Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jason Clyburne' _publ_contact_author_address ; Department of Chemistry Saint Mary's University 923 Robie Street Halifax Nova Scotia B3H3 C3 CANADA ; _publ_contact_author_email JASON.CLYBURNE@SMU.CA _publ_section_title ; Flexible coordination of the carboxylate ligand in tin(II) amides and a 1,3-diaza-2,4-distannacyclobutanediyl ; loop_ _publ_author_name 'Jason Clyburne' 'Guy M. Bernard' 'Diane A. Dickie' 'Ojisamola A. Labeodan' 'Peter T. K. Lee' ; A.R.Lewis ; 'Gabriele Schatte' 'R. Wasylishen' 'Noham Weinberg' #===END # CHEMICAL DATA data_7 _database_code_depnum_ccdc_archive 'CCDC 618666' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H38 Cl2 N2 Si4 Sn' _chemical_formula_weight 524.40 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' Cl Cl 0.1484 0.1585 '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 8.55900(10) _cell_length_b 11.3010(2) _cell_length_c 14.9150(3) _cell_angle_alpha 105.9710(12) _cell_angle_beta 96.8970(13) _cell_angle_gamma 108.9690(14) _cell_volume 1276.35(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 1.397 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7674 _exptl_absorpt_correction_T_max 0.8178 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10241 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.87 _reflns_number_total 6077 _reflns_number_gt 5637 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+1.0619P] 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 6077 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.660437(16) 0.444566(13) 0.676384(9) 0.01975(4) Uani 1 1 d . . . Cl1 Cl 0.40699(7) 0.46073(6) 0.60783(4) 0.03341(12) Uani 1 1 d . . . Cl2 Cl 0.89580(8) 0.31199(7) 0.55721(5) 0.04357(14) Uani 1 1 d . . . Si1 Si 0.40259(7) 0.15310(6) 0.66031(4) 0.02709(12) Uani 1 1 d . . . Si2 Si 0.74804(7) 0.27366(6) 0.80546(4) 0.02450(12) Uani 1 1 d . . . Si3 Si 0.67367(8) 0.67176(6) 0.86936(4) 0.02814(12) Uani 1 1 d . . . Si4 Si 0.94925(8) 0.73847(6) 0.75618(4) 0.02794(13) Uani 1 1 d . . . N1 N 0.5977(2) 0.28342(16) 0.72001(12) 0.0214(3) Uani 1 1 d . . . N2 N 0.7790(2) 0.62411(16) 0.78056(12) 0.0245(3) Uani 1 1 d . . . C1 C 0.7646(3) 0.4053(2) 0.55146(16) 0.0303(5) Uani 1 1 d . . . H1A H 0.6703 0.3558 0.4937 0.036 Uiso 1 1 calc R . . H1B H 0.8322 0.4908 0.5449 0.036 Uiso 1 1 calc R . . C11 C 0.3718(4) 0.1160(2) 0.52807(17) 0.0414(6) Uani 1 1 d . . . H11A H 0.3500 0.1880 0.5112 0.050 Uiso 1 1 calc R . . H11B H 0.2749 0.0323 0.4951 0.050 Uiso 1 1 calc R . . H11C H 0.4744 0.1082 0.5085 0.050 Uiso 1 1 calc R . . C12 C 0.3908(3) -0.0042(2) 0.6827(2) 0.0420(6) Uani 1 1 d . . . H12A H 0.4743 -0.0353 0.6549 0.050 Uiso 1 1 calc R . . H12B H 0.2767 -0.0720 0.6531 0.050 Uiso 1 1 calc R . . H12C H 0.4154 0.0123 0.7519 0.050 Uiso 1 1 calc R . . C13 C 0.2208(3) 0.1909(3) 0.6999(2) 0.0496(7) Uani 1 1 d . . . H13A H 0.2357 0.2084 0.7691 0.060 Uiso 1 1 calc R . . H13B H 0.1148 0.1149 0.6661 0.060 Uiso 1 1 calc R . . H13C H 0.2162 0.2693 0.6852 0.060 Uiso 1 1 calc R . . C21 C 0.8047(3) 0.1252(2) 0.76076(19) 0.0373(5) Uani 1 1 d . . . H21A H 0.7155 0.0466 0.7635 0.045 Uiso 1 1 calc R . . H21B H 0.9128 0.1391 0.8009 0.045 Uiso 1 1 calc R . . H21C H 0.8154 0.1120 0.6944 0.045 Uiso 1 1 calc R . . C22 C 0.6687(4) 0.2690(3) 0.91593(19) 0.0510(7) Uani 1 1 d . . . H22A H 0.6578 0.3536 0.9467 0.061 Uiso 1 1 calc R . . H22B H 0.7490 0.2545 0.9603 0.061 Uiso 1 1 calc R . . H22C H 0.5577 0.1966 0.8989 0.061 Uiso 1 1 calc R . . C23 C 0.9524(3) 0.4194(2) 0.8379(2) 0.0438(6) Uani 1 1 d . . . H23A H 0.9948 0.4228 0.7801 0.053 Uiso 1 1 calc R . . H23B H 1.0361 0.4106 0.8840 0.053 Uiso 1 1 calc R . . H23C H 0.9335 0.5012 0.8667 0.053 Uiso 1 1 calc R . . C31 C 0.4760(3) 0.5322(3) 0.86124(19) 0.0406(6) Uani 1 1 d . . . H31A H 0.3928 0.5114 0.8024 0.049 Uiso 1 1 calc R . . H31B H 0.4287 0.5580 0.9168 0.049 Uiso 1 1 calc R . . H31C H 0.5024 0.4538 0.8602 0.049 Uiso 1 1 calc R . . C32 C 0.8108(4) 0.7224(3) 0.99114(18) 0.0499(7) Uani 1 1 d . . . H32A H 0.8393 0.6477 0.9982 0.060 Uiso 1 1 calc R . . H32B H 0.7497 0.7484 1.0398 0.060 Uiso 1 1 calc R . . H32C H 0.9153 0.7976 0.9993 0.060 Uiso 1 1 calc R . . C33 C 0.6091(4) 0.8110(3) 0.8581(2) 0.0464(6) Uani 1 1 d . . . H33A H 0.7107 0.8908 0.8713 0.056 Uiso 1 1 calc R . . H33B H 0.5400 0.8287 0.9041 0.056 Uiso 1 1 calc R . . H33C H 0.5428 0.7863 0.7929 0.056 Uiso 1 1 calc R . . C41 C 1.1137(3) 0.6692(3) 0.7254(2) 0.0440(6) Uani 1 1 d . . . H41A H 1.1663 0.6548 0.7815 0.053 Uiso 1 1 calc R . . H41B H 1.2007 0.7318 0.7060 0.053 Uiso 1 1 calc R . . H41C H 1.0604 0.5844 0.6726 0.053 Uiso 1 1 calc R . . C42 C 1.0616(4) 0.8916(3) 0.8629(2) 0.0513(7) Uani 1 1 d . . . H42A H 0.9808 0.9322 0.8833 0.062 Uiso 1 1 calc R . . H42B H 1.1525 0.9547 0.8462 0.062 Uiso 1 1 calc R . . H42C H 1.1104 0.8683 0.9153 0.062 Uiso 1 1 calc R . . C43 C 0.8681(3) 0.7865(2) 0.65562(18) 0.0372(5) Uani 1 1 d . . . H43A H 0.8079 0.7068 0.5993 0.045 Uiso 1 1 calc R . . H43B H 0.9636 0.8472 0.6401 0.045 Uiso 1 1 calc R . . H43C H 0.7901 0.8308 0.6746 0.045 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 0.02026(7) 0.02026(7) 0.02070(7) 0.00835(5) 0.00503(5) 0.00874(5) Cl1 0.0300(3) 0.0402(3) 0.0336(3) 0.0146(2) 0.0006(2) 0.0182(2) Cl2 0.0483(4) 0.0484(4) 0.0476(3) 0.0154(3) 0.0208(3) 0.0323(3) Si1 0.0225(3) 0.0242(3) 0.0314(3) 0.0089(2) 0.0066(2) 0.0050(2) Si2 0.0278(3) 0.0258(3) 0.0250(3) 0.0121(2) 0.0064(2) 0.0134(2) Si3 0.0372(3) 0.0253(3) 0.0236(3) 0.0063(2) 0.0067(2) 0.0153(2) Si4 0.0261(3) 0.0206(3) 0.0336(3) 0.0104(2) 0.0025(2) 0.0050(2) N1 0.0226(8) 0.0201(8) 0.0233(8) 0.0101(7) 0.0060(6) 0.0077(6) N2 0.0270(9) 0.0190(8) 0.0255(8) 0.0067(7) 0.0029(7) 0.0076(7) C1 0.0346(12) 0.0364(12) 0.0287(11) 0.0142(9) 0.0145(9) 0.0190(10) C11 0.0511(15) 0.0307(12) 0.0314(12) 0.0034(10) -0.0032(11) 0.0117(11) C12 0.0400(14) 0.0293(12) 0.0494(15) 0.0177(11) 0.0078(11) 0.0010(10) C13 0.0255(12) 0.0483(16) 0.0676(19) 0.0127(14) 0.0166(12) 