb1 N1 79.17(15) . . ? N2 Pb1 N1 85.58(15) . . ? N3 Pb1 C15 29.88(18) . . ? N2 Pb1 C15 136.17(17) . . ? N1 Pb1 C15 71.29(14) . . ? N2 Si1 C12 108.7(3) . . ? N2 Si1 C20 118.7(3) . . ? C12 Si1 C20 101.1(3) . . ? N2 Si1 C13 112.1(3) . . ? C12 Si1 C13 105.6(4) . . ? C20 Si1 C13 109.4(4) . . ? N3 Si2 C22 114.1(3) . . ? N3 Si2 C23 111.7(3) . . ? C22 Si2 C23 106.1(3) . . ? N3 Si2 C21 109.1(3) . . ? C22 Si2 C21 108.5(3) . . ? C23 Si2 C21 107.0(4) . . ? C1 N1 C5 123.7(4) . . ? C1 N1 Pb1 121.9(3) . . ? C5 N1 Pb1 114.1(3) . . ? C7 N2 Si1 138.3(4) . . ? C7 N2 Pb1 113.0(4) . . ? Si1 N2 Pb1 108.61(18) . . ? C15 N3 Si2 121.3(4) . . ? C15 N3 Pb1 95.1(4) . . ? Si2 N3 Pb1 127.6(2) . . ? N1 C1 C6 122.7(4) . . ? N1 C1 C2 117.5(5) . . ? C6 C1 C2 119.5(4) . . ? C3 C2 C1 118.7(5) . . ? C4 C3 C2 120.6(5) . . ? C5 C4 C3 121.3(6) . . ? C4 C5 N1 118.1(5) . . ? C4 C5 C14 124.9(6) . . ? N1 C5 C14 117.0(5) . . ? C1 C6 C7 133.6(4) . . ? N2 C7 C6 125.9(5) . . ? N2 C7 C8 117.5(5) . . ? C6 C7 C8 116.6(4) . . ? C11 C8 C7 108.0(5) . . ? C11 C8 C9 105.0(6) . . ? C7 C8 C9 114.0(5) . . ? C11 C8 C10 109.9(6) . . ? C7 C8 C10 112.5(6) . . ? C9 C8 C10 107.0(5) . . ? C15 C14 C5 127.3(6) . . ? C14 C15 N3 122.6(5) . . ? C14 C15 C16 122.2(6) . . ? N3 C15 C16 115.2(5) . . ? C14 C15 Pb1 91.5(4) . . ? N3 C15 Pb1 55.0(3) . . ? C16 C15 Pb1 120.7(4) . . ? C19 C16 C15 107.2(6) . . ? C19 C16 C17 112.7(7) . . ? C15 C16 C17 113.5(5) . . ? C19 C16 C18 107.3(8) . . ? C15 C16 C18 109.5(6) . . ? C17 C16 C18 106.6(7) . . ? _diffrn_measured_fraction_theta_max 0.844 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.844 _refine_diff_density_max 2.722 _refine_diff_density_min -3.803 _refine_diff_density_rms 0.210 data_p21n_c _database_code_CSD 198208 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H33 Ge N3 Si2' _chemical_formula_weight 528.33 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONCLINIC _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.8767(18) _cell_length_b 13.7394(18) _cell_length_c 14.587(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.110(3) _cell_angle_gamma 90.00 _cell_volume 2770.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour RED _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.55 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.7638 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18346 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.04 _reflns_number_total 6692 _reflns_number_gt 4768 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART CCD DIFFRACTOMETER' _computing_cell_refinement 'BRUKER SMART CCD DIFFRACTOMETER' _computing_data_reduction 'BRUKER SMART CCD DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6692 