Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Michael F. Lappert' _publ_contact_author_address ; The Chemistry Laboratory University of Sussex Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; Synthesis and structures of b-diketiminatotin(II) halides, an amide and of Sn(=E)[{N(R)C(Ph)}2CH](NR2) (E = S or Se, R = SiMe3) ; loop_ _publ_author_name 'Michael F. Lappert' 'Peter B. Hitchcock' 'Jin Hu' 'Alexei Khovostov' data_(3)-jun1095 _database_code_depnum_ccdc_archive 'CCDC 247918' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H29 Br0.60 Cl0.40 N2 Si2 Sn' _chemical_formula_weight 546.64 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' Br Br -0.2901 2.4595 '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' 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 6.434(1) _cell_length_b 11.986(4) _cell_length_c 17.262(1) _cell_angle_alpha 98.87(2) _cell_angle_beta 100.23(1) _cell_angle_gamma 104.26(2) _cell_volume 1242.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 550 _exptl_absorpt_coefficient_mu 2.148 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details psi-scans _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 'Nonius CAD4' _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5978 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.97 _reflns_number_total 5978 _reflns_number_gt 4008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4 software' _computing_cell_refinement 'Nonius CAD4 software' _computing_data_reduction 'Nonius CAD4 software' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The halide ligand appears to be an unresolved mixture of Br and Cl in a ratio that refined to 0.604:0.396 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^)+(0.0287P)^2^+0.4596P] 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 5978 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn Sn 0.27851(5) 0.62822(3) 0.696454(18) 0.05355(12) Uani 1 1 d . . . Br Br 0.67442(10) 0.75222(7) 0.75537(5) 0.0790(3) Uani 0.604(4) 1 d P . . Cl Cl 0.67442(10) 0.75222(7) 0.75537(5) 0.0790(3) Uani 0.396(4) 1 d P . . Si1 Si 0.04535(18) 0.53256(9) 0.84118(7) 0.0433(3) Uani 1 1 d . . . Si2 Si 0.02370(19) 0.76721(11) 0.57276(6) 0.0524(3) Uani 1 1 d . . . N2 N 0.1748(5) 0.7810(3) 0.67194(17) 0.0406(7) Uani 1 1 d . . . N1 N 0.1873(5) 0.6595(2) 0.81157(18) 0.0395(7) Uani 1 1 d . . . C1 C 0.2326(6) 0.7710(3) 0.8502(2) 0.0365(8) Uani 1 1 d . . . C2 C 0.2690(6) 0.8686(3) 0.8147(2) 0.0410(9) Uani 1 1 d . . . H2 H 0.3330 0.9410 0.8499 0.049 Uiso 1 1 calc R . . C3 C 0.2222(6) 0.8720(3) 0.7335(2) 0.0369(8) Uani 1 1 d . . . C4 C 0.2503(7) 0.7961(3) 0.9387(2) 0.0443(9) Uani 1 1 d . . . C5 C 0.4039(7) 0.7615(4) 0.9896(3) 0.0538(10) Uani 1 1 d . . . H5 H 0.4950 0.7218 0.9683 0.065 Uiso 1 1 calc R . . C9 C 0.1169(9) 0.8553(4) 0.9722(3) 0.0627(12) Uani 1 1 d . . . H9 H 0.0154 0.8808 0.9391 0.075 Uiso 1 1 calc R . . C6 C 0.4216(9) 0.7858(4) 1.0717(3) 0.0716(14) Uani 1 1 d . . . H6 H 0.5269 0.7635 1.1053 0.086 Uiso 1 1 calc R . . C7 C 0.2878(11) 0.8416(5) 1.1042(3) 0.0811(17) Uani 1 1 d . . . H7 H 0.2998 0.8563 1.1595 0.097 Uiso 1 1 calc R . . C8 C 0.1338(11) 0.8765(4) 1.0544(3) 0.0842(17) Uani 1 1 d . . . H8 H 0.0411 0.9143 1.0763 0.101 Uiso 1 1 calc R . . C10 C 0.2336(6) 0.9919(3) 0.7164(2) 0.0415(9) Uani 1 1 d . . . C11 C 0.0986(8) 1.0554(4) 0.7425(2) 0.0554(11) Uani 1 1 d . . . H11 H -0.0025 1.0238 0.7713 0.066 Uiso 1 1 calc R . . C12 C 0.1128(10) 1.1659(4) 0.7260(3) 0.0731(14) Uani 1 1 d . . . H12 H 0.0179 1.2074 0.7421 0.088 Uiso 1 1 calc R . . C13 C 0.2668(10) 1.2144(4) 0.6860(3) 0.0754(16) Uani 1 1 d . . . H13 H 0.2777 1.2894 0.6758 0.091 Uiso 1 1 calc R . . C14 C 0.4036(9) 1.1535(4) 0.6610(3) 0.0698(14) Uani 1 1 d . . . H14 H 0.5083 1.1872 0.6343 0.084 Uiso 1 1 calc R . . C15 C 0.3879(7) 1.0412(4) 0.6753(2) 0.0546(11) Uani 1 1 d . . . H15 H 0.4802 0.9993 0.6574 0.066 Uiso 1 1 calc R . . C16 C -0.1512(8) 0.4376(4) 0.7483(3) 0.0705(14) Uani 1 1 d . . . H16A H -0.0716 0.4205 0.7081 0.106 Uiso 1 1 calc R . . H16B H -0.2546 0.4779 0.7285 0.106 Uiso 1 1 calc R . . H16C H -0.2287 0.3655 0.7606 0.106 Uiso 1 1 calc R . . C17 C 0.2426(7) 0.4524(4) 0.8781(3) 0.0597(12) Uani 1 1 d . . . H17A H 0.3263 0.4387 0.8386 0.090 Uiso 1 1 calc R . . H17B H 0.1631 0.3785 0.8873 0.090 Uiso 1 1 calc R . . H17C H 0.3403 0.4987 0.9275 0.090 Uiso 1 1 calc R . . C18 C -0.1204(7) 0.5613(4) 0.9152(3) 0.0608(12) Uani 1 1 d . . . H18A H -0.2208 0.6027 0.8946 0.091 Uiso 1 1 calc R . . H18B H -0.0246 0.6081 0.9648 0.091 Uiso 1 1 calc R . . H18C H -0.2018 0.4879 0.9246 0.091 Uiso 1 1 calc R . . C19 C -0.1356(8) 0.8752(5) 0.5618(3) 0.0712(14) Uani 1 1 d . . . H19A H -0.2338 0.8695 0.5978 0.107 Uiso 1 1 calc R . . H19B H -0.2193 0.8589 0.5074 0.107 Uiso 1 1 calc R . . H19C H -0.0365 0.9531 0.5744 0.107 Uiso 1 1 calc R . . C20 C 0.2153(9) 0.7757(6) 0.5039(3) 0.099(2) Uani 1 1 d . . . H20A H 0.2965 0.7192 0.5104 0.148 Uiso 1 1 calc R . . H20B H 0.3157 0.8533 0.5163 0.148 Uiso 1 1 calc R . . H20C H 0.1329 0.7591 0.4493 0.148 Uiso 1 1 calc R . . C21 C -0.1776(9) 0.6192(4) 0.5453(3) 0.0802(16) Uani 1 1 d . . . H21A H -0.1009 0.5605 0.5503 0.120 Uiso 1 1 calc R . . H21B H -0.2585 0.6060 0.4908 0.120 Uiso 1 1 calc R . . H21C H -0.2776 0.6145 0.5807 0.120 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 Sn 0.0702(2) 0.04897(18) 0.04832(18) 0.00556(12) 0.02388(15) 0.02455(15) Br 0.0457(4) 0.1150(7) 0.0952(6) 0.0470(5) 0.0274(4) 0.0330(4) Cl 0.0457(4) 0.1150(7) 0.0952(6) 0.0470(5) 0.0274(4) 0.0330(4) Si1 0.0405(6) 0.0358(5) 0.0526(7) 0.0113(5) 0.0103(5) 0.0079(5) Si2 0.0447(7) 0.0740(8) 0.0324(6) 0.0016(5) 0.0057(5) 0.0132(6) N2 0.0409(18) 0.0454(18) 0.0343(16) 0.0056(13) 0.0076(14) 0.0123(15) N1 0.0414(18) 0.0341(16) 0.0421(17) 0.0062(13) 0.0110(14) 0.0086(13) C1 0.036(2) 0.0363(19) 0.0357(19) 0.0055(15) 0.0084(16) 0.0074(16) C2 0.046(2) 0.0349(19) 0.035(2) 0.0015(15) 0.0039(17) 0.0048(17) C3 0.035(2) 0.0393(19) 0.0351(19) 0.0076(15) 0.0091(16) 0.0071(16) C4 0.056(3) 0.0350(19) 0.038(2) 0.0082(16) 0.0096(18) 0.0058(18) C5 0.050(3) 0.054(2) 0.050(2) 0.011(2) 0.001(2) 0.008(2) C9 0.097(4) 0.058(3) 0.045(2) 0.016(2) 0.022(2) 0.035(3) C6 0.082(4) 0.071(3) 0.045(3) 0.017(2) -0.008(3) 0.003(3) C7 0.126(5) 0.066(3) 0.039(3) 0.010(2) 0.017(3) 0.005(3) C8 0.144(6) 0.068(3) 0.053(3) 0.011(2) 0.041(3) 0.041(4) C10 0.048(2) 0.044(2) 0.0273(18) 0.0080(16) 0.0016(16) 0.0069(18) C11 0.072(3) 0.051(2) 0.045(2) 0.0093(19) 0.013(2) 0.021(2) C12 0.104(4) 0.051(3) 0.068(3) 0.014(2) 0.011(3) 0.033(3) C13 0.107(5) 0.047(3) 0.056(3) 0.014(2) -0.006(3) 0.005(3) C14 0.080(4) 0.062(3) 0.050(3) 0.021(2) 0.003(3) -0.009(3) C15 0.053(3) 0.059(3) 0.041(2) 0.0111(19) 0.002(2) 0.002(2) C16 0.062(3) 0.050(3) 0.078(3) 0.005(2) -0.007(3) -0.002(2) C17 0.060(3) 0.050(2) 0.076(3) 0.021(2) 0.014(2) 0.023(2) C18 0.047(3) 0.062(3) 0.084(3) 0.030(2) 0.029(2) 0.016(2) C19 0.063(3) 0.093(4) 0.052(3) 0.015(3) -0.007(2) 0.026(3) C20 0.072(4) 0.173(6) 0.049(3) 0.007(3) 0.023(3) 0.034(4) C21 0.070(4) 0.076(3) 0.068(3) -0.014(3) -0.005(3) 0.003(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 Sn N2 2.172(3) . ? Sn N1 2.174(3) . ? Sn Br 2.5457(10) . ? Si1 N1 1.770(3) . ? Si1 C18 1.848(4) . ? Si1 C17 1.855(4) . ? Si1 C16 1.863(5) . ? Si2 N2 1.774(3) . ? Si2 C19 1.850(5) . ? Si2 C20 1.855(5) . ? Si2 C21 1.855(5) . ? N2 C3 1.333(4) . ? N1 C1 1.334(4) . ? C1 C2 1.391(5) . ? C1 C4 1.489(5) . ? C2 C3 1.389(5) . ? C3 C10 1.498(5) . ? C4 C9 1.387(6) . ? C4 C5 1.388(6) . ? C5 C6 1.381(6) . ? C9 C8 1.383(6) . ? C6 C7 1.358(7) . ? C7 C8 1.381(8) . ? C10 C11 1.377(6) . ? C10 C15 1.390(5) . ? C11 C12 1.382(6) . ? C12 C13 1.372(7) . ? C13 C14 1.359(7) . ? C14 C15 1.387(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 Sn N1 87.35(11) . . ? N2 Sn Br 91.98(9) . . ? N1 Sn Br 92.53(8) . . ? N1 Si1 C18 114.52(17) . . ? N1 Si1 C17 109.60(18) . . ? C18 Si1 C17 111.2(2) . . ? N1 Si1 C16 105.95(19) . . ? C18 Si1 C16 106.7(2) . . ? C17 Si1 C16 108.5(2) . . ? N2 Si2 C19 114.65(19) . . ? N2 Si2 C20 108.8(2) . . ? C19 Si2 C20 110.6(3) . . ? N2 Si2 C21 106.4(2) . . ? C19 Si2 C21 107.0(3) . . ? C20 Si2 C21 109.2(3) . . ? C3 N2 Si2 127.3(3) . . ? C3 N2 Sn 116.8(2) . . ? Si2 