0.0080(11) C21 0.0359(12) 0.0351(12) 0.0515(15) 0.0195(11) 0.0142(11) 0.0210(10) C22 0.0691(19) 0.073(2) 0.0306(13) 0.0251(14) 0.0205(13) 0.0421(17) C23 0.0353(13) 0.0315(12) 0.0574(16) 0.0180(12) -0.0118(11) 0.0085(10) C31 0.0473(15) 0.0366(13) 0.0403(13) 0.0092(11) 0.0239(11) 0.0169(11) C32 0.0655(19) 0.0542(17) 0.0268(12) 0.0102(12) 0.0037(12) 0.0237(14) C33 0.0558(17) 0.0391(14) 0.0555(16) 0.0167(13) 0.0175(13) 0.0296(13) C41 0.0248(11) 0.0367(13) 0.0745(19) 0.0263(13) 0.0141(12) 0.0092(10) C42 0.0446(15) 0.0337(14) 0.0503(16) 0.0046(12) -0.0008(12) -0.0055(11) C43 0.0438(14) 0.0317(12) 0.0421(13) 0.0209(11) 0.0113(11) 0.0139(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 2.0270(17) . ? Sn1 N1 2.0318(16) . ? Sn1 C1 2.160(2) . ? Sn1 Cl1 2.3689(5) . ? Cl2 C1 1.782(2) . ? Si1 N1 1.7530(17) . ? Si1 C13 1.862(3) . ? Si1 C11 1.867(3) . ? Si1 C12 1.871(3) . ? Si2 N1 1.7516(17) . ? Si2 C22 1.863(3) . ? Si2 C21 1.867(2) . ? Si2 C23 1.869(3) . ? Si3 N2 1.7508(19) . ? Si3 C31 1.864(3) . ? Si3 C32 1.866(3) . ? Si3 C33 1.870(3) . ? Si4 N2 1.7574(18) . ? Si4 C43 1.863(2) . ? Si4 C41 1.865(3) . ? Si4 C42 1.868(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Sn1 N1 116.50(7) . . ? N2 Sn1 C1 117.81(8) . . ? N1 Sn1 C1 109.66(8) . . ? N2 Sn1 Cl1 102.34(5) . . ? N1 Sn1 Cl1 108.49(5) . . ? C1 Sn1 Cl1 99.94(6) . . ? N1 Si1 C13 112.08(11) . . ? N1 Si1 C11 110.28(10) . . ? C13 Si1 C11 109.47(14) . . ? N1 Si1 C12 112.06(10) . . ? C13 Si1 C12 106.21(13) . . ? C11 Si1 C12 106.51(12) . . ? N1 Si2 C22 110.58(11) . . ? N1 Si2 C21 112.96(10) . . ? C22 Si2 C21 108.46(13) . . ? N1 Si2 C23 110.64(9) . . ? C22 Si2 C23 108.93(15) . . ? C21 Si2 C23 105.06(12) . . ? N2 Si3 C31 111.53(10) . . ? N2 Si3 C32 110.62(12) . . ? C31 Si3 C32 106.66(13) . . ? N2 Si3 C33 111.53(11) . . ? C31 Si3 C33 106.77(13) . . ? C32 Si3 C33 109.53(14) . . ? N2 Si4 C43 109.43(10) . . ? N2 Si4 C41 111.70(10) . . ? C43 Si4 C41 109.85(13) . . ? N2 Si4 C42 111.55(11) . . ? C43 Si4 C42 108.65(13) . . ? C41 Si4 C42 105.56(14) . . ? Si2 N1 Si1 123.22(9) . . ? Si2 N1 Sn1 118.94(9) . . ? Si1 N1 Sn1 117.49(9) . . ? Si3 N2 Si4 122.74(10) . . ? Si3 N2 Sn1 118.44(9) . . ? Si4 N2 Sn1 116.17(9) . . ? Cl2 C1 Sn1 112.76(11) . . ? Cl2 C1 H1A 109.0 . . ? Sn1 C1 H1A 109.0 . . ? Cl2 C1 H1B 109.0 . . ? Sn1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si3 C33 H33A 109.5 . . ? Si3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si4 C41 H41A 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si4 C42 H42A 109.5 . . ? Si4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si4 C43 H43A 109.5 . . ? Si4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C22 Si2 N1 Si1 -68.63(16) . . . . ? C21 Si2 N1 Si1 53.13(15) . . . . ? C23 Si2 N1 Si1 170.59(13) . . . . ? C22 Si2 N1 Sn1 118.31(14) . . . . ? C21 Si2 N1 Sn1 -119.93(11) . . . . ? C23 Si2 N1 Sn1 -2.47(15) . . . . ? C13 Si1 N1 Si2 109.54(15) . . . . ? C11 Si1 N1 Si2 -128.23(13) . . . . ? C12 Si1 N1 Si2 -9.77(16) . . . . ? C13 Si1 N1 Sn1 -77.31(14) . . . . ? C11 Si1 N1 Sn1 44.93(14) . . . . ? C12 Si1 N1 Sn1 163.39(11) . . . . ? N2 Sn1 N1 Si2 -45.29(12) . . . . ? C1 Sn1 N1 Si2 91.73(11) . . . . ? Cl1 Sn1 N1 Si2 -160.04(8) . . . . ? N2 Sn1 N1 Si1 141.25(9) . . . . ? C1 Sn1 N1 Si1 -81.73(11) . . . . ? Cl1 Sn1 N1 Si1 26.51(10) . . . . ? C31 Si3 N2 Si4 169.37(13) . . . . ? C32 Si3 N2 Si4 -72.09(15) . . . . ? C33 Si3 N2 Si4 50.08(16) . . . . ? C31 Si3 N2 Sn1 8.54(15) . . . . ? C32 Si3 N2 Sn1 127.08(13) . . . . ? C33 Si3 N2 Sn1 -110.75(13) . . . . ? C43 Si4 N2 Si3 -95.06(14) . . . . ? C41 Si4 N2 Si3 143.07(14) . . . . ? C42 Si4 N2 Si3 25.19(17) . . . . ? C43 Si4 N2 Sn1 66.17(13) . . . . ? C41 Si4 N2 Sn1 -55.69(14) . . . . ? C42 Si4 N2 Sn1 -173.58(12) . . . . ? N1 Sn1 N2 Si3 -59.89(12) . . . . ? C1 Sn1 N2 Si3 166.65(9) . . . . ? Cl1 Sn1 N2 Si3 58.27(10) . . . . ? N1 Sn1 N2 Si4 138.04(9) . . . . ? C1 Sn1 N2 Si4 4.57(13) . . . . ? Cl1 Sn1 N2 Si4 -103.80(9) . . . . ? N2 Sn1 C1 Cl2 98.30(12) . . . . ? N1 Sn1 C1 Cl2 -38.10(14) . . . . ? Cl1 Sn1 C1 Cl2 -151.96(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.486 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.072 data_4 _database_code_depnum_ccdc_archive 'CCDC 618667' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H74 Cl4 N2 O4 Si4 Sn2' _chemical_formula_weight 1426.79 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.429(2) _cell_length_b 13.276(3) _cell_length_c 14.405(3) _cell_angle_alpha 104.92(3) _cell_angle_beta 110.62(3) _cell_angle_gamma 101.70(3) _cell_volume 1706.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.225 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.125 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9299 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5990 _reflns_number_gt 5004 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.1919P] 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 5990 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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 -0.01688(2) 0.405316(16) 0.102391(18) 0.02212(8) Uani 1 1 d . . . O1 O 0.1389(2) 0.57698(15) 0.16818(17) 0.0254(5) Uani 1 1 d . . . O2 O -0.0105(2) 0.35679(16) -0.05342(17) 0.0252(5) Uani 1 1 d . . . N1 N 0.1513(3) 0.34563(19) 0.1619(2) 0.0245(6) Uani 1 1 d . . . Si1 Si 0.14689(10) 0.29936(8) 0.26324(8) 0.0330(2) Uani 1 1 d . . . Si2 Si 0.27382(9) 0.33032(7) 0.10855(8) 0.0295(2) Uani 1 1 d . . . C1 C 0.0986(3) 0.6540(2) 0.1444(3) 0.0206(7) Uani 1 1 d . . . C2 C 0.1567(3) 0.7660(2) 0.2305(2) 0.0209(7) Uani 1 1 d . . . C3 C 0.1165(3) 0.7820(2) 0.3145(2) 0.0224(7) Uani 1 1 d . . . C4 C 0.1730(3) 0.8868(2) 0.3936(2) 0.0235(7) Uani 1 1 d . . . H4A H 0.1466 0.8981 0.4513 0.028 Uiso 1 1 calc R . . C5 C 0.2675(3) 0.9753(2) 0.3897(3) 0.0233(7) Uani 1 1 d . . . C6 C 0.3039(3) 0.9567(2) 0.3052(3) 0.0241(7) Uani 1 1 d . . . H6A H 0.3682 1.0162 0.3018 0.029 Uiso 1 1 calc R . . C7 C 0.2498(3) 0.8536(2) 0.2240(2) 0.0217(7) Uani 1 1 d . . . C10 C 0.2961(3) 