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 Ge1 Ge 0.567985(13) 0.824564(13) 0.359996(14) 0.04720(8) Uani 1 1 d . . . Si2 Si 0.40904(4) 0.69638(4) 0.25883(4) 0.05451(14) Uani 1 1 d . . . Si1 Si 0.69096(4) 0.85658(5) 0.17369(4) 0.05940(15) Uani 1 1 d . . . N1 N 0.55671(10) 0.97009(10) 0.37528(10) 0.0465(3) Uani 1 1 d . . . N3 N 0.45129(10) 0.81790(10) 0.27022(11) 0.0480(3) Uani 1 1 d . . . N2 N 0.68175(10) 0.85191(11) 0.29129(11) 0.0524(4) Uani 1 1 d . . . C5 C 0.63750(13) 1.00663(14) 0.42234(13) 0.0524(4) Uani 1 1 d . . . C4 C 0.63472(16) 1.10010(15) 0.45952(15) 0.0637(5) Uani 1 1 d . . . H4A H 0.6877 1.1245 0.4959 0.076 Uiso 1 1 calc R . . C3 C 0.55289(16) 1.15575(14) 0.44179(16) 0.0639(6) Uani 1 1 d . . . H3A H 0.5504 1.2179 0.4667 0.077 Uiso 1 1 calc R . . C2 C 0.47530(15) 1.12031(13) 0.38789(15) 0.0615(5) Uani 1 1 d . . . H2A H 0.4213 1.1594 0.3739 0.074 Uiso 1 1 calc R . . C1 C 0.47703(13) 1.02542(12) 0.35372(13) 0.0493(4) Uani 1 1 d . . . C14 C 0.39954(13) 0.98612(13) 0.29436(14) 0.0539(5) Uani 1 1 d . . . H14A H 0.3478 1.0282 0.2803 0.065 Uiso 1 1 calc R . . C15 C 0.38971(12) 0.89618(13) 0.25508(13) 0.0480(4) Uani 1 1 d . . . C16 C 0.30162(13) 0.88433(13) 0.18850(14) 0.0540(5) Uani 1 1 d . . . C21 C 0.30842(17) 0.88057(18) 0.09459(17) 0.0757(6) Uani 1 1 d . . . H21A H 0.3689 0.8812 0.0718 0.091 Uiso 1 1 calc R . . C20 C 0.2257(2) 0.8759(2) 0.03444(19) 0.0929(8) Uani 1 1 d . . . H20A H 0.2310 0.8747 -0.0287 0.111 Uiso 1 1 calc R . . C19 C 0.13657(19) 0.87305(18) 0.0668(2) 0.0833(7) Uani 1 1 d . . . H19A H 0.0813 0.8689 0.0259 0.100 Uiso 1 1 calc R . . C18 C 0.12853(16) 0.87626(16) 0.1593(2) 0.0737(6) Uani 1 1 d . . . H18A H 0.0678 0.8742 0.1815 0.088 Uiso 1 1 calc R . . C17 C 0.21033(13) 0.88257(14) 0.21979(16) 0.0589(5) Uani 1 1 d . . . H17A H 0.2041 0.8857 0.2827 0.071 Uiso 1 1 calc R . . C6 C 0.72501(13) 0.94970(15) 0.42625(14) 0.0581(5) Uani 1 1 d . . . H6A H 0.7681 0.9555 0.4785 0.070 Uiso 1 1 calc R . . C7 C 0.74919(13) 0.88772(14) 0.35848(14) 0.0529(4) Uani 1 1 d . . . C8 C 0.85087(14) 0.85118(16) 0.36301(14) 0.0580(5) Uani 1 1 d . . . C9 C 0.92889(14) 0.91067(18) 0.39180(15) 0.0674(6) Uani 1 1 d . . . H9A H 0.9185 0.9756 0.4061 0.081 Uiso 1 1 calc R . . C10 C 1.02183(16) 0.8735(2) 0.39918(18) 0.0860(8) Uani 1 1 d . . . H10A H 1.0735 0.9134 0.4196 0.103 Uiso 1 1 calc R . . C11 C 1.03849(17) 0.7802(2) 0.37720(19) 0.0906(8) Uani 1 1 d . . . H11A H 1.1015 0.7566 0.3821 0.109 Uiso 1 1 calc R . . C12 C 0.96293(18) 0.7192(2) 0.3474(2) 0.0886(8) Uani 1 1 d . . . H12A H 0.9746 0.6548 0.3323 0.106 Uiso 1 1 calc R . . C13 C 0.86910(15) 0.75596(17) 0.34039(17) 0.0739(6) Uani 