N2 Sn 115.83(15) . . ? C1 N1 Si1 126.9(3) . . ? C1 N1 Sn 117.5(2) . . ? Si1 N1 Sn 115.53(15) . . ? N1 C1 C2 125.3(3) . . ? N1 C1 C4 118.8(3) . . ? C2 C1 C4 115.9(3) . . ? C3 C2 C1 128.5(3) . . ? N2 C3 C2 126.4(3) . . ? N2 C3 C10 118.9(3) . . ? C2 C3 C10 114.8(3) . . ? C9 C4 C5 118.6(4) . . ? C9 C4 C1 121.2(4) . . ? C5 C4 C1 120.2(4) . . ? C6 C5 C4 120.2(5) . . ? C8 C9 C4 120.4(5) . . ? C7 C6 C5 121.1(5) . . ? C6 C7 C8 119.5(5) . . ? C7 C8 C9 120.3(5) . . ? C11 C10 C15 119.4(4) . . ? C11 C10 C3 121.4(3) . . ? C15 C10 C3 119.2(4) . . ? C10 C11 C12 120.2(4) . . ? C13 C12 C11 120.0(5) . . ? C14 C13 C12 120.3(5) . . ? C13 C14 C15 120.4(5) . . ? C14 C15 C10 119.6(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.848 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.090 #===END data_(5)-jun1495 _database_code_depnum_ccdc_archive 'CCDC 247919' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H25 Cl N2 Si Sn' _chemical_formula_weight 427.61 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 24.938(8) _cell_length_b 6.302(1) _cell_length_c 24.981(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.52(3) _cell_angle_gamma 90.00 _cell_volume 3872(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.516 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details psi-scans _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius CAD4' _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4858 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 21.98 _reflns_number_total 4738 _reflns_number_gt 3333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4 software' _computing_cell_refinement 'Nonius CAD4 software' _computing_data_reduction 'Nonius CAD4 software' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The C26 t-butyl group is disordered and the lower occupancy methyl C atoms were left isotropic. 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^)+(0.0151P)^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 4738 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 -0.07101(2) -0.15200(11) -0.05005(2) 0.03029(19) Uani 1 1 d . . . Cl1 Cl -0.04769(9) 0.2240(4) -0.06865(9) 0.0421(6) Uani 1 1 d . . . Si1 Si -0.17152(9) -0.2615(4) -0.14916(9) 0.0237(6) Uani 1 1 d . . . N1 N -0.1010(2) -0.2094(10) -0.1351(2) 0.0197(16) Uani 1 1 d . . . N2 N 0.0060(2) -0.2553(11) -0.0662(3) 0.0294(18) Uani 1 1 d . . . H2 H 0.0296 -0.2928 -0.0375 0.035 Uiso 1 1 calc R . . C1 C -0.0667(3) -0.1996(13) -0.1716(3) 0.025(2) Uani 1 1 d . . . C2 C -0.0113(3) -0.2240(14) -0.1617(3) 0.028(2) Uani 1 1 d . . . H2A H 0.0062 -0.2066 -0.1924 0.034 Uiso 1 1 calc R . . C3 C 0.0233(3) -0.2710(13) -0.1127(3) 0.023(2) Uani 1 1 d . . . C4 C -0.0905(3) -0.1538(14) -0.2295(3) 0.023(2) Uani 1 1 d . . . C5 C -0.1170(3) 0.0345(15) -0.2427(3) 0.033(2) Uani 1 1 d . . . H5 H -0.1198 0.1354 -0.2150 0.039 Uiso 1 1 calc R . . C6 C -0.1395(3) 0.0787(16) -0.2953(4) 0.041(3) Uani 1 1 d . . . H6 H -0.1579 0.2093 -0.3039 0.050 Uiso 1 1 calc R . . C7 C -0.1354(4) -0.0661(18) -0.3357(4) 0.048(3) Uani 1 1 d . . . H7 H -0.1507 -0.0345 -0.3722 0.058 Uiso 1 1 calc R . . C8 C -0.1090(3) -0.2577(16) -0.3232(4) 0.041(3) Uani 1 1 d . . . H8 H -0.1069 -0.3597 -0.3508 0.049 Uiso 1 1 calc R . . C9 C -0.0860(3) -0.2977(15) -0.2708(3) 0.034(2) Uani 1 1 d . . . H9 H -0.0666 -0.4263 -0.2623 0.040 Uiso 1 1 calc R . . C10 C 0.0809(3) -0.3475(15) -0.1148(3) 0.031(2) Uani 1 1 d . . . C11 C 0.1152(3) -0.3660(19) -0.0584(4) 0.063(3) Uani 1 1 d . . . H11C H 0.0985 -0.4692 -0.0369 0.095 Uiso 1 1 calc R . . H11B H 0.1172 -0.2274 -0.0404 0.095 Uiso 1 1 calc R . . H11A H 0.1519 -0.4134 -0.0618 0.095 Uiso 1 1 calc R . . C12 C 0.0782(4) -0.5621(17) -0.1420(4) 0.070(4) Uani 1 1 d . . . H12C H 0.0575 -0.5505 -0.1789 0.105 Uiso 1 1 calc R . . H12B H 0.0602 -0.6634 -0.1211 0.105 Uiso 1 1 calc R . . H12A H 0.1151 -0.6118 -0.1438 0.105 Uiso 1 1 calc R . . C13 C 0.1089(3) -0.1909(16) -0.1475(4) 0.054(3) Uani 1 1 d . . . H13C H 0.1458 -0.2406 -0.1492 0.081 Uiso 1 1 calc R . . H13B H 0.1107 -0.0514 -0.1299 0.081 Uiso 1 1 calc R . . H13A H 0.0882 -0.1797 -0.1843 0.081 Uiso 1 1 calc R . . C14 C -0.1859(3) -0.4429(13) -0.0936(3) 0.029(2) Uani 1 1 d . . . H14C H -0.2251 -0.4697 -0.0979 0.044 Uiso 1 1 calc R . . H14B H -0.1734 -0.3763 -0.0583 0.044 Uiso 1 1 calc R . . H14A H -0.1666 -0.5775 -0.0957 0.044 Uiso 1 1 calc R . . C15 C -0.2106(3) -0.0133(14) -0.1455(3) 0.036(2) Uani 1 1 d . . . H15C H -0.2059 0.0793 -0.1759 0.054 Uiso 1 1 calc R . . H15B H -0.1973 0.0594 -0.1112 0.054 Uiso 1 1 calc R . . H15A H -0.2492 -0.0473 -0.1475 0.054 Uiso 1 1 calc R . . C16 C -0.1962(3) -0.3998(15) -0.2140(3) 0.037(2) Uani 1 1 d . . . H16C H -0.2347 -0.4348 -0.2161 0.056 Uiso 1 1 calc R . . H16B H -0.1753 -0.5306 -0.2158 0.056 Uiso 1 1 calc R . . H16A H -0.1915 -0.3073 -0.2444 0.056 Uiso 1 1 calc R . . Sn2 Sn -0.41643(2) 0.12115(10) -0.00198(2) 0.02712(18) Uani 1 1 d . . . Cl2 Cl -0.45550(8) -0.2341(4) 0.01623(9) 0.0406(6) Uani 1 1 d . . . Si2 Si -0.28955(9) -0.0322(4) 0.01417(9) 0.0242(6) Uani 1 1 d . . . N3 N -0.3422(2) 0.0120(10) 0.0513(2) 0.0196(16) Uani 1 1 d . . . N4 N -0.4345(2) 0.2593(11) 0.0704(2) 0.0241(17) Uani 1 1 d . . . H4 H -0.4547 0.3744 0.0657 0.029 Uiso 1 1 calc R . . C17 C -0.3451(3) -0.0369(12) 0.1031(3) 0.0172(19) Uani 1 1 d . . . C18 C -0.3810(3) 0.0418(13) 0.1351(3) 0.022(2) Uani 1 1 d . . . H18 H -0.3787 -0.0176 0.1704 0.026 Uiso 1 1 calc R . . C19 C -0.4206(3) 0.2010(14) 0.1207(3) 0.026(2) Uani 1 1 d . A . C20 C -0.3063(3) -0.1993(12) 0.1315(3) 0.0158(19) Uani 1 1 d . . . C21 C -0.2695(3) -0.1494(14) 0.1771(3) 0.030(2) Uani 1 1 d . . . H21 H -0.2688 -0.0096 0.1914 0.036 Uiso 1 1 calc R . . C22 C -0.2338(4) -0.2992(14) 0.2022(3) 0.033(2) Uani 1 1 d . . . H22 H -0.2082 -0.2615 0.2333 0.040 Uiso 1 1 calc R . . C23 C -0.2350(3) -0.5041(15) 0.1825(3) 0.036(2) Uani 1 1 d . . . H23 H -0.2106 -0.6076 0.2002 0.043 Uiso 1 1 calc R . . C24 C -0.2717(3) -0.5576(15) 0.1372(3) 0.034(2) Uani 1 1 d . . . H24 H -0.2724 -0.6980 0.1232 0.040 Uiso 1 1 calc R . . C25 C -0.3076(3) -0.4063(14) 0.1120(3) 0.025(2) Uani 1 1 d . . . H25 H -0.3334 -0.4443 0.0811 0.031 Uiso 1 1 calc R . . C26 C -0.4496(3) 0.2996(14) 0.1646(3) 0.033(2) Uani 1 1 d . . . C30 C -0.2236(3) -0.1338(15) 0.0509(3) 0.033(2) Uani 1 1 d . . . H30C H -0.1977 -0.1472 0.0255 0.050 Uiso 1 1 calc R . . H30B H -0.2291 -0.2729 0.0666 0.050 Uiso 1 1 calc R . . H30A H -0.2091 -0.0346 0.0799 0.050 Uiso 1 1 calc R . . C31 C -0.3164(3) -0.2114(14) -0.0439(3) 0.041(2) Uani 1 1 d . . . H31C H -0.3498 -0.1508 -0.0644 0.062 Uiso 1 1 calc R . . H31B H -0.3242 -0.3513 -0.0299 0.062 Uiso 1 1 calc R . . H31A H -0.2892 -0.2258 -0.0678 0.062 Uiso 1 1 calc R . . C32 C -0.2754(4) 0.2283(14) -0.0139(4) 0.044(3) Uani 1 1 d . . . H32C H -0.2603 0.3239 0.0158 0.066 Uiso 1 1 calc R . . H32B H -0.3092 0.2884 -0.0337 0.066 Uiso 1 1 calc R . . H32A H -0.2491 0.2112 -0.0387 0.066 Uiso 1 1 calc R . . C27 C -0.4062(5) 0.375(3) 0.2125(5) 0.066(5) Uani 0.753(14) 1 d P A 1 H27A H -0.3822 0.4792 0.1993 0.098 Uiso 0.753(14) 1 calc PR A 1 H27B H -0.3846 0.2533 0.2281 0.098 Uiso 0.753(14) 1 calc PR A 1 H27C H -0.4242 0.4406 0.2403 0.098 Uiso 0.753(14) 1 calc PR A 1 C28 C -0.4864(6) 0.142(3) 0.1808(6) 0.076(6) Uani 0.753(14) 1 d P A 1 H28A H -0.5127 0.0992 0.1490 0.114 Uiso 0.753(14) 1 calc PR A 1 H28B H -0.5057 0.2032 0.2082 0.114 Uiso 0.753(14) 1 calc PR A 1 H28C H -0.4655 0.0181 0.1959 0.114 Uiso 0.753(14) 1 calc PR A 1 C29 C -0.4815(6) 0.500(2) 0.1440(5) 0.062(5) Uani 0.753(14) 1 d P A 1 H29A H -0.4565 0.6055 0.1330 0.093 Uiso 0.753(14) 1 calc PR A 1 H29B H -0.4989 0.5592 0.1731 0.093 Uiso 0.753(14) 1 calc PR A 1 H29C H -0.5093 0.4641 0.1129 0.093 Uiso 0.753(14) 1 calc PR A 1 C27A C -0.4321(19) 0.516(8) 0.1713(19) 0.066(15) Uiso 0.247(14) 1 d P A 2 H27D H -0.4396 0.5890 0.1362 0.099 Uiso 0.247(14) 1 calc PR A 2 H27E H -0.3929 0.5202 0.1851 0.099 Uiso 0.247(14) 1 calc PR A 2 H27F H -0.4517 0.5865 0.1972 0.099 Uiso 0.247(14) 1 calc PR A 2 C28A C -0.4397(13) 0.166(6) 0.2207(12) 0.029(10) Uiso 0.247(14) 1 d P A 2 H28D H -0.4550 0.0238 0.2143 0.043 Uiso 0.247(14) 1 calc PR A 2 H28E H -0.4574 0.2391 0.2478 0.043 Uiso 0.247(14) 1 calc PR A 2 