0.8405(2) 0.1368(3) 0.0228(7) Uani 1 1 d . . . C11 C 0.2780(3) 0.9089(3) 0.0778(3) 0.0331(8) Uani 1 1 d . . . H11A H 0.2301 0.9610 0.0909 0.040 Uiso 1 1 calc R . . C12 C 0.3285(4) 0.9024(3) 0.0005(3) 0.0401(9) Uani 1 1 d . . . H12A H 0.3153 0.9498 -0.0391 0.048 Uiso 1 1 calc R . . C13 C 0.3983(4) 0.8270(3) -0.0193(3) 0.0391(9) Uani 1 1 d . . . H13A H 0.4347 0.8232 -0.0716 0.047 Uiso 1 1 calc R . . C14 C 0.4148(3) 0.7571(3) 0.0371(3) 0.0365(9) Uani 1 1 d . . . H14A H 0.4609 0.7041 0.0226 0.044 Uiso 1 1 calc R . . C15 C 0.3645(3) 0.7640(2) 0.1148(3) 0.0290(8) Uani 1 1 d . . . H15A H 0.3769 0.7158 0.1535 0.035 Uiso 1 1 calc R . . C20 C 0.0137(3) 0.6932(2) 0.3230(3) 0.0241(7) Uani 1 1 d . . . C21 C 0.0465(4) 0.6741(3) 0.4176(3) 0.0327(8) Uani 1 1 d . . . H21A H 0.1367 0.7166 0.4769 0.039 Uiso 1 1 calc R . . C22 C -0.0510(4) 0.5937(3) 0.4264(3) 0.0392(9) Uani 1 1 d . . . H22A H -0.0277 0.5818 0.4918 0.047 Uiso 1 1 calc R . . C23 C -0.1813(4) 0.5309(3) 0.3415(3) 0.0389(9) Uani 1 1 d . . . H23A H -0.2473 0.4751 0.3478 0.047 Uiso 1 1 calc R . . C24 C -0.2159(4) 0.5490(3) 0.2473(3) 0.0349(9) Uani 1 1 d . . . H24A H -0.3063 0.5059 0.1886 0.042 Uiso 1 1 calc R . . C25 C -0.1194(3) 0.6302(2) 0.2373(3) 0.0282(8) Uani 1 1 d . . . H25A H -0.1443 0.6427 0.1721 0.034 Uiso 1 1 calc R . . C30 C 0.3267(3) 1.0856(2) 0.4755(2) 0.0252(7) Uani 1 1 d . . . C31 C 0.2412(4) 1.1237(2) 0.5213(3) 0.0319(8) Uani 1 1 d . . . H31A H 0.1446 1.0787 0.4984 0.038 Uiso 1 1 calc R . . C32 C 0.2950(4) 1.2271(3) 0.6002(3) 0.0418(9) Uani 1 1 d . . . H32A H 0.2359 1.2519 0.6321 0.050 Uiso 1 1 calc R . . C33 C 0.4337(4) 1.2933(3) 0.6321(3) 0.0439(10) Uani 1 1 d . . . H33A H 0.4702 1.3644 0.6856 0.053 Uiso 1 1 calc R . . C34 C 0.5200(4) 1.2570(3) 0.5870(3) 0.0410(10) Uani 1 1 d . . . H34A H 0.6161 1.3029 0.6095 0.049 Uiso 1 1 calc R . . C35 C 0.4669(4) 1.1536(2) 0.5088(3) 0.0345(9) Uani 1 1 d . . . H35A H 0.5268 1.1289 0.4778 0.041 Uiso 1 1 calc R . . C40 C -0.0230(4) 0.3011(3) 0.2794(3) 0.0414(9) Uani 1 1 d . . . H40A H -0.0271 0.3764 0.2965 0.062 Uiso 1 1 calc R . . H40B H -0.0238 0.2751 0.3371 0.062 Uiso 1 1 calc R . . H40C H -0.1072 0.2526 0.2131 0.062 Uiso 1 1 calc R . . C41 C 0.1437(5) 0.1534(3) 0.2312(4) 0.0594(13) Uani 1 1 d . . . H41A H 0.2308 0.1476 0.2218 0.089 Uiso 1 1 calc R . . H41B H 0.0576 0.1067 0.1655 0.089 Uiso 1 1 calc R . . H41C H 0.1410 0.1292 0.2895 0.089 Uiso 1 1 calc R . . C42 C 0.2984(4) 0.3877(4) 0.3952(3) 0.0650(13) Uani 1 1 d . . . H42A H 0.3911 0.3900 0.3916 0.098 Uiso 1 1 calc R . . H42B H 0.2913 0.3570 0.4489 0.098 Uiso 1 1 calc R . . H42C H 0.2927 0.4625 0.4144 0.098 Uiso 1 1 calc R . . C50 C 0.3336(3) 0.4491(2) 0.0693(3) 0.0309(8) Uani 1 1 d . . . H50A H 0.3727 0.5180 0.1305 0.046 Uiso 1 1 calc R . . H50B H 0.2508 0.4518 0.0116 0.046 Uiso 1 1 calc R . . H50C H 0.4088 0.4398 0.0451 0.046 Uiso 1 1 calc R . . C51 C 0.4448(4) 0.3278(3) 0.2088(3) 0.0480(10) Uani 1 1 d . . . H51A H 0.4866 0.3957 0.2714 0.072 Uiso 1 1 calc R . . H51B H 0.5140 0.3222 0.1777 0.072 Uiso 1 1 calc R . . H51C H 0.4232 0.2641 0.2299 0.072 Uiso 1 1 calc R . . C52 C 0.1991(4) 0.1988(3) -0.0089(3) 0.0428(10) Uani 1 1 d . . . H52A H 0.1678 0.1365 0.0115 0.064 Uiso 1 1 calc R . . H52B H 0.2743 0.1896 -0.0331 0.064 Uiso 1 1 calc R . . H52C H 0.1163 0.2016 -0.0665 0.064 Uiso 1 1 calc R . . C60 C 0.6686(4) -0.0005(3) 0.2741(4) 0.0601(12) Uani 1 1 d . . . H60A H 0.6401 -0.0335 0.3211 0.072 Uiso 1 1 calc R . . H60B H 0.6035 -0.0491 0.1996 0.072 Uiso 1 1 calc R . . Cl1 Cl 0.84652(13) 0.00539(11) 0.29805(13) 0.0870(4) Uani 1 1 d . . . Cl2 Cl 0.64600(12) 0.12894(9) 0.29570(10) 0.0666(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02543(13) 0.02300(12) 0.02034(13) 0.00829(9) 0.01082(10) 0.01009(9) O1 0.0285(12) 0.0211(11) 0.0256(13) 0.0067(10) 0.0103(10) 0.0103(9) O2 0.0259(11) 0.0299(12) 0.0157(13) 0.0038(10) 0.0082(10) 0.0080(9) N1 0.0295(14) 0.0236(13) 0.0236(16) 0.0108(12) 0.0121(12) 0.0109(11) Si1 0.0424(6) 0.0366(5) 0.0291(6) 0.0197(5) 0.0162(5) 0.0192(4) Si2 0.0304(5) 0.0292(5) 0.0336(6) 0.0121(4) 0.0151(5) 0.0154(4) C1 0.0182(15) 0.0225(16) 0.0210(19) 0.0040(14) 0.0117(14) 0.0051(13) C2 0.0221(16) 0.0212(15) 0.0164(17) 0.0038(13) 0.0056(14) 0.0092(13) C3 0.0246(16) 0.0238(16) 0.0170(18) 0.0063(14) 0.0061(14) 0.0107(13) C4 0.0297(17) 0.0286(17) 0.0159(18) 0.0061(14) 0.0124(14) 0.0146(14) C5 0.0281(17) 0.0225(16) 0.0202(18) 0.0052(14) 0.0099(14) 0.0138(14) C6 0.0273(17) 0.0199(16) 0.026(2) 0.0086(14) 0.0117(15) 0.0088(13) C7 0.0252(16) 0.0244(16) 0.0191(18) 0.0086(14) 0.0097(14) 0.0135(13) C10 0.0239(16) 0.0212(15) 0.0192(18) 0.0038(13) 0.0088(14) 0.0044(13) C11 0.040(2) 0.0279(18) 0.034(2) 0.0096(16) 0.0188(17) 0.0137(15) C12 0.055(2) 0.036(2) 0.036(2) 0.0173(18) 0.026(2) 0.0097(18) C13 0.044(2) 0.041(2) 0.034(2) 0.0070(18) 0.0282(19) 0.0058(17) C14 0.0297(19) 0.0346(19) 0.042(2) 0.0024(18) 0.0197(18) 0.0102(15) C15 0.0260(17) 0.0259(17) 0.032(2) 0.0052(15) 0.0135(16) 0.0080(14) C20 0.0311(18) 0.0230(16) 0.0222(19) 0.0043(14) 0.0158(15) 0.0133(14) C21 0.040(2) 0.0303(18) 0.024(2) 0.0080(15) 0.0114(16) 0.0110(15) C22 0.058(2) 0.036(2) 0.037(2) 0.0197(18) 0.028(2) 0.0178(18) C23 0.048(2) 0.0278(18) 0.055(3) 0.0160(19) 0.037(2) 0.0117(17) C24 0.0325(19) 0.0309(18) 0.038(2) 0.0030(17) 0.0205(17) 0.0067(15) C25 0.0324(18) 0.0296(17) 0.028(2) 0.0081(15) 0.0182(16) 0.0136(15) C30 0.0331(18) 0.0228(16) 0.0172(18) 0.0069(14) 0.0057(15) 0.0137(14) C31 0.046(2) 0.0277(18) 0.024(2) 0.0061(15) 0.0169(17) 0.0177(16) C32 0.067(3) 0.035(2) 0.030(2) 0.0079(17) 0.025(2) 0.026(2) C33 0.071(3) 0.0268(19) 0.019(2) 0.0002(16) 0.005(2) 0.022(2) C34 0.043(2) 0.0240(18) 0.033(2) 0.0036(16) -0.0024(18) 0.0072(16) C35 0.038(2) 0.0268(18) 0.030(2) 0.0049(16) 0.0061(17) 0.0153(15) C40 0.061(2) 0.044(2) 0.035(2) 0.0241(18) 0.028(2) 0.0226(19) C41 0.083(3) 0.055(3) 0.089(4) 0.054(3) 0.058(3) 0.047(2) C42 0.059(3) 0.099(3) 0.030(3) 0.030(2) 0.010(2) 0.019(2) C50 0.0271(18) 0.0340(18) 0.027(2) 0.0066(15) 