1 1 d . . . H13A H 0.8178 0.7155 0.3201 0.089 Uiso 1 1 calc R . . C27 C 0.3600(2) 0.65695(17) 0.1424(2) 0.0938(8) Uani 1 1 d . . . H27A H 0.3064 0.6977 0.1213 0.141 Uiso 1 1 calc R . . H27B H 0.3387 0.5906 0.1448 0.141 Uiso 1 1 calc R . . H27C H 0.4096 0.6621 0.1007 0.141 Uiso 1 1 calc R . . C25 C 0.31590(19) 0.67486(16) 0.3406(2) 0.0867(8) Uani 1 1 d . . . H25A H 0.2615 0.7168 0.3253 0.130 Uiso 1 1 calc R . . H25B H 0.3429 0.6885 0.4021 0.130 Uiso 1 1 calc R . . H25C H 0.2952 0.6082 0.3365 0.130 Uiso 1 1 calc R . . C26 C 0.51193(16) 0.61287(15) 0.2924(2) 0.0835(7) Uani 1 1 d . . . H26A H 0.5617 0.6220 0.2516 0.125 Uiso 1 1 calc R . . H26B H 0.4897 0.5467 0.2887 0.125 Uiso 1 1 calc R . . H26C H 0.5374 0.6269 0.3544 0.125 Uiso 1 1 calc R . . C24 C 0.81433(16) 0.8891(2) 0.14363(18) 0.0862(7) Uani 1 1 d . . . H24A H 0.8325 0.9512 0.1700 0.129 Uiso 1 1 calc R . . H24B H 0.8146 0.8925 0.0779 0.129 Uiso 1 1 calc R . . H24C H 0.8595 0.8405 0.1674 0.129 Uiso 1 1 calc R . . C22 C 0.6585(2) 0.7362(2) 0.1214(2) 0.1107(10) Uani 1 1 d . . . H22A H 0.5948 0.7181 0.1362 0.166 Uiso 1 1 calc R . . H22B H 0.7043 0.6882 0.1453 0.166 Uiso 1 1 calc R . . H22C H 0.6595 0.7402 0.0558 0.166 Uiso 1 1 calc R . . C23 C 0.6052(2) 0.9482(3) 0.1219(2) 0.1329(14) Uani 1 1 d . . . H23A H 0.5409 0.9326 0.1367 0.199 Uiso 1 1 calc R . . H23B H 0.6071 0.9482 0.0563 0.199 Uiso 1 1 calc R . . H23C H 0.6229 1.0115 0.1458 0.199 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 0.04812(12) 0.04385(11) 0.04968(13) -0.00060(8) 0.00470(8) -0.00219(8) Si2 0.0544(3) 0.0441(3) 0.0640(4) -0.0088(2) 0.0000(3) -0.0041(2) Si1 0.0534(3) 0.0721(4) 0.0535(4) -0.0027(3) 0.0094(3) -0.0003(3) N1 0.0496(8) 0.0451(8) 0.0455(9) -0.0047(6) 0.0084(7) -0.0051(6) N3 0.0470(8) 0.0431(8) 0.0538(9) -0.0018(6) 0.0032(7) -0.0017(6) N2 0.0459(8) 0.0593(9) 0.0522(10) -0.0102(7) 0.0054(7) -0.0037(7) C5 0.0577(11) 0.0550(11) 0.0456(11) -0.0065(8) 0.0099(9) -0.0095(9) C4 0.0694(13) 0.0657(13) 0.0578(13) -0.0177(10) 0.0148(10) -0.0197(11) C3 0.0777(14) 0.0507(11) 0.0673(14) -0.0176(10) 0.0277(12) -0.0126(10) C2 0.0684(13) 0.0449(10) 0.0733(15) -0.0041(9) 0.0167(11) 0.0006(9) C1 0.0551(10) 0.0436(9) 0.0508(11) -0.0016(8) 0.0135(9) -0.0022(8) C14 0.0499(10) 0.0482(10) 0.0636(13) 0.0007(9) 0.0051(9) 0.0069(8) C15 0.0460(9) 0.0519(10) 0.0465(11) 0.0024(8) 0.0071(8) -0.0002(8) C16 0.0562(11) 0.0473(10) 0.0577(13) 0.0031(9) 0.0008(9) 0.0006(8) C21 0.0705(14) 0.0953(17) 0.0610(15) 0.0059(13) 0.0038(12) -0.0055(12) C20 0.105(2) 0.111(2) 0.0593(16) 0.0076(14) -0.0145(15) -0.0191(17) C19 0.0779(17) 0.0783(16) 0.088(2) 0.0057(14) -0.0265(14) -0.0062(13) C18 0.0557(13) 0.0648(14) 