H28F H -0.4005 0.1558 0.2342 0.043 Uiso 0.247(14) 1 calc PR A 2 C29A C -0.5138(15) 0.269(7) 0.1401(16) 0.049(13) Uiso 0.247(14) 1 d P A 2 H29D H -0.5223 0.3419 0.1051 0.074 Uiso 0.247(14) 1 calc PR A 2 H29E H -0.5359 0.3283 0.1655 0.074 Uiso 0.247(14) 1 calc PR A 2 H29F H -0.5219 0.1171 0.1350 0.074 Uiso 0.247(14) 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 Sn1 0.0282(3) 0.0421(4) 0.0209(3) -0.0030(3) 0.0052(3) -0.0037(3) Cl1 0.0509(15) 0.0314(15) 0.0419(14) -0.0052(12) 0.0013(11) 0.0026(12) Si1 0.0234(13) 0.0221(14) 0.0258(13) -0.0009(11) 0.0040(10) 0.0005(11) N1 0.019(3) 0.019(4) 0.021(4) -0.004(3) 0.001(3) -0.001(3) N2 0.026(4) 0.027(5) 0.032(4) -0.001(4) -0.006(3) -0.001(4) C1 0.022(5) 0.023(5) 0.031(5) 0.003(4) 0.010(4) 0.002(4) C2 0.024(5) 0.032(6) 0.028(5) 0.005(4) 0.006(4) -0.003(4) C3 0.034(5) 0.014(5) 0.020(5) -0.005(4) 0.006(4) -0.002(4) C4 0.019(4) 0.025(6) 0.025(5) 0.005(4) 0.003(4) -0.006(4) C5 0.029(5) 0.041(7) 0.031(5) 0.002(5) 0.013(4) -0.001(5) C6 0.043(6) 0.042(7) 0.039(6) 0.007(5) 0.004(5) 0.011(5) C7 0.037(6) 0.073(9) 0.033(6) 0.005(6) -0.003(5) -0.013(6) C8 0.036(6) 0.045(7) 0.042(6) -0.003(5) 0.006(5) 0.012(5) C9 0.026(5) 0.038(6) 0.036(5) 0.005(5) 0.002(4) 0.010(5) C10 0.023(5) 0.032(6) 0.038(5) 0.002(5) 0.004(4) 0.010(5) C11 0.033(6) 0.085(9) 0.066(7) 0.005(7) -0.006(5) 0.028(7) C12 0.050(7) 0.050(8) 0.112(10) -0.038(7) 0.017(7) 0.005(6) C13 0.027(5) 0.057(8) 0.078(7) 0.015(6) 0.010(5) 0.011(5) C14 0.031(5) 0.026(6) 0.032(5) 0.000(4) 0.010(4) 0.000(4) C15 0.036(5) 0.024(6) 0.048(6) 0.001(5) 0.004(4) 0.008(5) C16 0.038(5) 0.038(6) 0.036(5) -0.008(5) 0.008(4) 0.000(5) Sn2 0.0301(3) 0.0272(4) 0.0228(3) 0.0041(3) 0.0010(3) 0.0059(3) Cl2 0.0301(12) 0.0265(14) 0.0592(15) 0.0042(12) -0.0105(11) -0.0006(11) Si2 0.0277(13) 0.0189(14) 0.0275(13) -0.0002(11) 0.0091(10) 0.0016(12) N3 0.019(4) 0.016(4) 0.024(4) -0.005(3) 0.002(3) 0.006(3) N4 0.018(4) 0.018(4) 0.037(4) -0.004(4) 0.008(3) 0.003(3) C17 0.021(4) 0.010(5) 0.017(4) -0.008(4) -0.006(4) 0.000(4) C18 0.029(5) 0.022(5) 0.014(4) 0.007(4) 0.004(4) 0.001(4) C19 0.024(5) 0.029(6) 0.023(5) 0.000(4) 0.002(4) -0.006(4) C20 0.019(4) 0.019(5) 0.010(4) 0.001(4) 0.004(3) 0.001(4) C21 0.044(5) 0.024(5) 0.023(5) 0.010(4) 0.007(4) 0.011(5) C22 0.050(6) 0.028(6) 0.018(5) -0.004(4) -0.005(4) 0.001(5) C23 0.042(6) 0.034(7) 0.031(5) 0.018(5) 0.007(5) 0.012(5) C24 0.036(5) 0.030(6) 0.038(6) 0.004(5) 0.018(5) 0.008(5) C25 0.023(5) 0.032(6) 0.023(5) 0.002(4) 0.008(4) -0.005(5) C26 0.036(5) 0.029(6) 0.032(5) -0.002(4) 0.005(4) 0.009(5) C30 0.031(5) 0.040(6) 0.030(5) -0.004(5) 0.011(4) -0.012(5) C31 0.049(6) 0.031(6) 0.046(6) -0.003(5) 0.014(5) 0.004(5) C32 0.052(6) 0.028(6) 0.061(6) 0.010(5) 0.034(5) 0.005(5) C27 0.071(10) 0.074(13) 0.052(9) -0.027(9) 0.011(8) 0.001(10) C28 0.072(12) 0.075(12) 0.101(13) -0.009(11) 0.071(11) -0.023(10) C29 0.089(12) 0.059(11) 0.049(9) 0.007(8) 0.038(9) 0.043(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 Sn1 N2 2.129(6) . ? Sn1 N1 2.163(6) . ? Sn1 Cl1 2.502(3) . ? Si1 N1 1.767(6) . ? Si1 C16 1.852(8) . ? Si1 C15 1.853(8) . ? Si1 C14 1.878(8) . ? N1 C1 1.351(9) . ? N2 C3 1.309(9) . ? C1 C2 1.371(10) . ? C1 C4 1.496(10) . ? C2 C3 1.408(10) . ? C3 C10 1.524(10) . ? C4 C5 1.371(11) . ? C4 C9 1.393(11) . ? C5 C6 1.369(11) . ? C6 C7 1.376(12) . ? C7 C8 1.386(13) . ? C8 C9 1.362(11) . ? C10 C12 1.510(12) . ? C10 C13 1.521(12) . ? C10 C11 1.527(11) . ? Sn2 N4 2.123(6) . ? Sn2 N3 2.202(6) . ? Sn2 Cl2 2.513(2) . ? Si2 N3 1.751(6) . ? Si2 C32 1.843(9) . ? Si2 C30 1.860(8) . ? Si2 C31 1.872(8) . ? N3 C17 1.344(9) . ? N4 C19 1.299(9) . ? C17 C18 1.387(10) . ? C17 C20 1.503(10) . ? C18 C19 1.413(11) . ? C19 C26 1.540(11) . ? C20 C21 1.376(10) . ? C20 C25 1.391(11) . ? C21 C22 1.376(11) . ? C22 C23 1.380(12) . ? C23 C24 1.375(11) . ? C24 C25 1.386(11) . ? C26 C27A 1.43(5) . ? C26 C28 1.453(15) . ? C26 C29 1.536(15) . ? C26 C27 1.549(14) . ? C26 C28A 1.62(3) . ? C26 C29A 1.63(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Sn1 N1 86.5(2) . . ? N2 Sn1 Cl1 90.56(19) . . ? N1 Sn1 Cl1 91.66(18) . . ? N1 Si1 C16 115.9(3) . . ? N1 Si1 C15 110.4(4) . . ? C16 Si1 C15 109.8(4) . . ? N1 Si1 C14 105.8(3) . . ? C16 Si1 C14 106.4(4) . . ? C15 Si1 C14 108.1(4) . . ? C1 N1 Si1 126.5(5) . . ? C1 N1 Sn1 120.1(5) . . ? Si1 N1 Sn1 113.4(3) . . ? C3 N2 Sn1 129.1(5) . . ? N1 C1 C2 127.1(7) . . ? N1 C1 C4 117.8(6) . . ? C2 C1 C4 115.0(7) . . ? C1 C2 C3 129.5(7) . . ? N2 C3 C2 120.8(7) . . ? N2 C3 C10 120.3(7) . . ? C2 C3 C10 118.9(7) . . ? C5 C4 C9 118.6(7) . . ? C5 C4 C1 119.9(8) . . ? C9 C4 C1 121.5(8) . . ? C6 C5 C4 120.8(9) . . ? C5 C6 C7 120.0(9) . . ? C6 C7 C8 120.2(9) . . ? C9 C8 C7 119.0(9) . . ? C8 C9 C4 121.3(9) . . ? C12 C10 C13 109.3(8) . . ? C12 C10 C3 109.0(7) . . ? C13 C10 C3 109.3(7) . . ? C12 C10 C11 108.9(8) . . ? C13 C10 C11 107.9(8) . . ? C3 C10 C11 112.3(7) . . ? N4 Sn2 N3 83.6(2) . . ? N4 Sn2 Cl2 93.87(19) . . ? N3 Sn2 Cl2 85.68(17) . . ? N3 Si2 C32 105.5(3) . . ? N3 Si2 C30 118.3(3) . . ? C32 Si2 C30 106.5(4) . . ? N3 Si2 C31 107.6(3) . . ? C32 Si2 C31 108.0(4) . . ? C30 Si2 C31 110.4(4) . . ? C17 N3 Si2 129.6(5) . . ? C17 N3 Sn2 118.7(5) . . ? Si2 N3 Sn2 111.0(3) . . ? C19 N4 Sn2 130.3(6) . . ? N3 C17 C18 128.0(7) . . ? N3 C17 C20 118.6(6) . . ? C18 C17 C20 113.4(6) . . ? C17 C18 C19 126.7(7) . . ? N4 C19 C18 120.8(7) . . ? N4 C19 C26 119.5(7) . . ? C18 C19 C26 119.7(7) . . ? C21 C20 C25 118.6(7) . . ? C21 C20 C17 121.6(7) . . ? C25 C20 C17 119.8(6) . . ? C20 C21 C22 120.9(8) . . ? C21 C22 C23 120.3(8) . . ? C24 C23 C22 119.7(8) . . ? C23 C24 C25 119.8(9) . . ? C24 C25 C20 120.7(8) . . ? C27A C26 C28 144(2) . . ? C28 C26 C29 109.8(10) . . ? C27A C26 C19 107.3(19) . . ? C28 C26 C19 108.3(8) . . ? C29 C26 C19 111.8(8) . . ? C28 C26 C27 112.8(10) . . ? C29 C26 C27 105.2(10) . . ? C19 C26 C27 108.9(8) . . ? C27A C26 C28A 113(2) . . ? C19 C26 C28A 112.7(13) . . ? C27A C26 C29A 115(3) . . ? C19 C26 C29A 103.4(15) . . ? C28A C26 C29A 105(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 21.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.551 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.112 #===END data_(6)-sep1096 _database_code_depnum_ccdc_archive 'CCDC 247920' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C13 H17 Cl N2 Sn), (C7 H8)' _chemical_formula_sum 'C33 H42 Cl2 N4 Sn2' _chemical_formula_weight 802.99 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' Sn Sn -0.6537 1.4246 '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 11.280(6) _cell_length_b 25.044(12) _cell_length_c 12.767(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.19(3) _cell_angle_gamma 90.00 _cell_volume 3446(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.632 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details psi-scans _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius CAD4' _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4776 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0933 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 22.99 _reflns_number_total 4776 _reflns_number_gt 3434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4 software' _computing_cell_refinement 'Nonius CAD4 software' _computing_data_reduction 'Nonius CAD4 software' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The C6 ring of the toluene solvate was included as a rigid body. 