0.0105(16) 0.0094(15) C51 0.040(2) 0.059(2) 0.060(3) 0.032(2) 0.025(2) 0.0267(19) C52 0.045(2) 0.034(2) 0.056(3) 0.0121(18) 0.029(2) 0.0167(17) C60 0.038(2) 0.070(3) 0.054(3) 0.027(2) 0.008(2) -0.005(2) Cl1 0.0596(8) 0.1033(10) 0.1110(12) 0.0520(9) 0.0448(8) 0.0195(7) Cl2 0.0597(7) 0.0629(7) 0.0664(8) 0.0210(6) 0.0259(6) 0.0034(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N1 2.072(2) . ? Sn1 O2 2.199(2) . ? Sn1 O1 2.243(2) . ? O1 C1 1.262(3) . ? O2 C1 1.259(4) 2_565 ? N1 Si2 1.727(3) . ? N1 Si1 1.734(3) . ? Si1 C42 1.863(4) . ? Si1 C41 1.863(4) . ? Si1 C40 1.871(4) . ? Si2 C51 1.871(4) . ? Si2 C50 1.873(3) . ? Si2 C52 1.875(4) . ? C1 O2 1.259(4) 2_565 ? C1 C2 1.507(4) . ? C2 C3 1.395(4) . ? C2 C7 1.402(4) . ? C3 C4 1.399(4) . ? C3 C20 1.486(4) . ? C4 C5 1.399(4) . ? C5 C6 1.378(4) . ? C5 C30 1.489(4) . ? C6 C7 1.399(4) . ? C7 C10 1.479(4) . ? C10 C15 1.389(4) . ? C10 C11 1.393(4) . ? C11 C12 1.381(5) . ? C12 C13 1.382(5) . ? C13 C14 1.381(5) . ? C14 C15 1.384(5) . ? C20 C21 1.388(5) . ? C20 C25 1.393(4) . ? C21 C22 1.382(5) . ? C22 C23 1.372(5) . ? C23 C24 1.374(5) . ? C24 C25 1.392(4) . ? C30 C31 1.382(4) . ? C30 C35 1.390(4) . ? C31 C32 1.388(4) . ? C32 C33 1.373(5) . ? C33 C34 1.376(5) . ? C34 C35 1.384(4) . ? C60 Cl1 1.745(4) . ? C60 Cl2 1.746(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 N1 Sn1 O2 90.08(9) . . ? N1 Sn1 O1 90.97(9) . . ? O2 Sn1 O1 96.63(8) . . ? C1 O1 Sn1 121.23(18) . . ? C1 O2 Sn1 132.18(19) 2_565 . ? Si2 N1 Si1 122.61(15) . . ? Si2 N1 Sn1 123.93(14) . . ? Si1 N1 Sn1 113.18(13) . . ? N1 Si1 C42 113.09(17) . . ? N1 Si1 C41 111.06(17) . . ? C42 Si1 C41 110.3(2) . . ? N1 Si1 C40 110.39(14) . . ? C42 Si1 C40 105.69(19) . . ? C41 Si1 C40 105.91(17) . . ? N1 Si2 C51 111.00(16) . . ? N1 Si2 C50 112.45(13) . . ? C51 Si2 C50 104.50(16) . . ? N1 Si2 C52 111.70(14) . . ? C51 Si2 C52 107.49(17) . . ? C50 Si2 C52 109.34(17) . . ? O2 C1 O1 124.3(3) 2_565 . ? O2 C1 C2 117.3(3) 2_565 . ? O1 C1 C2 118.4(3) . . ? C3 C2 C7 120.8(3) . . ? C3 C2 C1 120.2(3) . . ? C7 C2 C1 119.0(3) . . ? C2 C3 C4 118.8(3) . . ? C2 C3 C20 122.9(3) . . ? C4 C3 C20 118.2(3) . . ? C5 C4 C3 121.5(3) . . ? C6 C5 C4 118.1(3) . . ? C6 C5 C30 121.6(3) . . ? C4 C5 C30 120.3(3) . . ? C5 C6 C7 122.5(3) . . ? C6 C7 C2 118.3(3) . . ? C6 C7 C10 118.9(3) . . ? C2 C7 C10 122.8(3) . . ? C15 C10 C11 118.2(3) . . ? C15 C10 C7 121.4(3) . . ? C11 C10 C7 120.3(3) . . ? C12 C11 C10 121.1(3) . . ? C11 C12 C13 120.0(3) . . ? C14 C13 C12 119.7(3) . . ? C13 C14 C15 120.3(3) . . ? C14 C15 C10 120.7(3) . . ? C21 C20 C25 118.8(3) . . ? C21 C20 C3 120.5(3) . . ? C25 C20 C3 120.7(3) . . ? C22 C21 C20 120.5(3) . . ? C23 C22 C21 120.6(3) . . ? C22 C23 C24 119.7(3) . . ? C23 C24 C25 120.5(3) . . ? C24 C25 C20 120.0(3) . . ? C31 C30 C35 118.7(3) . . ? C31 C30 C5 120.4(3) . . ? C35 C30 C5 120.9(3) . . ? C30 C31 C32 120.8(3) . . ? C33 C32 C31 119.8(4) . . ? C32 C33 C34 120.2(3) . . ? C33 C34 C35 120.0(3) . . ? C34 C35 C30 120.5(3) . . ? Cl1 C60 Cl2 112.6(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.710 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.080 #===END # CHEMICAL DATA data_5 _database_code_depnum_ccdc_archive 'CCDC 618668' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H86 N2 O4 Si4 Sn2, C H2 Cl2' _chemical_formula_sum 'C63 H88 Cl2 N2 O4 Si4 Sn2' _chemical_formula_weight 1357.99 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' # Crystal Data _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 17.2290(2) _cell_length_b 19.5480(2) _cell_length_c 20.4440(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.4530(6) _cell_angle_gamma 90.00 _cell_volume 6854.23(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19459 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8026 _exptl_absorpt_correction_T_max 0.8026 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; # EXPERIMENTAL DETAIL _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD (BruKer AXS-Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32092 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 28.28 _reflns_number_total 16974 _reflns_number_gt 11179 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution ; SIR-97 (A. Altomare, G. Cascarano et al.) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Cameron (WinGX v1.64-05), Ortep (SHELXTL-NT v6.10, Bruker AXS) ; _computing_publication_material 'WinGX v1.64-05 (L. J. Farrugia)' # REFINEMENT DATA _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^)+(0.0193P)^2^+5.5228P] 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 16974 _refine_ls_number_parameters 718 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 0.193735(10) 0.250412(9) 0.584405(8) 0.02518(5) Uani 1 1 d . . . Sn2 Sn 0.299480(10) 0.251111(9) 0.396179(8) 0.02502(5) Uani 1 1 d . . . Cl91 Cl 0.26887(6) 0.30676(6) 0.00025(5) 0.0766(3) Uani 1 1 d . . . Cl92 Cl 0.24855(6) 0.18166(6) 0.07367(6) 0.0841(3) Uani 1 1 d . . . Si41 Si 0.28463(5) 0.10438(4) 0.63720(4) 0.03506(18) Uani 1 1 d . . . Si42 Si 0.19013(5) 0.18449(5) 0.72856(4) 0.0399(2) Uani 1 1 d . . . Si81 Si 0.32257(5) 0.34157(4) 0.26717(4) 0.03439(19) Uani 1 1 d . . . Si82 Si 0.18995(5) 0.38792(4) 0.34242(4) 0.03443(18) Uani 1 1 d . . . O11 O 0.17070(10) 0.17263(9) 0.50601(8) 0.0277(4) Uani 1 1 d . . . O12 O 0.17602(10) 0.22753(9) 0.41035(8) 0.0284(4) Uani 1 1 d . . . O51 O 0.31860(11) 0.27252(9) 0.57530(8) 0.0312(4) Uani 1 1 d . . . O52 O 0.32715(11) 0.32473(9) 0.47913(8) 0.0308(4) Uani 1 1 d . . . N41 N 0.22616(13) 0.17379(11) 0.65291(10) 0.0290(5) Uani 1 1 d . . . N81 N 0.26683(13) 0.33207(11) 0.33294(9) 0.0279(5) Uani 1 1 d . . . C11 C 0.08500(14) 0.13651(12) 0.41500(11) 0.0210(5) Uani 1 1 d . . . C12 C 0.10287(15) 0.08859(12) 0.36800(11) 0.0236(5) Uani 1 1 d . . . C13 C 0.04403(16) 0.04587(13) 0.34057(12) 0.0290(6) Uani 1 1 d . . . H13 H 0.0554 0.0132 0.3084 0.035 Uiso 1 1 calc . . . C14 C -0.03079(16) 0.05022(13) 0.35929(14) 0.0317(6) Uani 1 1 d . . . H14 H -0.0702 0.0203 