0.098(2) -0.0022(13) -0.0091(12) -0.0029(10) C17 0.0535(11) 0.0563(11) 0.0657(14) -0.0025(10) 0.0000(10) 0.0000(9) C6 0.0555(11) 0.0679(12) 0.0503(12) -0.0064(9) 0.0005(9) -0.0068(9) C7 0.0479(10) 0.0583(11) 0.0523(12) 0.0007(9) 0.0038(9) -0.0048(8) C8 0.0509(11) 0.0704(13) 0.0527(12) 0.0053(10) 0.0046(9) -0.0015(9) C9 0.0522(11) 0.0885(16) 0.0612(14) 0.0016(11) 0.0046(10) -0.0083(11) C10 0.0522(13) 0.127(2) 0.0781(18) 0.0067(16) 0.0016(12) -0.0116(14) C11 0.0540(14) 0.130(3) 0.089(2) 0.0229(18) 0.0119(13) 0.0118(16) C12 0.0746(16) 0.0888(17) 0.105(2) 0.0180(16) 0.0225(15) 0.0185(14) C13 0.0586(12) 0.0764(15) 0.0879(18) 0.0082(13) 0.0136(12) -0.0011(11) C27 0.117(2) 0.0730(16) 0.0859(19) -0.0246(14) -0.0195(16) -0.0011(14) C25 0.0949(18) 0.0610(14) 0.109(2) -0.0018(13) 0.0350(16) -0.0162(12) C26 0.0798(15) 0.0502(12) 0.117(2) -0.0092(12) -0.0123(15) 0.0017(11) C24 0.0712(15) 0.116(2) 0.0733(18) -0.0003(15) 0.0170(13) -0.0149(14) C22 0.121(2) 0.134(3) 0.080(2) -0.0481(18) 0.0258(17) -0.038(2) C23 0.110(2) 0.178(3) 0.117(3) 0.076(2) 0.041(2) 0.061(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 N2 1.9798(15) . ? Ge1 N3 1.9920(16) . ? Ge1 N1 2.0195(14) . ? Si2 N3 1.7724(14) . ? Si2 C27 1.853(3) . ? Si2 C25 1.859(2) . ? Si2 C26 1.863(2) . ? Si1 N2 1.7326(17) . ? Si1 C23 1.848(3) . ? Si1 C22 1.860(3) . ? Si1 C24 1.859(2) . ? N1 C1 1.356(2) . ? N1 C5 1.358(2) . ? N3 C15 1.379(2) . ? N2 C7 1.384(2) . ? C5 C4 1.396(3) . ? C5 C6 1.441(3) . ? C4 C3 1.374(3) . ? C3 C2 1.365(3) . ? C2 C1 1.397(2) . ? C1 C14 1.425(3) . ? C14 C15 1.364(2) . ? C15 C16 1.501(3) . ? C16 C21 1.382(3) . ? C16 C17 1.384(3) . ? C21 C20 1.382(3) . ? C20 C19 1.363(3) . ? C19 C18 1.364(4) . ? C18 C17 1.377(3) . ? C6 C7 1.369(3) . ? C7 C8 1.493(3) . ? C8 C13 1.378(3) . ? C8 C9 1.391(3) . ? C9 C10 1.383(3) . ? C10 C11 1.346(4) . ? C11 C12 1.382(4) . ? C12 C13 1.392(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 N2 Ge1 N3 108.31(7) . . ? N2 Ge1 N1 86.62(6) . . ? N3 Ge1 N1 92.96(6) . . ? N3 Si2 C27 116.90(10) . . ? N3 Si2 C25 109.44(9) . . ? C27 Si2 C25 108.79(14) . . ? N3 Si2 C26 108.43(9) . . ? C27 Si2 C26 105.74(12) . . ? C25 Si2 C26 107.07(13) . . ? N2 Si1 C23 109.17(12) . . ? N2 Si1 C22 109.66(11) . . ? C23 Si1 C22 108.33(19) . . ? N2 Si1 C24 113.15(10) . . ? C23 Si1 C24 108.24(13) . . ? C22 Si1 C24 108.17(12) . . ? C1 N1 C5 121.99(15) . . ? C1 N1 Ge1 126.81(11) . . ? C5 N1 Ge1 110.69(12) . . ? C15 N3 Si2 121.64(12) . . ? C15 N3 Ge1 121.68(12) . . ? Si2 N3 Ge1 110.34(8) . . ? C7 N2 Si1 125.67(13) . . ? C7 N2 Ge1 103.21(12) . . ? Si1 N2 Ge1 129.84(9) . . ? N1 C5 C4 119.11(18) . . ? N1 C5 C6 118.31(16) . . ? C4 C5 C6 122.43(18) . . ? C3 C4 C5 