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^)+(0.1037P)^2^+10.1016P] 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 4776 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.1987 _refine_ls_wR_factor_gt 0.1766 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.16112(8) 0.55651(3) 0.09960(6) 0.0299(3) Uani 1 1 d . . . Cl1 Cl 0.0050(3) 0.50562(11) 0.1714(2) 0.0349(7) Uani 1 1 d . . . N1 N 0.0097(9) 0.5994(4) -0.0087(7) 0.029(2) Uani 1 1 d . . . H1 H -0.0142 0.5875 -0.0766 0.035 Uiso 1 1 calc R . . N2 N 0.1710(9) 0.6246(4) 0.2015(8) 0.033(2) Uani 1 1 d . . . H2 H 0.2363 0.6258 0.2599 0.039 Uiso 1 1 calc R . . Sn2 Sn 0.29428(9) 0.48740(3) 0.42693(7) 0.0344(3) Uani 1 1 d . . . Cl2 Cl 0.4089(3) 0.57374(13) 0.4051(3) 0.0456(9) Uani 1 1 d . . . N3 N 0.3398(10) 0.4963(4) 0.5980(7) 0.033(2) Uani 1 1 d . . . H3 H 0.3993 0.4748 0.6351 0.039 Uiso 1 1 calc R . . N4 N 0.1343(9) 0.5302(4) 0.4345(8) 0.031(2) Uani 1 1 d . . . H4 H 0.0711 0.5282 0.3745 0.037 Uiso 1 1 calc R . . C1 C -0.0533(11) 0.6405(4) 0.0099(8) 0.027(3) Uani 1 1 d . . . C2 C -0.0127(12) 0.6714(5) 0.1036(9) 0.031(3) Uani 1 1 d . . . H2A H -0.0653 0.7003 0.1085 0.037 Uiso 1 1 calc R . . C3 C 0.0929(10) 0.6662(4) 0.1904(8) 0.024(3) Uani 1 1 d . . . C4 C -0.1791(12) 0.6545(5) -0.0747(9) 0.030(3) Uani 1 1 d . . . C5 C -0.2055(13) 0.6197(5) -0.1753(10) 0.047(4) Uani 1 1 d . . . H5A H -0.1414 0.6255 -0.2118 0.071 Uiso 1 1 calc R . . H5B H -0.2869 0.6290 -0.2256 0.071 Uiso 1 1 calc R . . H5C H -0.2052 0.5822 -0.1539 0.071 Uiso 1 1 calc R . . C6 C -0.1814(16) 0.7131(6) -0.1068(14) 0.070(5) Uani 1 1 d . . . H6A H -0.1160 0.7198 -0.1414 0.104 Uiso 1 1 calc R . . H6B H -0.1672 0.7354 -0.0411 0.104 Uiso 1 1 calc R . . H6C H -0.2623 0.7218 -0.1585 0.104 Uiso 1 1 calc R . . C7 C -0.2783(13) 0.6443(7) -0.0221(11) 0.055(4) Uani 1 1 d . . . H7A H -0.2637 0.6664 0.0438 0.082 Uiso 1 1 calc R . . H7B H -0.2775 0.6065 -0.0020 0.082 Uiso 1 1 calc R . . H7C H -0.3592 0.6533 -0.0736 0.082 Uiso 1 1 calc R . . C8 C 0.1235(11) 0.7088(5) 0.2762(9) 0.030(3) Uani 1 1 d . . . C9 C 0.1762(12) 0.6955(5) 0.3866(10) 0.037(3) Uani 1 1 d . . . H9 H 0.1931 0.6592 0.4074 0.044 Uiso 1 1 calc R . . C10 C 0.2036(11) 0.7353(5) 0.4653(10) 0.037(3) Uani 1 1 d . . . H10 H 0.2383 0.7263 0.5404 0.044 Uiso 1 1 calc R . . C11 C 0.1805(12) 0.7885(5) 0.4346(11) 0.042(3) Uani 1 1 d . . . H11 H 0.2002 0.8157 0.4888 0.050 Uiso 1 1 calc R . . C12 C 0.1283(14) 0.8019(5) 0.3244(11) 0.046(4) Uani 1 1 d . . . H12 H 0.1126 0.8381 0.3026 0.056 Uiso 1 1 calc R . . C13 C 0.1004(13) 0.7615(4) 0.2483(10) 0.037(3) Uani 1 1 d . . . H13 H 0.0637 0.7705 0.1733 0.044 Uiso 1 1 calc R . . C14 C 0.2949(11) 0.5286(5) 0.6611(10) 0.030(3) Uani 1 1 d . . . C15 C 0.1961(12) 0.5592(5) 0.6195(10) 0.035(3) Uani 1 1 d . . . H15 H 0.1795 0.5847 0.6685 0.042 Uiso 1 1 calc R . . C16 C 0.1130(11) 0.5593(4) 0.5137(9) 0.029(3) Uani 1 1 d . . . C17 C 0.3650(12) 0.5268(5) 0.7850(10) 0.038(3) Uani 1 1 d . . . C18 C 0.3200(15) 0.5690(6) 0.8496(11) 0.053(4) Uani 1 1 d . . . H18A H 0.2299 0.5661 0.8341 0.079 Uiso 1 1 calc R . . H18B H 0.3410 0.6045 0.8282 0.079 Uiso 1 1 calc R . . H18C H 0.3601 0.5636 0.9281 0.079 Uiso 1 1 calc R . . C19 C 0.5017(13) 0.5317(7) 0.8090(11) 0.062(4) Uani 1 1 d . . . H19A H 0.5315 0.5047 0.7674 0.093 Uiso 1 1 calc R . . H19B H 0.5415 0.5264 0.8876 0.093 Uiso 1 1 calc R . . H19C H 0.5221 0.5674 0.7877 0.093 Uiso 1 1 calc R . . C20 C 0.3400(16) 0.4709(6) 0.8274(12) 0.065(5) Uani 1 1 d . . . H20A H 0.2505 0.4660 0.8135 0.097 Uiso 1 1 calc R . . H20B H 0.3816 0.4684 0.9064 0.097 Uiso 1 1 calc R . . H20C H 0.3722 0.4431 0.7891 0.097 Uiso 1 1 calc R . . C21 C -0.0020(11) 0.5917(4) 0.4859(9) 0.029(3) Uani 1 1 d . . . C22 C -0.0575(12) 0.6084(5) 0.3798(10) 0.036(3) Uani 1 1 d . . . H22 H -0.0202 0.5993 0.3244 0.044 Uiso 1 1 calc R . . C23 C -0.1678(14) 0.6385(5) 0.3512(11) 0.046(4) Uani 1 1 d . . . H23 H -0.2058 0.6491 0.2774 0.055 Uiso 1 1 calc R . . C24 C -0.2191(12) 0.6521(5) 0.4317(11) 0.042(3) Uani 1 1 d . . . H24 H -0.2938 0.6723 0.4140 0.051 Uiso 1 1 calc R . . C25 C -0.1647(13) 0.6372(5) 0.5355(11) 0.044(4) Uani 1 1 d . . . H25 H -0.2014 0.6482 0.5901 0.053 Uiso 1 1 calc R . . C26 C -0.0589(13) 0.6070(5) 0.5670(10) 0.039(3) Uani 1 1 d . . . H26 H -0.0243 0.5965 0.6413 0.046 Uiso 1 1 calc R . . C27 C 0.4954(12) 0.7870(5) 0.6647(11) 0.071(5) Uani 1 1 d G . . C28 C 0.4464(13) 0.7670(9) 0.7446(10) 0.147(13) Uani 1 1 d G . . H28 H 0.4247 0.7906 0.7941 0.176 Uiso 1 1 calc R . . C29 C 0.4291(13) 0.7123(10) 0.7521(14) 0.177(19) Uani 1 1 d G . . H29 H 0.3956 0.6986 0.8067 0.213 Uiso 1 1 calc R . . C30 C 0.4609(16) 0.6777(6) 0.6796(19) 0.31(4) Uani 1 1 d G . . H30 H 0.4491 0.6403 0.6847 0.366 Uiso 1 1 calc R . . C31 C 0.5099(15) 0.6977(6) 0.5997(15) 0.145(12) Uani 1 1 d G . . H31 H 0.5316 0.6740 0.5502 0.174 Uiso 1 1 calc R . . C32 C 0.5272(11) 0.7524(6) 0.5922(10) 0.082(6) Uani 1 1 d G . . H32 H 0.5607 0.7661 0.5376 0.098 Uiso 1 1 calc R . . C33 C 0.501(2) 0.8408(9) 0.654(3) 0.174(15) Uani 1 1 d . . . H33A H 0.5374 0.8492 0.5951 0.260 Uiso 0.50 1 calc PR . . H33B H 0.5534 0.8561 0.7231 0.260 Uiso 0.50 1 calc PR . . H33C H 0.4177 0.8559 0.6368 0.260 Uiso 0.50 1 calc PR . . H33D H 0.4683 0.8583 0.7082 0.260 Uiso 0.50 1 calc PR . . H33E H 0.4523 0.8514 0.5802 0.260 Uiso 0.50 1 calc PR . . H33F H 0.5880 0.8516 0.6665 0.260 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 0.0295(5) 0.0281(5) 0.0316(5) -0.0023(3) 0.0084(4) 0.0081(4) Cl1 0.045(2) 0.0322(16) 0.0298(16) -0.0047(12) 0.0141(15) -0.0032(14) N1 0.041(7) 0.026(5) 0.019(5) -0.005(4) 0.007(5) 0.009(5) N2 0.029(6) 0.031(6) 0.031(5) 0.002(4) -0.004(5) 0.007(5) Sn2 0.0345(6) 0.0381(5) 0.0304(5) -0.0081(4) 0.0094(4) 0.0038(4) Cl2 0.036(2) 0.0400(19) 0.062(2) 0.0087(15) 0.0150(17) 0.0071(15) N3 0.032(6) 0.042(6) 0.024(5) 0.006(4) 0.007(5) 0.012(5) N4 0.016(6) 0.046(6) 0.036(6) -0.003(5) 0.014(5) -0.002(5) C1 0.035(8) 0.028(6) 0.019(6) -0.004(5) 0.011(5) -0.001(6) C2 0.033(8) 0.030(7) 0.033(7) -0.003(5) 0.015(6) 0.003(6) C3 0.020(7) 0.026(6) 0.023(6) -0.006(5) 0.004(5) -0.001(5) C4 0.035(8) 0.033(7) 0.025(6) 0.000(5) 0.010(6) 0.006(6) C5 0.045(9) 0.051(8) 0.034(7) -0.013(6) -0.008(7) 0.009(7) C6 0.063(12) 0.039(9) 0.083(12) 0.012(8) -0.014(10) -0.004(8) C7 0.039(9) 0.092(12) 0.037(8) 0.000(7) 0.017(7) 0.018(8) C8 0.015(7) 0.041(7) 0.034(7) -0.014(5) 0.009(5) -0.008(5) C9 0.027(8) 0.046(8) 0.034(7) -0.003(6) 0.002(6) 0.005(6) C10 0.021(7) 0.058(9) 0.031(7) -0.014(6) 0.006(6) 0.002(6) C11 0.027(8) 0.048(9) 0.052(9) -0.025(7) 0.014(7) -0.001(6) C12 0.052(10) 0.045(8) 0.041(8) -0.008(6) 0.013(7) 0.007(7) C13 0.045(9) 0.025(7) 0.040(7) -0.004(5) 0.011(7) -0.004(6) C14 0.025(7) 0.032(7) 0.042(7) -0.005(5) 0.025(6) -0.009(6) C15 0.035(8) 0.032(7) 0.036(7) -0.007(5) 0.007(6) 0.011(6) C16 0.033(8) 0.029(6) 0.027(6) 0.002(5) 0.011(6) 0.010(6) C17 0.035(8) 0.054(8) 0.028(7) -0.005(6) 0.014(6) -0.006(7) C18 0.062(11) 0.058(9) 0.030(7) -0.007(6) 0.001(7) 0.006(8) C19 0.035(9) 0.107(13) 0.036(8) -0.006(8) -0.002(7) -0.006(9) C20 0.068(12) 0.071(11) 0.055(9) 0.023(8) 0.019(9) -0.009(9) C21 0.025(7) 0.027(7) 0.036(7) 0.004(5) 0.014(6) 0.002(5) C22 0.038(8) 0.040(7) 0.035(7) 0.003(6) 0.017(6) 0.002(6) C23 0.050(10) 0.041(8) 0.041(8) 0.006(6) 0.007(7) 0.004(7) C24 0.023(8) 0.046(8) 0.054(9) 0.005(6) 0.004(7) 0.005(6) C25 0.039(9) 0.054(9) 0.051(9) 0.007(7) 0.029(7) 0.009(7) C26 0.042(9) 0.039(7) 0.034(7) -0.001(6) 0.010(6) 0.008(7) C27 0.060(12) 0.066(12) 0.077(12) -0.006(9) 0.002(10) 0.016(10) C28 0.032(12) 0.28(4) 0.12(2) 0.11(2) 0.009(12) 0.025(18) C29 0.07(2) 0.23(4) 0.20(3) 0.17(3) -0.014(19) 0.02(2) C30 0.031(16) 0.38(6) 0.48(8) 0.35(6) 0.02(3) 0.00(3) C31 0.09(2) 0.11(2) 0.17(3) 0.000(19) -0.053(19) 0.019(16) C32 0.032(10) 0.107(16) 0.098(14) -0.028(12) 0.007(10) -0.006(10) C33 0.10(2) 0.088(17) 0.26(4) -0.02(2) -0.06(2) -0.020(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 Sn1 N2 2.129(9) . ? Sn1 N1 2.142(9) . ? Sn1 Cl1 2.554(3) . ? N1 C1 1.312(14) . ? N2 C3 1.344(14) . ? Sn2 N3 2.102(9) . ? Sn2 N4 2.125(10) . ? Sn2 Cl2 2.576(4) . ? N3 C14 1.343(15) . ? N4 C16 1.325(14) . ? C1 C2 1.384(15) . ? C1 C4 1.548(16) . ? C2 C3 1.372(16) . ? C3 C8 1.495(15) . ? C4 C7 1.487(18) . ? C4 C5 1.506(16) . ? C4 C6 1.522(18) . ? C8 C13 1.373(17) . ? C8 C9 1.398(16) . ? C9 C10 1.384(17) . ? C10 C11 1.391(18) . ? C11 C12 1.397(19) . ? C12 C13 1.372(17) . ? C14 C15 1.328(17) . ? C14 C17 1.546(17) . ? C15 C16 1.398(17) . ? C16 C21 1.483(16) . ? C17 C19 1.485(19) . ? C17 C18 1.516(18) . ? C17 C20 1.558(19) . ? C21 C22 1.378(16) . ? C21 C26 1.423(16) . ? C22 C23 1.408(18) . ? C23 C24 1.363(18) . ? C24 C25 1.338(18) . ? C25 C26 1.369(18) . ? C27 C33 1.36(2) . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? 