0.3404 0.038 Uiso 1 1 calc . . . C15 C -0.04827(14) 0.09807(13) 0.40547(13) 0.0289(6) Uani 1 1 d . . . H15 H -0.0999 0.1011 0.4179 0.035 Uiso 1 1 calc . . . C16 C 0.00927(14) 0.14214(12) 0.43413(11) 0.0230(5) Uani 1 1 d . . . C17 C 0.14836(14) 0.18249(12) 0.44592(11) 0.0223(5) Uani 1 1 d . . . C21 C 0.18346(15) 0.08164(14) 0.34724(12) 0.0297(6) Uani 1 1 d . . . C22 C 0.23701(16) 0.03857(15) 0.38269(15) 0.0381(7) Uani 1 1 d . . . C23 C 0.31229(19) 0.03438(18) 0.3623(2) 0.0566(10) Uani 1 1 d . . . H23 H 0.3501 0.0070 0.3870 0.068 Uiso 1 1 calc . . . C24 C 0.3335(2) 0.0684(2) 0.3079(2) 0.0611(11) Uani 1 1 d . . . C25 C 0.2785(2) 0.10699(19) 0.27220(16) 0.0545(10) Uani 1 1 d . . . H25 H 0.2918 0.1286 0.2331 0.065 Uiso 1 1 calc . . . C26 C 0.20384(17) 0.11575(15) 0.29112(13) 0.0371(7) Uani 1 1 d . . . C27 C 0.21448(19) -0.00266(16) 0.43993(17) 0.0519(9) Uani 1 1 d . . . H27A H 0.1881 0.0270 0.4695 0.062 Uiso 1 1 calc R . . H27B H 0.2614 -0.0222 0.4637 0.062 Uiso 1 1 calc R . . H27C H 0.1792 -0.0396 0.4239 0.062 Uiso 1 1 calc R . . C28 C 0.4168(2) 0.0651(2) 0.2891(3) 0.0993(18) Uani 1 1 d . . . H28A H 0.4163 0.0645 0.2411 0.119 Uiso 1 1 calc R . . H28B H 0.4420 0.0234 0.3074 0.119 Uiso 1 1 calc R . . H28C H 0.4458 0.1052 0.3068 0.119 Uiso 1 1 calc R . . C29 C 0.1470(2) 0.16277(17) 0.25300(14) 0.0527(9) Uani 1 1 d . . . H29A H 0.0972 0.1390 0.2428 0.063 Uiso 1 1 calc R . . H29B H 0.1680 0.1764 0.2121 0.063 Uiso 1 1 calc R . . H29C H 0.1387 0.2035 0.2794 0.063 Uiso 1 1 calc R . . C31 C -0.01273(14) 0.19615(13) 0.48061(12) 0.0240(5) Uani 1 1 d . . . C32 C -0.03163(15) 0.26199(13) 0.45659(12) 0.0291(6) Uani 1 1 d . . . C33 C -0.05370(17) 0.31152(14) 0.49994(14) 0.0362(7) Uani 1 1 d . . . H33 H -0.0652 0.3563 0.4838 0.043 Uiso 1 1 calc . . . C34 C -0.05956(18) 0.29803(15) 0.56572(14) 0.0388(7) Uani 1 1 d . . . C35 C -0.04233(17) 0.23229(15) 0.58779(13) 0.0363(7) Uani 1 1 d . . . H35 H -0.0474 0.2217 0.6325 0.044 Uiso 1 1 calc . . . C36 C -0.01789(15) 0.18120(14) 0.54718(12) 0.0294(6) Uani 1 1 d . . . C37 C -0.03098(19) 0.27852(16) 0.38510(13) 0.0412(7) Uani 1 1 d . . . H37A H -0.0362 0.3281 0.3787 0.049 Uiso 1 1 calc R . . H37B H -0.0746 0.2552 0.3600 0.049 Uiso 1 1 calc R . . H37C H 0.0183 0.2631 0.3697 0.049 Uiso 1 1 calc R . . C38 C -0.0850(2) 0.35278(17) 0.61104(17) 0.0614(10) Uani 1 1 d . . . H38A H -0.0878 0.3968 0.5881 0.074 Uiso 1 1 calc R . . H38B H -0.0473 0.3558 0.6500 0.074 Uiso 1 1 calc R . . H38C H -0.1365 0.3412 0.6245 0.074 Uiso 1 1 calc R . . C39 C 0.00197(18) 0.11072(15) 0.57389(14) 0.0411(7) Uani 1 1 d . . . H39A H -0.0310 0.0767 0.5494 0.049 Uiso 1 1 calc R . . H39B H -0.0071 0.1089 0.6205 0.049 Uiso 1 1 calc R . . H39C H 0.0569 0.1008 0.5692 0.049 Uiso 1 1 calc R . . C41 C 0.22700(18) 0.02302(15) 0.62771(17) 0.0476(8) Uani 1 1 d . . . H41A H 0.2097 0.0099 0.6703 0.057 Uiso 1 1 calc R . . H41B H 0.2597 -0.0133 0.6120 0.057 Uiso 1 1 calc R . . H41C H 0.1814 0.0300 0.5959 0.057 Uiso 1 1 calc R . . C42 C 0.33589(16) 0.11339(14) 0.56112(14) 0.0351(6) Uani 1 1 d . . . H42A H 0.2973 0.1160 0.5227 0.042 Uiso 1 1 calc R . . H42B H 0.3698 0.0737 0.5568 0.042 Uiso 1 1 calc R . . H42C H 0.3675 0.1552 0.5639 0.042 Uiso 1 1 calc R . . C43 C 0.36235(19) 0.0910(2) 0.70689(16) 0.0593(10) Uani 1 1 d . . . H43A H 0.3903 0.1340 0.7165 0.071 Uiso 1 1 calc R . . H43B H 0.3991 0.0560 0.6946 0.071 Uiso 1 1 calc R . . H43C H 0.3382 0.0759 0.7459 0.071 Uiso 1 1 calc R . . C44 C 0.1380(2) 0.10704(18) 0.75566(16) 0.0610(10) Uani 1 1 d . . . H44A H 0.0948 0.0957 0.7227 0.073 Uiso 1 1 calc R . . H44B H 0.1175 0.1164 0.7979 0.073 Uiso 1 1 calc R . . H44C H 0.1744 0.0684 0.7606 0.073 Uiso 1 1 calc R . . C45 C 0.1183(2) 0.25705(17) 0.72406(15) 0.0531(9) Uani 1 1 d . . . H45A H 0.1457 0.3002 0.7179 0.064 Uiso 1 1 calc R . . H45B H 0.0930 0.2591 0.7650 0.064 Uiso 1 1 calc R . . H45C H 0.0788 0.2497 0.6870 0.064 Uiso 1 1 calc R . . C46 C 0.2654(2) 0.2061(2) 0.79781(15) 0.0668(11) Uani 1 1 d . . . H46A H 0.2956 0.1650 0.8109 0.080 Uiso 1 1 calc R . . H46B H 0.2395 0.2231 0.8353 0.080 Uiso 1 1 calc R . . H46C H 0.3004 0.2414 0.7834 0.080 Uiso 1 1 calc R . . C51 C 0.41691(15) 0.35666(13) 0.56933(12) 0.0282(6) Uani 1 1 d . . . C52 C 0.49327(16) 0.33420(15) 0.56524(12) 0.0334(6) Uani 1 1 d . . . C53 C 0.55450(17) 0.37446(17) 0.59371(15) 0.0459(8) Uani 1 1 d . . . H53 H 0.6068 0.3598 0.5917 0.055 Uiso 1 1 calc . . . C54 C 0.5401(2) 0.43456(19) 0.62435(17) 0.0585(10) Uani 1 1 d . . . H54 H 0.5824 0.4616 0.6428 0.070 Uiso 1 1 calc . . . C55 C 0.4646(2) 0.45638(17) 0.62879(16) 0.0516(9) Uani 1 1 d . . . H55 H 0.4555 0.4981 0.6507 0.062 Uiso 1 1 calc . . . C56 C 0.40136(17) 0.41761(14) 0.60128(13) 0.0347(7) Uani 1 1 d . . . C57 C 0.34940(14) 0.31457(12) 0.53900(12) 0.0235(5) Uani 1 1 d . . . C61 C 0.51106(15) 0.26765(15) 0.53391(14) 0.0342(7) Uani 1 1 d . . . C62 C 0.52109(17) 0.20883(17) 0.57312(16) 0.0449(8) Uani 1 1 d . . . C63 C 0.54006(19) 0.14751(17) 0.5432(2) 0.0574(10) Uani 1 1 d . . . H63 H 0.5474 0.1075 0.5694 0.069 Uiso 1 1 calc . . . C64 C 0.54847(19) 0.14328(19) 0.4770(2) 0.0602(10) Uani 1 1 d . . . C65 C 0.53939(18) 0.20169(19) 0.43960(17) 0.0522(9) Uani 1 1 d . . . H65 H 0.5455 0.1993 0.3940 0.063 Uiso 1 1 calc . . . C66 C 0.52138(16) 0.26432(15) 0.46702(14) 0.0376(7) Uani 1 1 d . . . C67 C 0.5113(2) 0.2119(2) 0.64520(16) 0.0618(10) Uani 1 1 d . . . H67A H 0.4588 0.2284 0.6515 0.074 Uiso 1 1 calc R . . H67B H 0.5501 0.2431 0.6669 0.074 Uiso 1 1 calc R . . H67C H 0.5185 0.1661 0.6643 0.074 Uiso 1 1 calc R . . C68 C 0.5676(3) 0.0751(2) 0.4465(3) 0.0938(16) Uani 1 1 d . . . H68A H 0.5930 0.0833 0.4063 0.113 Uiso 1 1 calc R . . H68B H 0.5195 0.0491 0.4359 0.113 Uiso 1 1 calc R . . H68C H 0.6028 0.0491 0.4777 0.113 Uiso 1 1 calc R . . C69 C 0.51537(19) 0.32828(16) 0.42524(14) 0.0465(8) Uani 1 1 d . . . H69A H 0.4655 0.3510 0.4299 0.056 Uiso 1 1 calc R . . H69B H 0.5185 0.3160 0.3791 0.056 Uiso 1 1 calc R . . H69C H 0.5583 0.3593 0.4397 0.056 Uiso 