119.32(19) . . ? C2 C3 C4 120.40(18) . . ? C3 C2 C1 120.05(19) . . ? N1 C1 C2 118.70(17) . . ? N1 C1 C14 118.95(15) . . ? C2 C1 C14 122.31(18) . . ? C15 C14 C1 129.81(17) . . ? C14 C15 N3 127.02(17) . . ? C14 C15 C16 114.54(16) . . ? N3 C15 C16 118.44(15) . . ? C21 C16 C17 118.12(19) . . ? C21 C16 C15 121.44(18) . . ? C17 C16 C15 120.34(18) . . ? C20 C21 C16 120.3(2) . . ? C19 C20 C21 120.6(3) . . ? C20 C19 C18 119.9(2) . . ? C19 C18 C17 120.0(2) . . ? C18 C17 C16 121.1(2) . . ? C7 C6 C5 124.67(18) . . ? C6 C7 N2 122.60(17) . . ? C6 C7 C8 117.94(18) . . ? N2 C7 C8 119.24(17) . . ? C13 C8 C9 118.39(19) . . ? C13 C8 C7 120.09(18) . . ? C9 C8 C7 121.50(19) . . ? C10 C9 C8 120.1(2) . . ? C11 C10 C9 120.8(2) . . ? C10 C11 C12 120.7(2) . . ? C11 C12 C13 118.8(3) . . ? C8 C13 C12 121.1(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.242 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.040 data_p-1_d _database_code_CSD 198209 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H33 N3 Si2 Sn' _chemical_formula_weight 574.43 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' 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 8.6497(17) _cell_length_b 11.619(2) _cell_length_c 13.869(3) _cell_angle_alpha 84.69(3) _cell_angle_beta 83.38(3) _cell_angle_gamma 88.21(3) _cell_volume 1378.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 1.214 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RAXIS-IIC RIGAKU' _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4629 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.53 _reflns_number_total 4629 _reflns_number_gt 4507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAXIS-IIC RIGAKU' _computing_cell_refinement 'BIOTEX RIGAKU' _computing_data_reduction 'BIOTEX RIGAKU' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1082P)^2^+0.2922P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.034(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4629 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1498 _refine_ls_wR_factor_gt 0.1485 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.03959(3) -0.02755(2) 0.348286(15) 0.05170(19) Uani 1 1 d . . . N1 N 0.1374(4) -0.1402(3) 0.2343(2) 0.0522(7) Uani 1 1 d . . . N2 N 0.0248(4) 0.1129(3) 0.2313(2) 0.0539(7) Uani 1 1 d . . . N3 N -0.1612(4) -0.1352(3) 0.3492(2) 0.0566(8) Uani 1 1 d . . . Si1 Si -0.09282(14) 0.23211(10) 0.26313(8) 0.0568(3) Uani 1 1 d . . . Si2 Si -0.33018(14) -0.12354(12) 0.29322(9) 0.0634(3) Uani 1 1 d . . . C1 C 0.1276(5) -0.2563(3) 0.2624(3) 0.0553(9) Uani 1 1 d . . . C2 C 0.2066(5) -0.3347(4) 0.2056(3) 0.0657(10) Uani 1 1 d . . . H2A H 0.2022 -0.4133 0.2254 0.079 Uiso 1 1 calc R . . C3 