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 Sn1 N1 83.1(3) . . ? N2 Sn1 Cl1 95.6(3) . . ? N1 Sn1 Cl1 88.8(3) . . ? C1 N1 Sn1 130.4(7) . . ? C3 N2 Sn1 129.9(8) . . ? N3 Sn2 N4 81.3(4) . . ? N3 Sn2 Cl2 92.7(3) . . ? N4 Sn2 Cl2 92.4(3) . . ? C14 N3 Sn2 131.9(8) . . ? C16 N4 Sn2 131.3(8) . . ? N1 C1 C2 122.5(11) . . ? N1 C1 C4 119.0(9) . . ? C2 C1 C4 118.5(10) . . ? C3 C2 C1 129.1(11) . . ? N2 C3 C2 123.0(10) . . ? N2 C3 C8 118.2(10) . . ? C2 C3 C8 118.8(10) . . ? C7 C4 C5 107.5(12) . . ? C7 C4 C6 109.4(12) . . ? C5 C4 C6 110.1(11) . . ? C7 C4 C1 107.7(10) . . ? C5 C4 C1 112.0(10) . . ? C6 C4 C1 110.1(10) . . ? C13 C8 C9 118.9(11) . . ? C13 C8 C3 120.7(11) . . ? C9 C8 C3 120.3(11) . . ? C10 C9 C8 119.8(12) . . ? C9 C10 C11 120.2(12) . . ? C10 C11 C12 120.1(11) . . ? C13 C12 C11 118.5(13) . . ? C12 C13 C8 122.5(12) . . ? C15 C14 N3 122.0(12) . . ? C15 C14 C17 122.8(11) . . ? N3 C14 C17 115.3(11) . . ? C14 C15 C16 129.1(11) . . ? N4 C16 C15 121.1(11) . . ? N4 C16 C21 117.5(10) . . ? C15 C16 C21 121.4(10) . . ? C19 C17 C18 108.9(12) . . ? C19 C17 C14 113.3(10) . . ? C18 C17 C14 112.6(11) . . ? C19 C17 C20 106.6(13) . . ? C18 C17 C20 108.2(12) . . ? C14 C17 C20 106.9(11) . . ? C22 C21 C26 117.6(11) . . ? C22 C21 C16 120.8(11) . . ? C26 C21 C16 121.6(10) . . ? C21 C22 C23 121.7(12) . . ? C24 C23 C22 118.6(12) . . ? C25 C24 C23 120.3(13) . . ? C24 C25 C26 123.4(13) . . ? C25 C26 C21 118.4(12) . . ? C33 C27 C28 118.2(19) . . ? C33 C27 C32 121.6(19) . . ? C28 C27 C32 120.0 . . ? C27 C28 C29 120.0 . . ? C30 C29 C28 120.0 . . ? C29 C30 C31 120.0 . . ? C30 C31 C32 120.0 . . ? C31 C32 C27 120.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.277 _refine_diff_density_min -1.104 _refine_diff_density_rms 0.184 #===END data_(8)-feb596 _database_code_depnum_ccdc_archive 'CCDC 247921' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H47 N3 Si4 Sn' _chemical_formula_weight 644.73 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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 21.258(4) _cell_length_b 9.153(2) _cell_length_c 36.160(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.90(1) _cell_angle_gamma 90.00 _cell_volume 6799(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type none _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 'Nonius CAD4' _diffrn_measurement_method 'omega-2theta scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12247 _diffrn_reflns_av_R_equivalents 0.0992 _diffrn_reflns_av_sigmaI/netI 0.2180 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 24.98 _reflns_number_total 11921 _reflns_number_gt 4388 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4 software' _computing_cell_refinement 'Nonius CAD4 software' _computing_data_reduction 'Nonius CAD4 software' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Very weak diffraction . 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^)+(0.0895P)^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 11921 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2515 _refine_ls_R_factor_gt 0.0953 _refine_ls_wR_factor_ref 0.2686 _refine_ls_wR_factor_gt 0.1954 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Sn1 Sn 0.76174(6) 0.30298(11) -0.00384(3) 0.0444(3) Uani 1 1 d . . . Si1 Si 0.6147(2) 0.1513(5) -0.01476(14) 0.0493(12) Uani 1 1 d . . . Si2 Si 0.9231(3) 0.2972(6) 0.04026(17) 0.0662(15) Uani 1 1 d . . . Si3 Si 0.7876(3) 0.0563(5) -0.07015(13) 0.0524(13) Uani 1 1 d . . . Si4 Si 0.7773(3) 0.3737(5) -0.08903(15) 0.0659(16) Uani 1 1 d . . . N1 N 0.6996(6) 0.1161(12) 0.0046(3) 0.044(3) Uani 1 1 d . . . N2 N 0.8483(7) 0.2049(14) 0.0363(4) 0.050(4) Uani 1 1 d . . . N3 N 0.7823(7) 0.2352(11) -0.0568(4) 0.039(4) Uani 1 1 d . . . C1 C 0.7224(8) 0.0131(16) 0.0303(4) 0.046(4) Uani 1 1 d . . . C2 C 0.7869(7) 0.0046(17) 0.0545(4) 0.052(4) Uani 1 1 d . . . H2 H 0.7928 -0.0702 0.0724 0.062 Uiso 1 1 calc R . . C3 C 0.8421(7) 0.0859(18) 0.0563(5) 0.050(4) Uani 1 1 d . . . C4 C 0.6069(10) 0.2809(19) -0.0552(6) 0.071(6) Uani 1 1 d . . . H4A H 0.6221 0.2350 -0.0752 0.107 Uiso 1 1 calc R . . H4B H 0.6326 0.3665 -0.0464 0.107 Uiso 1 1 calc R . . H4C H 0.5621 0.3083 -0.0649 0.107 Uiso 1 1 calc R . . C5 C 0.5618(7) -0.0073(16) -0.0343(5) 0.064(5) Uani 1 1 d . . . H5A H 0.5641 -0.0782 -0.0144 0.096 Uiso 1 1 calc R . . H5B H 0.5763 -0.0508 -0.0548 0.096 Uiso 1 1 calc R . . H5C H 0.5176 0.0252 -0.0437 0.096 Uiso 1 1 calc R . . C6 C 0.5855(10) 0.2423(15) 0.0237(6) 0.062(6) Uani 1 1 d . . . H6A H 0.5896 0.1762 0.0448 0.094 Uiso 1 1 calc R . . H6B H 0.5407 0.2696 0.0140 0.094 Uiso 1 1 calc R . . H6C H 0.6112 0.3280 0.0322 0.094 Uiso 1 1 calc R . . C7 C 0.9019(11) 0.479(2) 0.0179(7) 0.117(9) Uani 1 1 d . . . H7A H 0.8770 0.4667 -0.0081 0.175 Uiso 1 1 calc R . . H7B H 0.9411 0.5319 0.0183 0.175 Uiso 1 1 calc R . . H7C H 0.8767 0.5324 0.0318 0.175 Uiso 1 1 calc R . . C8 C 0.9721(12) 0.197(2) 0.0134(9) 0.154(14) Uani 1 1 d . . . H8A H 0.9461 0.1768 -0.0120 0.231 Uiso 1 1 calc R . . H8B H 0.9869 0.1066 0.0263 0.231 Uiso 1 1 calc R . . H8C H 1.0090 0.2550 0.0120 0.231 Uiso 1 1 calc R . . C9 C 0.9701(12) 0.339(3) 0.0891(7) 0.161(14) Uani 1 1 d . . . H9A H 0.9434 0.3921 0.1022 0.242 Uiso 1 1 calc R . . H9B H 1.0075 0.3962 0.0883 0.242 Uiso 1 1 calc R . . H9C H 0.9842 0.2491 0.1026 0.242 Uiso 1 1 calc R . . C10 C 0.6788(8) -0.1093(16) 0.0362(4) 0.047(4) Uani 1 1 d . . . C11 C 0.6476(8) -0.1107(17) 0.0652(5) 0.058(5) Uani 1 1 d . . . H11 H 0.6519 -0.0307 0.0816 0.070 Uiso 1 1 calc R . . C12 C 0.6111(11) -0.2248(18) 0.0705(6) 0.072(7) Uani 1 1 d . . . H12 H 0.5928 -0.2238 0.0913 0.087 Uiso 1 1 calc R . . C13 C 0.5996(10) -0.344(2) 0.0460(6) 0.073(6) Uani 1 1 d . . . H13 H 0.5720 -0.4196 0.0490 0.088 Uiso 1 1 calc R . . C14 C 0.6312(10) -0.3464(18) 0.0168(6) 0.074(6) Uani 1 1 d . . . H14 H 0.6256 -0.4261 0.0003 0.089 Uiso 1 1 calc R . . C15 C 0.6703(9) -0.2332(17) 0.0117(6) 0.053(5) Uani 1 1 d . . . H15 H 0.6914 -0.2374 -0.0078 0.063 Uiso 1 1 calc R . . C16 C 0.8999(8) 0.025(2) 0.0868(5) 0.056(5) Uani 1 1 d . . . C17 C 0.9336(9) -0.085(2) 0.0767(7) 0.091(7) Uani 1 1 d . . . H17 H 0.9239 -0.1198 0.0517 0.109 Uiso 1 1 calc R . . C18 C 0.9856(12) -0.147(3) 0.1061(10) 0.123(11) Uani 1 1 d . . . H18 H 1.0097 -0.2251 0.1005 0.147 Uiso 1 1 calc R . . C19 C 0.9992(13) -0.091(4) 0.1423(10) 0.138(15) Uani 1 1 d . . . H19 H 1.0349 -0.1267 0.1608 0.166 Uiso 1 1 calc R . . C20 C 0.9629(13) 0.011(4) 0.1515(7) 0.141(14) Uani 1 1 d . . . H20 H 0.9716 0.0437 0.1767 0.169 Uiso 1 1 calc R . . C21 C 0.9116(10) 0.073(3) 0.1240(6) 0.106(9) Uani 1 1 d . . . H21 H 0.8856 0.1445 0.1307 0.127 Uiso 1 1 calc R . . C22 C 0.8329(9) -0.0680(15) -0.0303(4) 0.066(6) Uani 1 1 d . . . H22A H 0.8755 -0.0287 -0.0192 0.099 Uiso 1 1 calc R . . H22B H 0.8370 -0.1634 -0.0405 0.099 Uiso 1 1 calc R . . H22C H 0.8094 -0.0748 -0.0110 0.099 Uiso 1 1 calc R . . C23 C 0.7060(8) -0.0276(17) -0.0902(5) 0.076(6) Uani 1 1 d . . . H23A H 0.6804 -0.0190 -0.0720 0.113 Uiso 1 1 calc R . . H23B H 0.7111 -0.1289 -0.0956 0.113 Uiso 1 1 calc R . . H23C H 0.6844 0.0220 -0.1134 0.113 Uiso 1 1 calc R . . C24 C 0.8343(10) 0.0357(19) -0.1074(6) 0.090(7) Uani 1 1 d . . . H24A H 0.8770 0.0764 -0.0979 0.135 Uiso 1 1 calc R . . H24B H 0.8119 0.0863 -0.1302 0.135 Uiso 1 1 calc R . . H24C H 0.8378 -0.0660 -0.1130 0.135 Uiso 1 1 calc R . . C25 C 0.7487(11) 0.5495(17) -0.0733(6) 0.092(7) Uani 1 1 d . . . H25A H 0.7769 0.5776 -0.0491 0.138 Uiso 1 1 calc R . . H25B H 0.7051 0.5379 -0.0707 0.138 Uiso 1 1 calc R . . H25C H 0.7493 0.6238 -0.0920 0.138 Uiso 1 1 calc R . . C26 C 0.7193(12) 0.332(2) -0.1357(5) 0.109(8) Uani 1 1 d . . . H26A H 0.7315 0.2417 -0.1455 0.163 Uiso 1 1 calc R . . H26B H 0.7204 0.4094 -0.1535 0.163 Uiso 1 1 calc R . . H26C H 0.6762 0.3235 -0.1323 0.163 Uiso 1 1 calc R . . C27 C 0.8584(10) 0.416(2) -0.0984(7) 0.108(8) Uani 1 1 d . . . H27A H 0.8895 0.4375 -0.0746 0.162 Uiso 1 1 calc R . . H27B H 0.8542 0.4981 -0.1152 0.162 Uiso 1 1 calc R . . H27C H 0.8730 0.3324 -0.1101 0.162 Uiso 1 1 calc R . . Sn2 Sn 0.51013(6) 0.32014(11) 0.24631(3) 0.0480(4) Uani 1 1 d . A 1 Si5 Si 0.3652(2) 0.1515(5) 0.23335(15) 0.0585(14) Uani 1 1 d . A 1 Si6 Si 0.6713(3) 0.3244(6) 0.28954(16) 0.0702(16) Uani 1 1 d . A 1 Si7 Si 0.5432(3) 0.0841(5) 0.17958(13) 0.0525(13) Uani 1 1 d . A 1 Si8 Si 0.5213(3) 0.4009(6) 0.16014(16) 0.0716(17) Uani 1 1 d . A 1 N4 N 0.4510(6) 0.1284(13) 0.2540(3) 0.046(3) Uani 1 1 d . A 1 N5 N 0.5962(7) 