1 1 calc R . . C71 C 0.31973(17) 0.44076(14) 0.60610(13) 0.0349(7) Uani 1 1 d . . . C72 C 0.2826(2) 0.48341(14) 0.55747(14) 0.0417(7) Uani 1 1 d . . . C73 C 0.2057(2) 0.50294(16) 0.56140(17) 0.0513(9) Uani 1 1 d . . . H73 H 0.1812 0.5320 0.5284 0.062 Uiso 1 1 calc . . . C74 C 0.1638(2) 0.48144(16) 0.61188(18) 0.0527(9) Uani 1 1 d . . . C75 C 0.2013(2) 0.44065(16) 0.65998(16) 0.0481(8) Uani 1 1 d . . . H75 H 0.1733 0.4259 0.6953 0.058 Uiso 1 1 calc . . . C76 C 0.27904(19) 0.42005(15) 0.65891(14) 0.0406(7) Uani 1 1 d . . . C77 C 0.3254(2) 0.50705(17) 0.50072(16) 0.0571(9) Uani 1 1 d . . . H77A H 0.3399 0.4673 0.4753 0.069 Uiso 1 1 calc R . . H77B H 0.3726 0.5318 0.5175 0.069 Uiso 1 1 calc R . . H77C H 0.2916 0.5374 0.4725 0.069 Uiso 1 1 calc R . . C78 C 0.0794(2) 0.5018(2) 0.6144(2) 0.0820(13) Uani 1 1 d . . . H78A H 0.0590 0.4804 0.6526 0.098 Uiso 1 1 calc R . . H78B H 0.0488 0.4865 0.5742 0.098 Uiso 1 1 calc R . . H78C H 0.0757 0.5516 0.6180 0.098 Uiso 1 1 calc R . . C79 C 0.3183(2) 0.37667(17) 0.71320(15) 0.0533(9) Uani 1 1 d . . . H79A H 0.2836 0.3715 0.7482 0.064 Uiso 1 1 calc R . . H79B H 0.3669 0.3987 0.7310 0.064 Uiso 1 1 calc R . . H79C H 0.3300 0.3315 0.6958 0.064 Uiso 1 1 calc R . . C81 C 0.2629(2) 0.3507(2) 0.18655(14) 0.0593(10) Uani 1 1 d . . . H81A H 0.2276 0.3115 0.1798 0.071 Uiso 1 1 calc R . . H81B H 0.2974 0.3523 0.1511 0.071 Uiso 1 1 calc R . . H81C H 0.2324 0.3930 0.1864 0.071 Uiso 1 1 calc R . . C82 C 0.3896(2) 0.41682(17) 0.27557(17) 0.0563(9) Uani 1 1 d . . . H82A H 0.3594 0.4590 0.2678 0.068 Uiso 1 1 calc R . . H82B H 0.4280 0.4133 0.2433 0.068 Uiso 1 1 calc R . . H82C H 0.4166 0.4177 0.3200 0.068 Uiso 1 1 calc R . . C83 C 0.38808(19) 0.26580(16) 0.25999(15) 0.0484(8) Uani 1 1 d . . . H83A H 0.4236 0.2616 0.3002 0.058 Uiso 1 1 calc R . . H83B H 0.4184 0.2720 0.2222 0.058 Uiso 1 1 calc R . . H83C H 0.3564 0.2242 0.2539 0.058 Uiso 1 1 calc R . . C84 C 0.10410(18) 0.36877(19) 0.28254(14) 0.0543(9) Uani 1 1 d . . . H84A H 0.1173 0.3785 0.2379 0.065 Uiso 1 1 calc R . . H84B H 0.0599 0.3973 0.2924 0.065 Uiso 1 1 calc R . . H84C H 0.0900 0.3204 0.2859 0.065 Uiso 1 1 calc R . . C85 C 0.15579(17) 0.38677(15) 0.42645(13) 0.0366(7) Uani 1 1 d . . . H85A H 0.1322 0.3423 0.4343 0.044 Uiso 1 1 calc R . . H85B H 0.1170 0.4230 0.4299 0.044 Uiso 1 1 calc R . . H85C H 0.2002 0.3945 0.4592 0.044 Uiso 1 1 calc R . . C86 C 0.2183(2) 0.47880(16) 0.32702(16) 0.0541(9) Uani 1 1 d . . . H86A H 0.2643 0.4909 0.3566 0.065 Uiso 1 1 calc R . . H86B H 0.1750 0.5093 0.3351 0.065 Uiso 1 1 calc R . . H86C H 0.2302 0.4837 0.2813 0.065 Uiso 1 1 calc R . . C91 C 0.2514(2) 0.2189(2) -0.00429(18) 0.0729(12) Uani 1 1 d . . . H91A H 0.2930 0.1966 -0.0270 0.087 Uiso 1 1 calc R . . H91B H 0.2011 0.2105 -0.0307 0.087 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 0.02939(10) 0.02604(9) 0.02061(8) 0.00036(8) 0.00498(7) -0.00220(8) Sn2 0.02570(10) 0.02641(10) 0.02328(9) -0.00049(8) 0.00408(7) -0.00462(8) Cl91 0.0560(6) 0.0776(7) 0.0963(8) 0.0191(6) 0.0076(5) -0.0096(5) Cl92 0.0635(7) 0.0891(8) 0.1016(8) 0.0267(7) 0.0185(6) -0.0127(6) Si41 0.0288(4) 0.0338(4) 0.0427(4) 0.0113(4) 0.0041(3) -0.0020(3) Si42 0.0537(6) 0.0435(5) 0.0234(4) 0.0033(4) 0.0090(3) -0.0125(4) Si81 0.0401(5) 0.0375(5) 0.0268(4) 0.0006(3) 0.0091(3) -0.0107(4) Si82 0.0380(5) 0.0369(5) 0.0281(4) 0.0032(3) 0.0018(3) 0.0018(4) O11 0.0294(10) 0.0296(10) 0.0235(9) -0.0016(8) -0.0007(7) -0.0025(8) O12 0.0267(10) 0.0275(9) 0.0314(9) 0.0012(8) 0.0044(8) -0.0095(8) O51 0.0321(11) 0.0292(10) 0.0319(10) 0.0026(8) 0.0015(8) -0.0112(8) O52 0.0362(11) 0.0303(10) 0.0249(9) -0.0014(8) -0.0023(8) -0.0072(8) N41 0.0303(13) 0.0327(13) 0.0240(10) 0.0065(10) 0.0027(9) -0.0041(10) N81 0.0316(13) 0.0306(12) 0.0214(10) 0.0022(9) 0.0030(9) -0.0058(10) C11 0.0204(13) 0.0193(12) 0.0231(12) 0.0029(10) 0.0002(9) -0.0027(10) C12 0.0244(14) 0.0210(13) 0.0253(12) 0.0001(10) 0.0017(10) -0.0017(10) C13 0.0300(15) 0.0238(14) 0.0330(14) -0.0066(11) 0.0015(11) -0.0009(11) C14 0.0251(15) 0.0240(14) 0.0447(16) -0.0047(12) -0.0041(12) -0.0062(11) C15 0.0182(13) 0.0284(14) 0.0408(15) 0.0019(12) 0.0057(11) -0.0018(11) C16 0.0205(13) 0.0234(13) 0.0249(12) 0.0040(11) 0.0022(10) 0.0013(10) C17 0.0207(13) 0.0220(13) 0.0249(12) -0.0044(11) 0.0055(10) 0.0017(10) C21 0.0255(15) 0.0326(15) 0.0317(14) -0.0141(12) 0.0058(11) -0.0036(12) C22 0.0274(16) 0.0335(16) 0.0540(18) -0.0128(14) 0.0069(13) -0.0027(13) C23 0.0285(18) 0.048(2) 0.093(3) -0.028(2) 0.0062(18) 0.0039(15) C24 0.041(2) 0.057(2) 0.090(3) -0.046(2) 0.035(2) -0.0184(18) C25 0.055(2) 0.062(2) 0.0517(19) -0.0319(18) 0.0304(17) -0.0327(19) C26 0.0436(18) 0.0387(17) 0.0306(14) -0.0170(13) 0.0114(13) -0.0198(14) C27 0.043(2) 0.0400(18) 0.070(2) 0.0083(17) -0.0075(16) 0.0075(15) C28 0.051(3) 0.095(3) 0.162(5) -0.068(3) 0.058(3) -0.028(2) C29 0.071(2) 0.057(2) 0.0304(15) 0.0036(15) 0.0034(15) -0.0261(19) C31 0.0179(13) 0.0262(14) 0.0287(13) -0.0002(11) 0.0058(10) -0.0002(10) C32 0.0266(14) 0.0301(15) 0.0307(13) 0.0026(11) 0.0041(11) 0.0015(11) C33 0.0404(18) 0.0275(15) 0.0412(16) 0.0005(13) 0.0068(13) 0.0053(13) C34 0.0430(18) 0.0357(17) 0.0393(16) -0.0068(14) 0.0130(13) 0.0027(14) C35 0.0377(17) 0.0449(18) 0.0283(14) -0.0003(13) 0.0138(12) -0.0005(13) C36 0.0231(14) 0.0334(15) 0.0329(14) 0.0049(12) 0.0082(11) -0.0005(12) C37 0.052(2) 0.0362(16) 0.0352(15) 0.0056(14) 0.0041(14) 0.0087(15) C38 0.081(3) 0.049(2) 0.057(2) -0.0126(18) 0.0273(19) 0.008(2) C39 0.0458(19) 0.0401(17) 0.0397(16) 0.0115(14) 0.0157(14) 0.0057(15) C41 0.042(2) 0.0323(17) 0.072(2) 0.0061(16) 0.0202(16) -0.0025(14) C42 0.0271(15) 0.0296(15) 0.0498(17) 0.0025(13) 0.0101(12) -0.0009(12) C43 0.041(2) 0.077(3) 0.059(2) 0.031(2) -0.0007(16) 0.0069(18) C44 0.082(3) 0.060(2) 0.0461(19) 0.0026(17) 0.0321(18) -0.020(2) C45 0.065(2) 0.061(2) 0.0372(16) -0.0049(16) 0.0271(15) -0.0032(19) C46 0.094(3) 0.072(3) 0.0318(17) 0.0023(18) -0.0086(18) -0.011(2) C51 0.0328(16) 0.0294(14) 0.0223(12) 0.0001(11) 