C 0.2930(6) -0.2963(4) 0.1182(4) 0.0712(12) Uani 1 1 d . . . H3A H 0.3471 -0.3490 0.0796 0.085 Uiso 1 1 calc R . . C4 C 0.2977(5) -0.1816(4) 0.0898(3) 0.0638(10) Uani 1 1 d . . . H4A H 0.3547 -0.1559 0.0312 0.077 Uiso 1 1 calc R . . C5 C 0.2174(5) -0.1010(4) 0.1479(3) 0.0545(9) Uani 1 1 d . . . C6 C 0.2196(5) 0.0194(4) 0.1177(3) 0.0581(9) Uani 1 1 d . . . H6A H 0.2936 0.0393 0.0651 0.070 Uiso 1 1 calc R . . C7 C 0.1348(5) 0.1110(4) 0.1507(3) 0.0551(9) Uani 1 1 d . . . C8 C 0.1700(5) 0.2225(3) 0.0905(3) 0.0578(9) Uani 1 1 d . . . C9 C 0.2992(5) 0.2845(4) 0.1050(4) 0.0715(12) Uani 1 1 d . . . H9A H 0.3617 0.2572 0.1528 0.086 Uiso 1 1 calc R . . C10 C 0.3344(7) 0.3861(5) 0.0487(5) 0.0880(16) Uani 1 1 d . . . H10A H 0.4205 0.4273 0.0592 0.106 Uiso 1 1 calc R . . C11 C 0.2452(8) 0.4271(5) -0.0220(5) 0.0954(18) Uani 1 1 d . . . H11A H 0.2707 0.4958 -0.0596 0.114 Uiso 1 1 calc R . . C12 C 0.1183(8) 0.3675(5) -0.0379(4) 0.0862(16) Uani 1 1 d . . . H12A H 0.0574 0.3962 -0.0861 0.103 Uiso 1 1 calc R . . C13 C 0.0800(6) 0.2653(4) 0.0168(3) 0.0694(11) Uani 1 1 d . . . H13A H -0.0057 0.2247 0.0049 0.083 Uiso 1 1 calc R . . C24 C 0.0044(7) 0.3746(4) 0.2581(5) 0.0828(15) Uani 1 1 d . . . H24A H 0.0909 0.3665 0.2960 0.124 Uiso 1 1 calc R . . H24B H -0.0688 0.4308 0.2842 0.124 Uiso 1 1 calc R . . H24C H 0.0408 0.3996 0.1917 0.124 Uiso 1 1 calc R . . C23 C -0.1732(6) 0.2003(5) 0.3937(3) 0.0782(13) Uani 1 1 d . . . H23A H -0.2254 0.1278 0.4015 0.117 Uiso 1 1 calc R . . H23B H -0.2458 0.2606 0.4125 0.117 Uiso 1 1 calc R . . H23C H -0.0898 0.1962 0.4340 0.117 Uiso 1 1 calc R . . C22 C -0.2594(6) 0.2560(5) 0.1879(4) 0.0747(12) Uani 1 1 d . . . H22A H -0.3130 0.1848 0.1884 0.112 Uiso 1 1 calc R . . H22B H -0.2205 0.2821 0.1221 0.112 Uiso 1 1 calc R . . H22C H -0.3299 0.3134 0.2145 0.112 Uiso 1 1 calc R . . C14 C 0.0305(5) -0.2936(4) 0.3519(3) 0.0595(9) Uani 1 1 d . . . H14A H 0.0658 -0.3574 0.3895 0.071 Uiso 1 1 calc R . . C15 C -0.1081(5) -0.2433(4) 0.3860(3) 0.0551(8) Uani 1 1 d . . . C16 C -0.2067(5) -0.3052(4) 0.4691(3) 0.0582(9) Uani 1 1 d . . . C17 C -0.2184(6) -0.4247(4) 0.4799(4) 0.0701(11) Uani 1 1 d . . . H17A H -0.1598 -0.4688 0.4357 0.084 Uiso 1 1 calc R . . C18 C -0.3157(6) -0.4793(5) 0.5554(4) 0.0822(14) Uani 1 1 d . . . H18A H -0.3241 -0.5593 0.5608 0.099 Uiso 1 1 calc R . . C19 C -0.3995(6) -0.4155(5) 0.6217(4) 0.0823(15) Uani 1 1 d . . . H19A H -0.4654 -0.4520 0.6724 0.099 Uiso 1 1 calc R . . C20 C -0.3867(6) -0.2977(5) 0.6139(4) 0.0801(14) Uani 1 1 d . . . H20A H -0.4419 -0.2548 0.6603 0.096 Uiso 1 1 calc R . . C21 C -0.2923(5) -0.2419(4) 0.5375(3) 0.0654(10) Uani 1 1 d . . . H21A H -0.2863 -0.1617 0.5320 0.079 