0.2262(14) 0.2874(4) 0.048(4) Uani 1 1 d . A 1 N6 N 0.5296(8) 0.2593(12) 0.1933(5) 0.057(5) Uani 1 1 d . A 1 C28 C 0.4752(7) 0.0287(15) 0.2803(4) 0.039(4) Uani 1 1 d . A 1 C29 C 0.5356(7) 0.0247(17) 0.3051(4) 0.049(4) Uani 1 1 d . A 1 H29 H 0.5406 -0.0476 0.3237 0.059 Uiso 1 1 calc R A 1 C30 C 0.5926(8) 0.1108(18) 0.3078(4) 0.048(4) Uani 1 1 d . A 1 C31 C 0.3565(10) 0.2812(19) 0.1931(6) 0.079(7) Uani 1 1 d . A 1 H31A H 0.3761 0.2403 0.1743 0.118 Uiso 1 1 calc R A 1 H31B H 0.3778 0.3714 0.2025 0.118 Uiso 1 1 calc R A 1 H31C H 0.3112 0.2992 0.1818 0.118 Uiso 1 1 calc R A 1 C32 C 0.3192(8) -0.0152(19) 0.2135(6) 0.079(6) Uani 1 1 d . A 1 H32A H 0.3220 -0.0854 0.2335 0.119 Uiso 1 1 calc R A 1 H32B H 0.3373 -0.0561 0.1940 0.119 Uiso 1 1 calc R A 1 H32C H 0.2744 0.0097 0.2025 0.119 Uiso 1 1 calc R A 1 C33 C 0.3286(11) 0.228(2) 0.2708(7) 0.095(9) Uani 1 1 d . A 1 H33A H 0.3332 0.1590 0.2913 0.142 Uiso 1 1 calc R A 1 H33B H 0.2832 0.2476 0.2599 0.142 Uiso 1 1 calc R A 1 H33C H 0.3505 0.3173 0.2806 0.142 Uiso 1 1 calc R A 1 C34 C 0.6466(11) 0.509(2) 0.2700(8) 0.136(11) Uani 1 1 d . A 1 H34A H 0.6232 0.5571 0.2860 0.204 Uiso 1 1 calc R A 1 H34B H 0.6191 0.4999 0.2445 0.204 Uiso 1 1 calc R A 1 H34C H 0.6846 0.5644 0.2695 0.204 Uiso 1 1 calc R A 1 C35 C 0.7144(13) 0.243(2) 0.2571(8) 0.125(11) Uani 1 1 d . A 1 H35A H 0.6845 0.2279 0.2326 0.188 Uiso 1 1 calc R A 1 H35B H 0.7329 0.1517 0.2673 0.188 Uiso 1 1 calc R A 1 H35C H 0.7485 0.3082 0.2544 0.188 Uiso 1 1 calc R A 1 C36 C 0.7250(12) 0.361(3) 0.3369(6) 0.153(13) Uani 1 1 d . A 1 H36A H 0.7003 0.4041 0.3529 0.230 Uiso 1 1 calc R A 1 H36B H 0.7587 0.4278 0.3345 0.230 Uiso 1 1 calc R A 1 H36C H 0.7443 0.2716 0.3481 0.230 Uiso 1 1 calc R A 1 C37 C 0.4335(8) -0.0973(17) 0.2862(4) 0.050(5) Uani 1 1 d . A 1 C38 C 0.4039(10) -0.098(2) 0.3144(5) 0.080(6) Uani 1 1 d . A 1 H38 H 0.4088 -0.0171 0.3306 0.096 Uiso 1 1 calc R A 1 C39 C 0.3647(12) -0.219(3) 0.3206(7) 0.085(7) Uani 1 1 d . A 1 H39 H 0.3419 -0.2160 0.3393 0.102 Uiso 1 1 calc R A 1 C40 C 0.3629(12) -0.335(2) 0.2980(9) 0.102(8) Uani 1 1 d . A 1 H40 H 0.3403 -0.4172 0.3025 0.122 Uiso 1 1 calc R A 1 C41 C 0.3914(11) -0.339(2) 0.2696(7) 0.084(7) Uani 1 1 d . A 1 H41 H 0.3863 -0.4180 0.2530 0.101 Uiso 1 1 calc R A 1 C42 C 0.4302(11) -0.217(2) 0.2653(7) 0.081(7) Uani 1 1 d . A 1 H42 H 0.4543 -0.2219 0.2472 0.098 Uiso 1 1 calc R A 1 C43 C 0.6490(8) 0.057(2) 0.3380(5) 0.058(5) Uani 1 1 d . A 1 C44 C 0.6862(10) -0.055(3) 0.3298(6) 0.094(7) Uani 1 1 d . A 1 H44 H 0.6775 -0.0888 0.3047 0.113 Uiso 1 1 calc R A 1 C45 C 0.7359(13) -0.118(3) 0.3571(10) 0.133(11) Uani 1 1 d . A 1 H45 H 0.7625 -0.1880 0.3501 0.160 Uiso 1 1 calc R A 1 C46 C 0.7458(15) -0.080(4) 0.3939(11) 0.145(15) Uani 1 1 d . A 1 H46 H 0.7740 -0.1340 0.4128 0.174 Uiso 1 1 calc R A 1 C47 C 0.7141(14) 0.041(4) 0.4039(7) 0.129(11) Uani 1 1 d . A 1 H47 H 0.7264 0.0799 0.4285 0.155 Uiso 1 1 calc R A 1 C48 C 0.6625(11) 0.102(3) 0.3756(6) 0.092(7) Uani 1 1 d . A 1 H48 H 0.6371 0.1749 0.3824 0.110 Uiso 1 1 calc R A 1 C49 C 0.5850(9) -0.0374(16) 0.2197(5) 0.074(6) Uani 1 1 d . A 1 H49A H 0.6254 0.0064 0.2332 0.112 Uiso 1 1 calc R A 1 H49B H 0.5935 -0.1303 0.2096 0.112 Uiso 1 1 calc R A 1 H49C H 0.5577 -0.0511 0.2368 0.112 Uiso 1 1 calc R A 1 C50 C 0.4662(9) -0.0092(18) 0.1550(5) 0.089(7) Uani 1 1 d . A 1 H50A H 0.4430 0.0495 0.1339 0.133 Uiso 1 1 calc R A 1 H50B H 0.4399 -0.0229 0.1727 0.133 Uiso 1 1 calc R A 1 H50C H 0.4760 -0.1025 0.1457 0.133 Uiso 1 1 calc R A 1 C51 C 0.5974(12) 0.081(2) 0.1461(6) 0.104(8) Uani 1 1 d . A 1 H51A H 0.6379 0.1281 0.1580 0.156 Uiso 1 1 calc R A 1 H51B H 0.5765 0.1308 0.1229 0.156 Uiso 1 1 calc R A 1 H51C H 0.6057 -0.0189 0.1404 0.156 Uiso 1 1 calc R A 1 C52 C 0.4842(10) 0.5675(16) 0.1764(6) 0.088(7) Uani 1 1 d . A 1 H52A H 0.4429 0.5424 0.1808 0.132 Uiso 1 1 calc R A 1 H52B H 0.4781 0.6416 0.1570 0.132 Uiso 1 1 calc R A 1 H52C H 0.5126 0.6035 0.1997 0.132 Uiso 1 1 calc R A 1 C53 C 0.4681(13) 0.349(2) 0.1116(5) 0.113(9) Uani 1 1 d . A 1 H53A H 0.4858 0.2645 0.1023 0.169 Uiso 1 1 calc R A 1 H53B H 0.4667 0.4289 0.0941 0.169 Uiso 1 1 calc R A 1 H53C H 0.4249 0.3283 0.1136 0.169 Uiso 1 1 calc R A 1 C54 C 0.6001(13) 0.460(3) 0.1521(8) 0.146(11) Uani 1 1 d . A 1 H54A H 0.6211 0.3785 0.1437 0.219 Uiso 1 1 calc R A 1 H54B H 0.6275 0.4980 0.1755 0.219 Uiso 1 1 calc R A 1 H54C H 0.5925 0.5352 0.1328 0.219 Uiso 1 1 calc R 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 Sn1 0.0515(8) 0.0358(6) 0.0443(7) -0.0042(6) 0.0098(6) -0.0054(6) Si1 0.040(3) 0.046(3) 0.058(3) 0.006(2) 0.005(2) 0.001(2) Si2 0.057(4) 0.065(3) 0.071(4) -0.004(3) 0.007(3) -0.022(3) Si3 0.067(4) 0.042(3) 0.047(3) -0.007(2) 0.012(3) 0.002(2) Si4 0.092(4) 0.049(3) 0.056(3) 0.012(2) 0.019(3) -0.001(3) N1 0.037(8) 0.042(7) 0.043(8) 0.007(6) -0.012(6) -0.009(6) N2 0.050(10) 0.050(8) 0.038(9) 0.000(7) -0.008(7) -0.013(7) N3 0.056(11) 0.039(8) 0.034(9) -0.003(5) 0.032(8) -0.001(6) C1 0.055(11) 0.042(9) 0.043(10) -0.004(7) 0.014(8) 0.004(8) C2 0.028(10) 0.069(11) 0.050(11) 0.023(8) -0.004(8) 0.005(8) C3 0.027(9) 0.060(11) 0.056(11) 0.007(9) -0.001(8) -0.002(8) C4 0.056(15) 0.095(14) 0.055(14) 0.013(10) 0.000(11) -0.019(11) C5 0.041(11) 0.057(11) 0.080(13) -0.002(9) -0.009(9) -0.008(8) C6 0.072(16) 0.042(10) 0.087(17) -0.003(8) 0.047(14) 0.004(8) C7 0.102(19) 0.082(16) 0.16(3) 0.007(15) 0.025(17) -0.038(14) C8 0.11(2) 0.084(16) 0.31(4) -0.06(2) 0.14(3) -0.011(16) C9 0.14(2) 0.19(3) 0.11(2) 0.024(19) -0.059(18) -0.11(2) C10 0.056(11) 0.045(10) 0.044(10) 0.019(8) 0.019(9) 0.001(8) C11 0.075(13) 0.045(10) 0.058(12) 0.011(8) 0.022(10) -0.014(9) C12 0.099(19) 0.043(11) 0.084(18) 0.015(10) 0.041(15) -0.001(11) C13 0.079(15) 0.065(13) 0.075(14) 0.021(11) 0.020(12) -0.027(11) C14 0.080(15) 0.038(10) 0.092(16) -0.002(10) 0.003(13) -0.010(10) C15 0.047(13) 0.055(11) 0.057(13) -0.003(8) 0.014(10) -0.001(8) C16 0.029(10) 0.081(13) 0.063(13) 0.030(10) 0.019(9) 0.001(9) C17 0.044(13) 0.123(19) 0.105(18) 0.016(15) 0.016(13) 0.015(13) C18 0.054(17) 0.11(2) 0.19(3) 0.03(2) 0.012(19) 0.022(14) C19 0.042(17) 0.22(4) 0.13(3) 0.06(3) -0.020(18) 0.007(19) C20 0.07(2) 0.28(5) 0.058(16) 0.05(2) -0.010(15) -0.04(2) C21 0.062(15) 0.18(2) 0.053(14) 0.027(15) -0.019(12) -0.020(15) C22 0.102(16) 0.030(9) 0.052(11) -0.002(8) -0.006(10) 0.009(9) C23 0.064(13) 0.054(11) 0.093(15) -0.015(10) -0.009(11) -0.007(10) C24 0.13(2) 0.058(12) 0.085(16) -0.010(11) 0.043(14) 0.024(12) C25 0.14(2) 0.033(10) 0.105(18) 0.010(10) 0.033(15) 0.012(12) C26 0.15(2) 0.117(18) 0.048(13) 0.022(12) 0.006(14) 0.023(17) C27 0.098(19) 0.099(17) 0.15(2) 0.041(16) 0.071(17) -0.014(14) Sn2 0.0571(8) 0.0404(7) 0.0449(7) -0.0061(5) 0.0102(6) -0.0024(6) Si5 0.048(3) 0.060(3) 0.061(3) 0.001(2) 0.002(3) 0.001(2) Si6 0.062(4) 0.083(4) 0.064(4) -0.015(3) 0.013(3) -0.029(3) Si7 0.066(4) 0.046(3) 0.043(3) 0.000(2) 0.012(3) 0.009(2) Si8 0.109(5) 0.053(3) 0.059(4) 0.015(3) 0.033(3) 0.008(3) N4 0.049(9) 0.040(7) 0.043(8) 0.008(6) 0.000(7) -0.002(6) N5 0.053(10) 0.068(9) 0.039(9) -0.009(7) 0.040(8) -0.026(7) N6 0.067(13) 0.043(9) 0.049(12) -0.001(6) -0.008(9) -0.004(6) C28 0.031(9) 0.037(9) 0.051(10) -0.004(7) 0.013(8) -0.001(7) C29 0.041(11) 0.064(11) 0.042(10) 0.007(8) 0.009(8) -0.001(8) C30 0.059(12) 0.062(11) 0.021(8) -0.009(7) 0.006(8) -0.010(9) C31 0.050(14) 0.081(14) 0.098(19) 0.042(12) 0.006(13) 0.015(11) C32 0.040(12) 0.092(15) 0.098(16) -0.007(12) 0.002(11) 0.001(10) C33 0.073(18) 0.081(15) 0.13(2) 0.002(13) 0.016(16) 0.039(12) C34 0.096(19) 0.112(19) 0.20(3) 0.044(18) 0.043(18) -0.064(16) C35 0.13(3) 0.12(2) 0.15(3) -0.042(16) 0.09(2) -0.020(16) C36 0.16(3) 0.21(3) 0.085(18) -0.039(18) 0.007(17) -0.13(2) C37 0.045(11) 0.050(10) 0.038(10) -0.007(8) -0.017(8) 0.012(8) C38 0.113(18) 0.078(14) 0.058(13) -0.017(11) 0.038(13) -0.021(13) C39 0.090(19) 0.094(17) 0.077(18) 0.019(14) 0.033(15) -0.024(14) C40 0.11(2) 0.043(13) 0.15(3) 0.009(15) 0.043(19) 0.014(13) C41 0.094(18) 0.055(13) 0.110(19) -0.028(12) 0.039(15) -0.010(12) C42 0.071(16) 0.055(12) 0.14(2) -0.031(13) 0.060(15) -0.012(11) C43 0.021(10) 0.092(14) 0.062(13) -0.005(10) 0.010(9) -0.008(9) C44 0.055(15) 0.16(2) 0.056(13) 0.004(14) -0.006(11) 0.004(15) C45 0.07(2) 0.17(3) 