0.0020(11) -0.0123(12) C52 0.0304(16) 0.0416(17) 0.0279(13) -0.0015(13) 0.0007(11) -0.0104(13) C53 0.0300(17) 0.061(2) 0.0469(17) -0.0111(16) 0.0035(13) -0.0156(15) C54 0.048(2) 0.069(2) 0.058(2) -0.0265(19) 0.0009(17) -0.0309(19) C55 0.054(2) 0.049(2) 0.0535(19) -0.0236(16) 0.0113(16) -0.0225(17) C56 0.0394(18) 0.0349(16) 0.0302(14) -0.0067(13) 0.0055(12) -0.0125(13) C57 0.0257(14) 0.0187(12) 0.0264(13) -0.0032(11) 0.0040(10) -0.0024(11) C61 0.0188(14) 0.0370(16) 0.0464(16) -0.0008(13) 0.0008(12) -0.0050(11) C62 0.0217(16) 0.050(2) 0.063(2) 0.0119(17) 0.0016(14) -0.0040(14) C63 0.0287(18) 0.0397(19) 0.104(3) 0.014(2) 0.0056(19) 0.0045(15) C64 0.034(2) 0.046(2) 0.101(3) -0.016(2) 0.0070(19) 0.0027(16) C65 0.0314(18) 0.063(2) 0.063(2) -0.0193(19) 0.0074(15) 0.0028(16) C66 0.0230(15) 0.0458(19) 0.0443(16) -0.0069(14) 0.0052(12) -0.0052(13) C67 0.047(2) 0.076(3) 0.061(2) 0.028(2) -0.0014(17) -0.0058(19) C68 0.076(3) 0.053(3) 0.152(5) -0.030(3) 0.012(3) 0.011(2) C69 0.045(2) 0.056(2) 0.0399(16) -0.0052(16) 0.0098(14) -0.0045(16) C71 0.0459(19) 0.0241(14) 0.0359(15) -0.0132(12) 0.0104(13) -0.0113(13) C72 0.056(2) 0.0263(15) 0.0429(17) -0.0116(14) 0.0061(15) -0.0099(15) C73 0.063(2) 0.0278(17) 0.062(2) -0.0111(16) -0.0017(18) 0.0011(16) C74 0.059(2) 0.0310(17) 0.069(2) -0.0185(17) 0.0071(19) 0.0000(16) C75 0.057(2) 0.0346(17) 0.056(2) -0.0213(16) 0.0261(17) -0.0131(16) C76 0.054(2) 0.0290(16) 0.0396(16) -0.0105(13) 0.0078(14) -0.0100(14) C77 0.080(3) 0.042(2) 0.0492(19) 0.0047(16) 0.0083(18) -0.0112(18) C78 0.065(3) 0.066(3) 0.117(4) -0.018(3) 0.017(2) 0.011(2) C79 0.071(3) 0.051(2) 0.0401(17) -0.0088(16) 0.0167(16) -0.0082(18) C81 0.070(3) 0.080(3) 0.0287(15) 0.0018(17) 0.0095(15) -0.003(2) C82 0.058(2) 0.047(2) 0.067(2) 0.0018(17) 0.0213(18) -0.0170(17) C83 0.051(2) 0.051(2) 0.0471(18) -0.0035(15) 0.0230(15) -0.0090(16) C84 0.041(2) 0.081(3) 0.0401(17) 0.0077(18) -0.0027(14) 0.0046(18) C85 0.0386(17) 0.0359(16) 0.0362(15) -0.0017(13) 0.0084(12) 0.0052(13) C86 0.074(3) 0.0405(19) 0.0495(19) 0.0149(16) 0.0132(17) 0.0069(18) C91 0.069(3) 0.074(3) 0.073(3) -0.010(2) -0.007(2) 0.009(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. ; # MOLECULAR GEOMETRY 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 N41 2.090(2) . ? Sn1 O11 2.2175(16) . ? Sn1 O51 2.2194(18) . ? Sn2 N81 2.087(2) . ? Sn2 O12 2.2222(17) . ? Sn2 O52 2.2407(16) . ? Cl91 C91 1.745(4) . ? Cl92 C91 1.757(4) . ? Si41 N41 1.738(2) . ? Si41 C42 1.869(3) . ? Si41 C41 1.875(3) . ? Si41 C43 1.879(3) . ? Si42 N41 1.733(2) . ? Si42 C44 1.871(3) . ? Si42 C46 1.875(3) . ? Si42 C45 1.879(3) . ? Si81 N81 1.735(2) . ? Si81 C81 1.866(3) . ? Si81 C82 1.868(3) . ? Si81 C83 1.876(3) . ? Si82 N81 1.742(2) . ? Si82 C84 1.866(3) . ? Si82 C85 1.868(3) . ? Si82 C86 1.877(3) . ? O11 C17 1.267(3) . ? O12 C17 1.264(3) . ? O51 C57 1.258(3) . ? O52 C57 1.263(3) . ? C11 C12 1.397(3) . ? C11 C16 1.402(3) . ? C11 C17 1.506(3) . ? C12 C13 1.390(3) . ? C12 C21 1.496(4) . ? C13 C14 1.382(4) . ? C13 H13 0.9500 . ? C14 C15 1.382(4) . ? C14 H14 0.9500 . ? C15 C16 1.399(3) . ? C15 H15 0.9500 . ? C16 C31 1.493(3) . ? C21 C22 1.400(4) . ? C21 C26 1.400(4) . ? C22 C23 1.402(4) . ? C22 C27 1.502(4) . ? C23 C24 1.375(5) . ? C23 H23 0.9500 . ? C24 C25 1.367(5) . ? C24 C28 1.522(5) . ? C25 C26 1.389(4) . ? C25 H25 0.9500 . ? C26 C29 1.506(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C36 1.403(3) . ? C31 C32 1.405(3) . ? C32 C33 1.390(4) . ? C32 C37 1.498(4) . ? C33 C34 1.384(4) . ? C33 H33 0.9500 . ? C34 C35 1.385(4) . ? C34 C38 1.508(4) . ? C35 C36 1.389(4) . ? C35 H35 0.9500 . ? C36 C39 1.509(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C51 C56 1.397(4) . ? C51 C52 1.397(4) . ? C51 C57 1.509(3) . ? C52 C53 1.398(4) . ? C52 C61 1.495(4) . ? C53 C54 1.365(5) . ? C53 H53 0.9500 . ? C54 C55 1.379(5) . ? C54 H54 0.9500 . ? C55 C56 1.401(4) . ? C55 H55 0.9500 . ? C56 C71 1.489(4) . ? C61 C66 1.397(4) . ? C61 C62 1.403(4) . ? C62 C63 1.398(5) . ? C62 C67 1.500(4) . ? C63 C64 1.377(5) . ? C63 H63 0.9500 . ? C64 C65 1.375(5) . ? C64 C68 1.520(5) . ? C65 C66 1.394(4) . ? C65 H65 0.9500 . ? C66 C69 1.512(4) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C71 C76 1.402(4) . ? C71 C72 1.404(4) . ? C72 C73 1.388(5) . ? C72 C77 1.505(4) . ? C73 C74 1.380(5) . ? C73 H73 0.9500 . ? C74 C75 1.378(5) . ? C74 C78 1.513(5) . ? C75 C76 1.400(4) . ? C75 H75 0.9500 . ? C76 C79 1.505(4) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 Sn1 O11 90.63(7) . . ? N41 Sn1 O51 89.79(8) . . ? O11 Sn1 O51 100.44(7) . . ? N81 Sn2 O12 91.90(7) . . ? N81 Sn2 O52 90.42(7) . . ? O12 Sn2 O52 99.91(6) . . ? N41 Si41 C42 114.11(12) . . ? N41 Si41 C41 111.76(12) . . ? C42 Si41 C41 106.34(14) . . ? N41 Si41 C43 110.66(14) . . ? C42 Si41 C43 106.57(14) . . ? C41 Si41 C43 106.98(16) . . ? N41 Si42 C44 112.90(13) . . ? N41 Si42 C46 114.86(15) . . ? C44 Si42 C46 106.00(17) . . ? N41 Si42 C45 109.72(12) . . ? C44 Si42 C45 107.05(17) . . ? C46 Si42 C45 105.78(17) . . ? N81 Si81 C81 113.31(13) . . ? N81 Si81 C82 113.33(13) . . ? C81 Si81 C82 106.86(16) . . ? N81 Si81 C83 110.94(12) . . ? C81 Si81 C83 106.93(16) . . ? C82 Si81 C83 104.92(15) . . ? N81 Si82 C84 111.41(14) . . ? N81 Si82 C85 113.84(11) . . ? C84 Si82 C85 107.56(14) . . ? N81 Si82 C86 111.23(14) . . ? C84 Si82 C86 106.40(16) . . ? C85 Si82 C86 105.98(14) . . ? C17 O11 Sn1 127.85(16) . . ? C17 O12 Sn2 129.60(16) . . ? C57 O51 Sn1 130.04(17) . . ? C57 O52 Sn2 130.96(16) . . ? Si42 N41 Si41 121.48(12) . . ? Si42 N41 Sn1 114.58(12) . . ? Si41 N41 Sn1 123.94(11) . . ? Si81 N81 Si82 120.14(12) . . ? Si81 N81 Sn2 115.14(12) . . ? Si82 N81 Sn2 124.72(11) . . ? C12 C11 C16 121.1(2) . . ? C12 C11 C17 119.4(2) . . ? C16 C11 C17 119.5(2) . . ? C13 C12 C11 118.7(2) . . ? C13 C12 C21 119.5(2) . . ? C11 C12 C21 121.8(2) . . ? C14 C13 C12 121.0(2) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 120.0(2) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 