Uiso 1 1 calc R . . C27 C -0.4772(6) -0.0267(6) 0.3534(4) 0.107(3) Uani 1 1 d . . . H27A H -0.5028 -0.0560 0.4202 0.161 Uiso 1 1 calc R . . H27B H -0.5692 -0.0234 0.3205 0.161 Uiso 1 1 calc R . . H27C H -0.4359 0.0494 0.3508 0.161 Uiso 1 1 calc R . . C25 C -0.4150(10) -0.2689(6) 0.2930(6) 0.129(3) Uani 1 1 d . . . H25A H -0.4408 -0.3012 0.3589 0.193 Uiso 1 1 calc R . . H25B H -0.3405 -0.3186 0.2595 0.193 Uiso 1 1 calc R . . H25C H -0.5073 -0.2617 0.2604 0.193 Uiso 1 1 calc R . . C26 C -0.2829(7) -0.0651(6) 0.1639(4) 0.0891(17) Uani 1 1 d . . . H26A H -0.2387 0.0100 0.1617 0.134 Uiso 1 1 calc R . . H26B H -0.3761 -0.0591 0.1322 0.134 Uiso 1 1 calc R . . H26C H -0.2093 -0.1161 0.1311 0.134 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 0.0560(3) 0.0504(3) 0.0470(2) 0.00321(13) -0.00418(13) -0.00271(14) N1 0.0508(17) 0.0531(18) 0.0507(17) -0.0007(13) 0.0001(12) -0.0038(13) N2 0.0571(19) 0.0527(18) 0.0489(17) 0.0079(13) -0.0019(12) -0.0046(13) N3 0.0510(18) 0.057(2) 0.0580(19) 0.0104(14) -0.0027(13) -0.0038(14) Si1 0.0630(7) 0.0516(7) 0.0534(6) 0.0021(5) -0.0018(4) 0.0011(5) Si2 0.0606(7) 0.0690(8) 0.0593(7) 0.0075(5) -0.0110(5) -0.0055(5) C1 0.054(2) 0.046(2) 0.064(2) 0.0001(16) -0.0060(16) -0.0004(15) C2 0.071(3) 0.050(2) 0.074(3) -0.0017(19) -0.0008(19) -0.0028(19) C3 0.078(3) 0.062(3) 0.073(3) -0.015(2) 0.001(2) 0.007(2) C4 0.069(3) 0.063(3) 0.055(2) -0.0016(18) 0.0043(17) 0.0024(19) C5 0.060(2) 0.055(2) 0.0471(19) 0.0007(16) -0.0022(15) -0.0015(16) C6 0.060(2) 0.057(2) 0.053(2) 0.0056(17) 0.0056(15) -0.0045(17) C7 0.054(2) 0.063(2) 0.0455(19) 0.0075(16) -0.0040(14) -0.0046(17) C8 0.064(2) 0.050(2) 0.056(2) 0.0026(17) 0.0027(16) 0.0006(17) C9 0.065(3) 0.065(3) 0.081(3) 0.007(2) -0.004(2) -0.009(2) C10 0.085(4) 0.071(3) 0.100(4) 0.014(3) 0.009(3) -0.017(3) C11 0.119(5) 0.066(3) 0.088(4) 0.025(3) 0.020(3) -0.002(3) C12 0.105(4) 0.073(3) 0.075(3) 0.021(3) -0.009(3) 0.009(3) C13 0.077(3) 0.067(3) 0.061(3) 0.008(2) -0.0056(19) 0.001(2) C24 0.098(4) 0.057(3) 0.090(4) -0.011(3) 0.003(3) -0.004(3) C23 0.089(3) 0.083(3) 0.057(3) 0.000(2) 0.007(2) 0.011(3) C22 0.077(3) 0.073(3) 0.069(3) 0.009(2) -0.005(2) 0.011(2) C14 0.061(2) 0.050(2) 0.063(2) 0.0099(17) -0.0027(17) -0.0001(17) C15 0.058(2) 0.050(2) 0.055(2) 0.0031(16) -0.0047(15) -0.0008(16) C16 0.054(2) 0.058(2) 0.060(2) 0.0092(17) -0.0063(16) -0.0028(17) C17 0.073(3) 0.058(3) 0.073(3) 0.010(2) 0.002(2) -0.001(2) C18 0.079(3) 0.069(3) 0.091(4) 0.027(3) -0.002(2) -0.014(2) C19 0.076(3) 0.083(4) 0.077(3) 0.028(3) 0.011(2) -0.003(2) C20 0.075(3) 0.090(4) 0.067(3) 0.013(2) 0.012(2) 0.006(3) C21 0.067(3) 0.061(3) 0.065(3) 0.0091(19) -0.0026(18) -0.0003(19) C27 0.065(4) 