0.14(3) 0.01(3) 0.01(2) 0.038(18) C46 0.09(2) 0.17(3) 0.16(3) 0.10(3) 0.02(3) 0.00(2) C47 0.11(2) 0.19(3) 0.063(17) 0.00(2) -0.021(17) -0.04(2) C48 0.081(17) 0.14(2) 0.058(14) 0.007(14) 0.020(13) -0.011(14) C49 0.097(16) 0.039(10) 0.085(14) -0.008(9) 0.020(12) 0.027(10) C50 0.096(17) 0.060(12) 0.083(15) -0.023(10) -0.025(13) 0.016(11) C51 0.17(2) 0.088(15) 0.085(16) -0.001(13) 0.093(17) 0.017(16) C52 0.124(19) 0.032(10) 0.100(17) 0.008(10) 0.012(14) -0.015(11) C53 0.20(3) 0.078(15) 0.051(13) 0.028(11) 0.019(15) 0.007(16) C54 0.16(3) 0.13(2) 0.17(3) 0.06(2) 0.08(2) -0.03(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 N3 2.162(13) . ? Sn1 N2 2.221(13) . ? Sn1 N1 2.229(12) . ? Si1 N1 1.788(12) . ? Si1 C4 1.857(18) . ? Si1 C6 1.861(18) . ? Si1 C5 1.862(14) . ? Si2 N2 1.772(14) . ? Si2 C9 1.83(2) . ? Si2 C8 1.84(2) . ? Si2 C7 1.85(2) . ? Si3 N3 1.718(11) . ? Si3 C23 1.865(16) . ? Si3 C24 1.88(2) . ? Si3 C22 1.893(14) . ? Si4 N3 1.707(13) . ? Si4 C26 1.86(2) . ? Si4 C25 1.861(17) . ? Si4 C27 1.88(2) . ? N1 C1 1.327(17) . ? N2 C3 1.332(19) . ? C1 C2 1.425(19) . ? C1 C10 1.50(2) . ? C2 C3 1.38(2) . ? C3 C16 1.53(2) . ? C10 C11 1.38(2) . ? C10 C15 1.42(2) . ? C11 C12 1.34(2) . ? C12 C13 1.39(2) . ? C13 C14 1.39(3) . ? C14 C15 1.37(2) . ? C16 C17 1.34(2) . ? C16 C21 1.37(3) . ? C17 C18 1.44(3) . ? C18 C19 1.37(4) . ? C19 C20 1.31(4) . ? C20 C21 1.39(3) . ? Sn2 N6 2.137(17) . ? Sn2 N5 2.213(16) . ? Sn2 N4 2.217(12) . ? Si5 N4 1.796(13) . ? Si5 C31 1.850(18) . ? Si5 C32 1.854(17) . ? Si5 C33 1.86(2) . ? Si6 N5 1.816(14) . ? Si6 C35 1.82(2) . ? Si6 C36 1.83(2) . ? Si6 C34 1.85(2) . ? Si7 N6 1.724(13) . ? Si7 C50 1.857(18) . ? Si7 C49 1.862(16) . ? Si7 C51 1.874(19) . ? Si8 N6 1.743(15) . ? Si8 C54 1.86(2) . ? Si8 C52 1.879(19) . ? Si8 C53 1.89(2) . ? N4 C28 1.324(17) . ? N5 C30 1.300(18) . ? C28 C29 1.365(19) . ? C28 C37 1.50(2) . ? C29 C30 1.43(2) . ? C30 C43 1.48(2) . ? C37 C42 1.32(2) . ? C37 C38 1.33(2) . ? C38 C39 1.44(3) . ? C39 C40 1.34(3) . ? C40 C41 1.32(3) . ? C41 C42 1.42(3) . ? C43 C44 1.37(3) . ? C43 C48 1.38(2) . ? C44 C45 1.38(3) . ? C45 C46 1.34(4) . ? C46 C47 1.39(4) . ? C47 C48 1.41(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 N3 Sn1 N2 98.1(5) . . ? N3 Sn1 N1 99.3(4) . . ? N2 Sn1 N1 91.2(4) . . ? N1 Si1 C4 107.5(8) . . ? N1 Si1 C6 106.6(8) . . ? C4 Si1 C6 108.9(9) . . ? N1 Si1 C5 117.3(6) . . ? C4 Si1 C5 106.1(8) . . ? C6 Si1 C5 110.3(8) . . ? N2 Si2 C9 115.5(10) . . ? N2 Si2 C8 109.7(9) . . ? C9 Si2 C8 111.6(14) . . ? N2 Si2 C7 106.3(8) . . ? C9 Si2 C7 104.3(11) . . ? C8 Si2 C7 108.9(12) . . ? N3 Si3 C23 112.3(8) . . ? N3 Si3 C24 112.5(7) . . ? C23 Si3 C24 106.9(9) . . ? N3 Si3 C22 114.6(7) . . ? C23 Si3 C22 106.8(8) . . ? C24 Si3 C22 103.0(9) . . ? N3 Si4 C26 112.2(9) . . ? N3 Si4 C25 113.7(8) . . ? C26 Si4 C25 105.2(10) . . ? N3 Si4 C27 112.1(9) . . ? C26 Si4 C27 107.7(11) . . ? C25 Si4 C27 105.4(10) . . ? C1 N1 Si1 123.5(11) . . ? C1 N1 Sn1 121.2(10) . . ? Si1 N1 Sn1 112.5(6) . . ? C3 N2 Si2 124.0(11) . . ? C3 N2 Sn1 120.3(10) . . ? Si2 N2 Sn1 115.8(7) . . ? Si4 N3 Si3 120.9(8) . . ? Si4 N3 Sn1 113.6(6) . . ? Si3 N3 Sn1 124.4(6) . . ? N1 C1 C2 126.1(15) . . ? N1 C1 C10 120.1(14) . . ? C2 C1 C10 113.8(14) . . ? C3 C2 C1 132.4(15) . . ? N2 C3 C2 128.2(14) . . ? N2 C3 C16 121.1(14) . . ? C2 C3 C16 110.7(14) . . ? C11 C10 C15 117.3(15) . . ? C11 C10 C1 123.3(15) . . ? C15 C10 C1 119.4(15) . . ? C12 C11 C10 121.6(17) . . ? C11 C12 C13 122(2) . . ? C14 C13 C12 117.2(17) . . ? C15 C14 C13 121.2(18) . . ? C14 C15 C10 120.4(19) . . ? C17 C16 C21 122.1(19) . . ? C17 C16 C3 117.7(18) . . ? C21 C16 C3 119.9(18) . . ? C16 C17 C18 117(2) . . ? C19 C18 C17 120(3) . . ? C20 C19 C18 121(3) . . ? C19 C20 C21 121(3) . . ? C16 C21 C20 119(3) . . ? N6 Sn2 N5 100.6(5) . . ? N6 Sn2 N4 98.8(5) . . ? N5 Sn2 N4 90.4(4) . . ? N4 Si5 C31 106.7(8) . . ? N4 Si5 C32 116.3(7) . . ? C31 Si5 C32 106.7(9) . . ? N4 Si5 C33 108.2(9) . . ? C31 Si5 C33 110.7(10) . . ? C32 Si5 C33 108.3(10) . . ? N5 Si6 C35 110.7(9) . . ? N5 Si6 C36 117.4(9) . . ? C35 Si6 C36 112.5(13) . . ? N5 Si6 C34 105.9(8) . . ? C35 Si6 C34 105.4(12) . . ? C36 Si6 C34 103.7(12) . . ? N6 Si7 C50 112.0(8) . . ? N6 Si7 C49 114.4(8) . . ? C50 Si7 C49 106.5(8) . . ? N6 Si7 C51 112.2(9) . . ? C50 Si7 C51 107.2(10) . . ? C49 Si7 C51 104.0(9) . . ? N6 Si8 C54 112.9(10) . . ? N6 Si8 C52 111.4(9) . . ? C54 Si8 C52 106.3(11) . . ? N6 Si8 C53 112.6(8) . . ? C54 Si8 C53 106.0(12) . . ? C52 Si8 C53 107.2(9) . . ? C28 N4 Si5 123.0(11) . . ? C28 N4 Sn2 120.5(10) . . ? Si5 N4 Sn2 113.8(6) . . ? C30 N5 Si6 123.9(13) . . ? C30 N5 Sn2 122.4(11) . . ? Si6 N5 Sn2 113.7(7) . . ? Si7 N6 Si8 119.3(10) . . ? Si7 N6 Sn2 125.8(8) . . ? Si8 N6 Sn2 114.5(7) . . ? N4 C28 C29 128.0(14) . . ? N4 C28 C37 119.8(13) . . ? C29 C28 C37 112.1(13) . . ? C28 C29 C30 132.0(15) . . ? N5 C30 C29 125.6(15) . . ? N5 C30 C43 122.3(16) . . ? C29 C30 C43 112.1(14) . . ? C42 C37 C38 118.1(19) . . ? C42 C37 C28 120.1(18) . . ? C38 C37 C28 121.6(15) . . ? C37 C38 C39 121.9(19) . . ? C40 C39 C38 117(2) . . ? C41 C40 C39 123(2) . . ? C40 C41 C42 117(2) . . ? C37 C42 C41 122(2) . . ? C44 C43 C48 116.9(19) . . ? C44 C43 C30 119.4(17) . . ? C48 C43 C30 123.4(18) . . ? C43 C44 C45 123(2) . . ? C46 C45 C44 120(3) . . ? C45 C46 C47 120(3) . . ? C46 C47 C48 118(3) . . ? C43 C48 C47 121(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.400 _refine_diff_density_min -1.627 _refine_diff_density_rms 0.138 #===END data_(11)-jan1897 _database_code_depnum_ccdc_archive 'CCDC 247922' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H47 N3 S Si4 Sn' _chemical_formula_weight 676.79 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' S S 0.1246 0.1234 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 18.795(5) _cell_length_b 8.974(6) _cell_length_c 21.617(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.82(2) _cell_angle_gamma 90.00 _cell_volume 3508(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.944 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details psi-scans _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 'Nonius CAD4' _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6338 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 24.97 _reflns_number_total 6149 _reflns_number_gt 4256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4 software' _computing_cell_refinement 'Nonius CAD4 software' _computing_data_reduction 'Nonius CAD4 software' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+1.4106P] 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 6149 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Sn Sn 0.027548(15) 0.24484(3) 0.777622(13) 0.03536(9) Uani 1 1 d . . . S S 0.01753(8) 0.00374(13) 0.74699(8) 0.0652(4) Uani 1 1 d . . . Si1 Si 0.03918(7) 0.34984(14) 0.63261(6) 0.0422(3) Uani 1 1 d . . . Si2 Si -0.06575(9) 0.20256(17) 0.88851(7) 0.0618(4) Uani 1 1 d . . . Si3 Si 0.11899(7) 0.54505(14) 0.84150(6) 0.0437(3) Uani 1 1 d . . . Si4 Si 0.20066(7) 0.25407(17) 0.87025(7) 0.0594(4) Uani 1 1 d . . . N1 N -0.00467(17) 0.3847(3) 0.69576(15) 0.0330(7) Uani 1 1 d . . . N2 N -0.06194(19) 0.2999(4) 0.81660(16) 0.0410(9) Uani 1 1 d . . . N3 N 0.11822(18) 0.3493(4) 0.83552(16) 0.0400(8) Uani 1 1 d . . . C1 C -0.0684(2) 0.4606(4) 0.68618(19) 0.0356(9) Uani 1 1 d . . . C2 C -0.1174(2) 0.4588(5) 0.7239(2) 0.0470(11) Uani 1 1 d . . . H2 H -0.1600 0.5146 0.7071 0.056 Uiso 1 1 calc R . . C3 C -0.1151(2) 0.3889(5) 0.7823(2) 0.0424(10) Uani 1 1 d . . . C4 C -0.0906(2) 0.5666(5) 0.63109(19) 0.0381(10) Uani 1 1 d . . . C5 C -0.0547(3) 0.7005(5) 0.6338(2) 0.0540(13) Uani 1 1 d . . . H5 H -0.0150 0.7222 0.6690 0.065 Uiso 1 1 calc R . . C6 C -0.0768(4) 0.8034(6) 0.5849(3) 0.0720(16) Uani 1 1 d . . . H6 H -0.0521 0.8940 0.5877 0.086 Uiso 1 1 calc R . . C7 C -0.1340(4) 0.7736(7) 0.5329(3) 0.0787(19) Uani 1 1 d . . . H7 H -0.1479 0.8423 0.4996 0.094 Uiso 1 1 calc R . . C8 C -0.1707(3) 0.6426(8) 0.5299(3) 0.0830(19) Uani 1 1 d . . . H8 H -0.2104 0.6225 0.4944 0.100 Uiso 1 1 calc R . . C9 C -0.1501(3) 0.5381(6) 0.5786(2) 0.0594(13) Uani 1 1 d . . . H9 H -0.1762 0.4492 0.5761 0.071 Uiso 1 1 calc R . . C10 C -0.1801(3) 0.4301(6) 0.8069(2) 0.0553(13) Uani 1 1 d . . . C11 C -0.1762(3) 0.5539(7) 0.8445(3) 0.0811(18) Uani 1 1 d . . . H11 H -0.1322 0.6071 0.8577 0.097 Uiso 1 1 calc R . . C12 C -0.2385(4) 0.6008(9) 0.8632(3) 0.105(2) Uani 1 1 d . . . H12 H -0.2354 0.6829 0.8900 0.126 Uiso 1 1 calc R . . C13 C -0.3031(4) 0.5256(10) 0.8419(4) 0.113(3) Uani 1 1 d . . . H13 H -0.3448 0.5579 0.8532 0.136 Uiso 1 1 calc R . . C14 C -0.3070(4) 0.4048(10) 0.8044(4) 0.117(3) Uani 1 1 d . . . H14 H -0.3514 0.3528 0.7907 0.140 Uiso 1 1 calc R . . C15 C -0.2461(3) 0.3573(8) 0.7863(3) 0.087(2) Uani 1 1 d . . . H15 H -0.2499 0.2745 0.7597 0.105 Uiso 1 1 calc R . . C16 C 0.1281(3) 0.2562(6) 0.6704(3) 0.0718(15) Uani 1 1 d . . . H16A H 0.1595 0.3224 0.7009 0.108 Uiso 1 1 calc R . . H16B H 0.1519 0.2298 0.6379 0.108 Uiso 1 1 calc R . . H16C H 0.1191 0.1678 0.6922 0.108 Uiso 1 1 calc R . . C17 C 0.0622(3) 0.5149(6) 0.5901(2) 0.0608(14) Uani 1 1 d . . . H17A H 0.0176 0.5672 0.5691 0.091 Uiso 1 1 calc R . . H17B H 0.0865 0.4831 0.5586 0.091 Uiso 1 1 calc R . . H17C H 0.0944 0.5798 0.6205 0.091 Uiso 1 1 calc R . . C18 C -0.0239(3) 0.2264(6) 0.5734(2) 0.0703(16) Uani 1 1 d . . . H18A H -0.0692 0.2782 0.5543 0.105 Uiso 1 1 calc R . . H18B H -0.0342 0.1386 0.5948 0.105 Uiso 1 1 calc R . . H18C H -0.0009 0.1985 0.5406 0.105 Uiso 1 1 calc R . . C19 C -0.1407(5) 0.0684(13) 0.8725(5) 0.239(7) Uani 1 1 d . . . H19A H -0.1363 0.0019 0.8390 0.359 Uiso 1 1 calc R . . H19B H -0.1872 0.1200 0.8593 0.359 Uiso 1 1 calc R . . H19C H -0.1384 0.0124 0.9109 0.359 Uiso 1 1 calc R . . C20 C -0.0732(7) 0.3269(10) 0.9515(3) 0.225(7) Uani 1 1 d . . . H20A H -0.1181 0.3834 0.9375 0.338 Uiso 1 1 calc R . . H20B H -0.0317 0.3935 0.9617 0.338 Uiso 1 1 calc R . . H20C H -0.0739 0.2702 0.9890 0.338 Uiso 1 1 calc R . . C21 C 0.0201(4) 0.0984(11) 0.9168(4) 0.170(5) Uani 1 1 d . . . H21A H 0.0255 0.0316 0.8837 0.255 Uiso 1 1 calc R . . H21B H 0.0191 0.0422 0.9543 0.255 Uiso 1 1 calc R . . H21C H 0.0611 0.1664 0.9273 0.255 Uiso 1 1 calc R . . C22 C 0.1482(3) 0.6333(5) 0.7749(2) 0.0629(14) Uani 1 1 d . . . H22A H 0.1954 0.5941 0.7738 0.094 Uiso 1 1 calc R . . H22B H 0.1521 0.7391 0.7815 0.094 Uiso 1 1 calc R . . H22C H 0.1123 0.6124 0.7348 0.094 Uiso 1 1 calc R . . C23 C 0.1835(3) 0.6116(6) 0.9182(3) 0.0801(18) Uani 1 1 d . . . H23A H 0.2324 0.5751 0.9215 0.120 Uiso 1 1 calc R . . H23B H 0.1672 0.5754 0.9539 0.120 Uiso 1 1 calc R . . H23C H 0.1840 0.7186 0.9188 0.120 Uiso 1 1 calc R . . C24 C 0.0282(3) 0.6239(5) 0.8420(3) 0.0594(13) Uani 1 1 d . . . H24A H 0.0121 0.5799 0.8764 0.089 Uiso 1 1 calc R . . H24B H -0.0073 0.6031 0.8018 0.089 Uiso 1 1 calc R . . H24C H 0.0327 0.7298 0.8483 0.089 Uiso 1 1 calc R . . C25 C 0.2201(4) 0.2464(8) 0.9599(3) 0.116(3) Uani 1 1 d . . . H25A H 0.2210 0.3458 0.9766 0.174 Uiso 1 1 calc R . . H25B H 0.2671 0.1997 0.9779 0.174 Uiso 1 1 calc R . . H25C H 0.1820 0.1899 0.9712 0.174 Uiso 1 1 calc R . . C26 C 0.2809(3) 0.3473(7) 0.8509(3) 0.090(2) Uani 1 1 d . . . H26A H 0.2836 0.4492 0.8648 0.135 Uiso 1 1 calc R . . H26B H 0.2745 0.3439 0.8053 0.135 Uiso 1 1 calc R . . H26C H 0.3257 0.2967 0.8725 0.135 Uiso 1 1 calc R . . C27 C 0.2003(3) 0.0575(6) 0.8425(3) 0.0806(18) Uani 1 1 d . . . H27A H 0.1601 0.0047 0.8519 0.121 Uiso 1 1 calc R . . H27B H 0.2462 0.0106 0.8642 0.121 Uiso 1 1 calc R . . H27C H 0.1943 0.0560 0.7969 0.121 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 Sn 0.03961(15) 0.02753(14) 0.03959(15) 0.00223(15) 0.01189(11) 0.00120(15) S 0.0717(9) 0.0284(6) 0.0920(10) -0.0076(7) 0.0163(8) -0.0030(6) Si1 0.0487(7) 0.0400(7) 0.0423(7) -0.0007(6) 0.0198(6) 0.0035(6) Si2 0.0757(10) 0.0625(10) 0.0570(9) 0.0169(7) 0.0345(8) 0.0024(8) Si3 0.0435(7) 0.0366(7) 0.0488(7) -0.0085(6) 0.0086(6) -0.0026(6) Si4 0.0510(7) 0.0520(8) 0.0634(8) 0.0007(8) -0.0046(6) 0.0138(8) N1 0.0365(18) 0.0277(17) 0.0353(18) 0.0020(15) 0.0104(15) 0.0031(15) N2 0.044(2) 0.040(2) 0.043(2) 0.0050(16) 0.0181(17) -0.0026(16) N3 0.040(2) 0.036(2) 0.040(2) 0.0008(16) 0.0046(16) 0.0030(16) C1 0.036(2) 0.032(2) 0.037(2) -0.0005(18) 0.0077(18) -0.0005(19) C2 0.037(2) 0.054(3) 0.051(3) 0.006(2) 0.012(2) 0.013(2) C3 0.039(2) 0.044(3) 0.047(3) -0.006(2) 0.017(2) -0.006(2) C4 0.039(2) 0.037(2) 0.039(2) 0.003(2) 0.0128(19) 0.008(2) C5 0.069(3) 0.040(3) 0.053(3) -0.001(2) 0.015(3) 0.000(2) C6 0.105(5) 0.035(3) 0.079(4) 0.015(3) 0.029(4) 0.006(3) C7 0.102(5) 0.073(5) 0.061(4) 0.030(3) 0.023(3) 0.042(4) C8 0.076(4) 0.103(5) 0.055(3) 0.018(4) -0.007(3) 0.028(4) C9 0.057(3) 0.062(3) 0.050(3) 0.005(3) 0.000(2) 0.003(3) C10 0.049(3) 0.065(3) 0.060(3) 0.009(3) 0.029(2) 0.009(3) C11 0.069(4) 0.089(5) 0.096(4) -0.015(4) 0.042(3) 0.009(3) C12 0.116(6) 0.109(6) 0.117(6) -0.018(5) 0.076(5) 0.024(5) C13 0.088(5) 0.134(7) 0.147(7) 0.022(6) 0.080(6) 0.032(5) C14 0.063(4) 0.144(8) 0.164(8) -0.005(6) 0.066(5) -0.018(5) C15 0.059(4) 0.094(5) 0.122(5) -0.015(4) 0.046(4) -0.012(3) C16 0.066(3) 0.087(4) 0.075(3) 0.021(3) 0.039(3) 0.032(3) C17 0.069(3) 0.062(3) 0.059(3) 0.007(3) 0.030(3) -0.004(3) C18 0.100(4) 0.054(4) 0.062(3) -0.018(3) 0.030(3) -0.013(3) C19 0.193(10) 0.274(14) 0.208(11) 0.154(10) -0.020(8) -0.142(10) C20 0.50(2) 0.126(7) 0.064(5) 0.019(5) 0.097(9) 0.090(11) C21 0.148(7) 0.249(11) 0.139(7) 0.142(8) 0.082(6) 0.102(8) C22 0.071(3) 0.043(3) 0.080(4) -0.002(3) 0.030(3) -0.007(3) C23 0.082(4) 0.071(4) 0.073(4) -0.028(3) -0.003(3) -0.001(3) C24 0.059(3) 0.034(3) 0.088(4) -0.010(3) 0.024(3) 0.005(2) C25 0.132(6) 0.117(6) 0.070(4) 0.017(4) -0.022(4) 0.034(5) C26 0.046(3) 0.077(4) 0.141(6) -0.014(4) 0.015(4) 0.011(3) C27 0.063(4) 0.049(3) 0.117(5) 0.008(3) 0.004(3) 0.024(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 Sn N3 2.046(3) . ? Sn N1 2.119(3) . ? Sn N2 2.134(3) . ? Sn S 2.2555(19) . ? Si1 N1 1.804(3) . ? Si1 C16 1.850(5) . ? Si1 C18 1.855(5) . ? Si1 C17 1.855(5) . ? Si2 C20 1.796(8) . ? Si2 N2 1.801(4) . ? Si2 C19 1.814(8) . ? Si2 C21 1.820(7) . ? Si3 N3 1.761(4) . ? Si3 C24 1.851(5) . ? Si3 C22 1.854(5) . ? Si3 C23 1.865(5) . ? Si4 N3 1.749(3) . ? Si4 C27 1.862(6) . ? Si4 C26 1.869(6) . ? Si4 C25 1.873(6) . ? N1 C1 1.344(5) . ? N2 C3 1.335(5) . ? C1 C2 1.387(5) . ? C1 C4 1.492(5) . ? C2 C3 1.401(6) . ? C3 C10 1.505(6) . ? C4 C5 1.372(6) . ? C4 C9 1.383(6) . ? C5 C6 1.379(7) . ? C6 C7 1.353(8) . ? C7 C8 1.356(8) . ? C8 C9 1.385(7) . ? C10 C15 1.364(7) . ? C10 C11 1.367(7) . ? C11 C12 1.403(7) . ? C12 C13 1.355(10) . ? C13 C14 1.343(10) . ? C14 C15 1.376(8) . ? 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 Sn N1 103.90(13) . . ? N3 Sn N2 105.49(14) . . ? N1 Sn N2 96.67(13) . . ? N3 Sn S 127.44(10) . . ? N1 Sn S 109.94(10) . . ? N2 Sn S 109.03(10) . . ? N1 Si1 C16 106.76(19) . . ? N1 Si1 C18 106.7(2) . . ? C16 Si1 C18 111.3(3) . . ? N1 Si1 C17 116.9(2) . . ? C16 Si1 C17 106.1(2) . . ? C18 Si1 C17 109.1(2) . . ? C20 Si2 N2 112.5(3) . . ? C20 Si2 C19 109.8(6) . . ? N2 Si2 C19 111.7(3) . . ? C20 Si2 C21 108.0(5) . . ? N2 Si2 C21 107.4(2) . . ? C19 Si2 C21 107.2(5) . . ? N3 Si3 C24 113.1(2) . . ? N3 Si3 C22 111.5(2) . . ? C24 Si3 C22 108.1(2) . . ? N3 Si3 C23 112.0(2) . . ? C24 Si3 C23 104.4(3) . . ? C22 Si3 C23 107.2(3) . . ? N3 Si4 C27 113.5(2) . . ? N3 Si4 C26 111.1(2) . . ? C27 Si4 C26 106.5(3) . . ? N3 Si4 C25 111.2(3) . . ? C27 Si4 C25 106.3(3) . . ? C26 Si4 C25 107.9(3) . . ? C1 N1 Si1 122.9(3) . . ? C1 N1 Sn 118.0(3) . . ? Si1 N1 Sn 116.35(16) . . ? C3 N2 Si2 124.7(3) . . ? C3 N2 Sn 118.0(3) . . ? Si2 N2 Sn 116.72(18) . . ? Si4 N3 Si3 117.8(2) . . ? Si4 N3 Sn 122.10(19) . . ? Si3 N3 Sn 119.38(18) . . ? N1 C1 C2 127.7(4) . . ? N1 C1 C4 119.3(3) . . ? C2 C1 C4 112.9(4) . . ? C1 C2 C3 132.2(4) . . ? N2 C3 C2 127.2(4) . . ? N2 C3 C10 120.5(4) . . ? C2 C3 C10 112.3(4) . . ? C5 C4 C9 118.4(4) . . ? C5 C4 C1 119.8(4) . . ? C9 C4 C1 121.6(4) . . ? C4 C5 C6 120.8(5) . . ? C7 C6 C5 120.6(5) . . ? C6 C7 C8 119.4(5) . . ? C7 C8 C9 121.1(6) . . ? C4 C9 C8 119.6(5) . . ? C15 C10 C11 118.7(5) . . ? C15 C10 C3 121.4(5) . . ? C11 C10 C3 119.5(5) . . ? C10 C11 C12 120.1(6) . . ? C13 C12 C11 119.5(7) . . ? C14 C13 C12 120.3(7) . . ? C13 C14 C15 120.5(7) . . ? C10 C15 C14 120.8(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.671 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.068 #===END