0.159(8) 0.097(5) -0.017(5) -0.013(3) 0.034(4) C25 0.148(7) 0.105(5) 0.141(6) 0.045(5) -0.083(5) -0.059(5) C26 0.105(4) 0.096(4) 0.066(3) 0.009(3) -0.021(3) -0.010(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 N3 2.170(3) . ? Sn1 N2 2.204(3) . ? Sn1 N1 2.221(3) . ? N1 C5 1.360(5) . ? N1 C1 1.372(5) . ? N2 C7 1.383(5) . ? N2 Si1 1.752(4) . ? N3 C15 1.396(5) . ? N3 Si2 1.728(4) . ? Si1 C23 1.871(5) . ? Si1 C22 1.874(5) . ? Si1 C24 1.872(5) . ? Si2 C27 1.849(6) . ? Si2 C25 1.862(6) . ? Si2 C26 1.862(5) . ? C1 C2 1.373(6) . ? C1 C14 1.454(6) . ? C2 C3 1.392(6) . ? C3 C4 1.354(7) . ? C4 C5 1.407(6) . ? C5 C6 1.423(6) . ? C6 C7 1.358(6) . ? C7 C8 1.495(6) . ? C8 C9 1.391(6) . ? C8 C13 1.401(6) . ? C9 C10 1.376(7) . ? C10 C11 1.360(9) . ? C11 C12 1.365(9) . ? C12 C13 1.377(7) . ? C14 C15 1.371(6) . ? C15 C16 1.494(5) . ? C16 C21 1.387(6) . ? C16 C17 1.388(6) . ? C17 C18 1.383(6) . ? C18 C19 1.364(8) . ? C19 C20 1.370(8) . ? C20 C21 1.384(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 N3 Sn1 N2 107.13(12) . . ? N3 Sn1 N1 81.81(13) . . ? N2 Sn1 N1 87.74(12) . . ? C5 N1 C1 121.1(3) . . ? C5 N1 Sn1 124.3(3) . . ? C1 N1 Sn1 114.2(2) . . ? C7 N2 Si1 125.7(3) . . ? C7 N2 Sn1 116.9(3) . . ? Si1 N2 Sn1 115.43(16) . . ? C15 N3 Si2 120.1(3) . . ? C15 N3 Sn1 102.7(2) . . ? Si2 N3 Sn1 135.00(18) . . ? N2 Si1 C23 106.8(2) . . ? N2 Si1 C22 112.3(2) . . ? C23 Si1 C22 108.5(2) . . ? N2 Si1 C24 117.2(2) . . ? C23 Si1 C24 105.0(3) . . ? C22 Si1 C24 106.5(3) . . ? N3 Si2 C27 112.2(2) . . ? N3 Si2 C25 110.1(3) . . ? C27 Si2 C25 109.1(4) . . ? N3 Si2 C26 109.1(2) . . ? C27 Si2 C26 108.6(3) . . ? C25 Si2 C26 107.6(3) . . ? N1 C1 C2 119.9(4) . . ? N1 C1 C14 118.6(4) . . ? C2 C1 C14 121.4(4) . . ? C1 C2 C3 120.0(4) . . ? C4 C3 C2 119.5(4) . . ? C3 C4 C5 120.8(4) . . ? N1 C5 C4 118.7(4) . . ? N1 C5 C6 120.2(4) . . ? C4 C5 C6 121.1(4) . . ? C7 C6 C5 132.5(4) . . ? C6 C7 N2 128.4(4) . . ? C6 C7 C8 113.6(3) . . ? N2 C7 C8 117.9(4) . . ? C9 C8 C13 118.4(4) . . ? C9 C8 C7 119.5(4) . . ? C13 C8 C7 122.1(4) . . ? C10 C9 C8 120.0(5) . . ? C11 C10 C9 120.9(6) . . ? C12 C11 C10 120.1(5) . . ? C11 C12 C13 120.5(5) . . ? C12 C13 C8 120.0(5) . . ? C15 C14 C1 126.0(4) . . ? C14 C15 N3 123.6(4) . . ? C14 C15 C16 118.7(4) . . ? N3 C15 C16 117.6(4) . . ? C21 C16 C17 118.2(4) . . ? C21 C16 C15 119.4(4) . . ? C17 C16 C15 122.4(4) . . ? C18 C17 C16 121.1(5) . . ? C19 C18 C17 119.8(5) . . ? C20 C19 C18 120.0(4) . . ? C19 C20 C21 120.6(5) . . ? C16 C21 C20 120.2(5) . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 25.53 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 1.255 _refine_diff_density_min -1.451 _refine_diff_density_rms 0.109