120.7(2) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 118.4(2) . . ? C15 C16 C31 119.3(2) . . ? C11 C16 C31 122.2(2) . . ? O12 C17 O11 124.6(2) . . ? O12 C17 C11 118.2(2) . . ? O11 C17 C11 117.2(2) . . ? C22 C21 C26 120.4(3) . . ? C22 C21 C12 119.4(2) . . ? C26 C21 C12 120.1(2) . . ? C21 C22 C23 117.6(3) . . ? C21 C22 C27 121.3(3) . . ? C23 C22 C27 121.0(3) . . ? C24 C23 C22 122.5(3) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C25 C24 C23 118.3(3) . . ? C25 C24 C28 120.8(4) . . ? C23 C24 C28 120.9(4) . . ? C24 C25 C26 122.2(3) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C21 118.7(3) . . ? C25 C26 C29 120.4(3) . . ? C21 C26 C29 120.9(3) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C36 C31 C32 119.7(2) . . ? C36 C31 C16 120.9(2) . . ? C32 C31 C16 119.3(2) . . ? C33 C32 C31 118.9(2) . . ? C33 C32 C37 120.0(2) . . ? C31 C32 C37 121.0(2) . . ? C34 C33 C32 122.5(3) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C33 C34 C35 117.4(3) . . ? C33 C34 C38 121.0(3) . . ? C35 C34 C38 121.6(3) . . ? C34 C35 C36 122.7(2) . . ? C34 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C35 C36 C31 118.7(2) . . ? C35 C36 C39 120.7(2) . . ? C31 C36 C39 120.5(2) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si41 C41 H41A 109.5 . . ? Si41 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si41 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si41 C42 H42A 109.5 . . ? Si41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si41 C43 H43A 109.5 . . ? Si41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si42 C44 H44A 109.5 . . ? Si42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si42 C45 H45A 109.5 . . ? Si42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si42 C46 H46A 109.5 . . ? Si42 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si42 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C56 C51 C52 121.3(2) . . ? C56 C51 C57 118.9(2) . . ? C52 C51 C57 119.8(2) . . ? C51 C52 C53 118.4(3) . . ? C51 C52 C61 122.1(2) . . ? C53 C52 C61 119.4(3) . . ? C54 C53 C52 120.8(3) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C53 C54 C55 120.7(3) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C54 C55 C56 120.6(3) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C51 C56 C55 118.2(3) . . ? C51 C56 C71 121.0(2) . . ? C55 C56 C71 120.8(3) . . ? O51 C57 O52 124.6(2) . . ? O51 C57 C51 117.7(2) . . ? O52 C57 C51 117.6(2) . . ? C66 C61 C62 120.1(3) . . ? C66 C61 C52 120.7(3) . . ? C62 C61 C52 119.2(3) . . ? C63 C62 C61 118.3(3) . . ? C63 C62 C67 121.1(3) . . ? C61 C62 C67 120.6(3) . . ? C64 C63 C62 122.1(3) . . ? C64 C63 H63 118.9 . . ? C62 C63 H63 118.9 . . ? C65 C64 C63 118.7(3) . . ? C65 C64 C68 121.1(4) . . ? C63 C64 C68 120.2(4) . . ? C64 C65 C66 121.6(3) . . ? C64 C65 H65 119.2 . . ? C66 C65 H65 119.2 . . ? C65 C66 C61 119.2(3) . . ? C65 C66 C69 120.3(3) . . ? C61 C66 C69 120.4(3) . . ? C62 C67 H67A 109.5 . . ? C62 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C62 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C64 C68 H68A 109.5 . . ? C64 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C64 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C66 C69 H69A 109.5 . . ? C66 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C66 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C76 C71 C72 119.3(3) . . ? C76 C71 C56 120.5(3) . . ? C72 C71 C56 120.2(3) . . ? C73 C72 C71 119.7(3) . . ? C73 C72 C77 120.0(3) . . ? C71 C72 C77 120.3(3) . . ? C74 C73 C72 122.0(3) . . ? C74 C73 H73 119.0 . . ? C72 C73 H73 119.0 . . ? C75 C74 C73 117.8(3) . . ? C75 C74 C78 121.0(4) . . ? C73 C74 C78 121.2(4) . . ? C74 C75 C76 122.6(3) . . ? C74 C75 H75 118.7 . . ? C76 C75 H75 118.7 . . ? C75 C76 C71 118.6(3) . . ? C75 C76 C79 120.9(3) . . ? C71 C76 C79 120.5(3) . . ? C72 C77 H77A 109.5 . . ? C72 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C72 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C74 C78 H78A 109.5 . . ? C74 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C74 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C76 C79 H79A 109.5 . . ? C76 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C76 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? Si81 C81 H81A 109.5 . . ? Si81 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? Si81 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? Si81 C82 H82A 109.5 . . ? Si81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? Si81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? Si81 C83 H83A 109.5 . . ? Si81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? Si81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? Si82 C84 H84A 109.5 . . ? Si82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? Si82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? Si82 C85 H85A 109.5 . . ? Si82 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? Si82 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? Si82 C86 H86A 109.5 . . ? Si82 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? Si82 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? Cl91 C91 Cl92 112.3(2) . . ? Cl91 C91 H91A 109.2 . . ? Cl92 C91 H91A 109.2 . . ? Cl91 C91 H91B 109.2 . . ? Cl92 C91 H91B 109.2 . . ? H91A C91 H91B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N41 Sn1 O11 C17 -178.8(2) . . . . ? O51 Sn1 O11 C17 -88.9(2) . . . . ? N81 Sn2 O12 C17 -178.3(2) . . . . ? O52 Sn2 O12 C17 -87.5(2) . . . . ? N41 Sn1 O51 C57 177.7(2) . . . . ? O11 Sn1 O51 C57 87.1(2) . . . . ? N81 Sn2 O52 C57 176.9(2) . . . . ? O12 Sn2 O52 C57 84.9(2) . . . . ? C44 Si42 N41 Si41 -52.6(2) . . . . ? C46 Si42 N41 Si41 69.1(2) . . . . ? C45 Si42 N41 Si41 -171.89(16) . . . . ? C44 Si42 N41 Sn1 127.62(16) . . . . ? C46 Si42 N41 Sn1 -110.68(16) . . . . ? C45 Si42 N41 Sn1 8.30(17) . . . . ? C42 Si41 N41 Si42 -166.18(14) . . . . ? C41 Si41 N41 Si42 73.12(18) . . . . ? C43 Si41 N41 Si42 -46.00(19) . . . . ? C42 Si41 N41 Sn1 13.61(18) . . . . ? C41 Si41 N41 Sn1 -107.09(16) . . . . ? C43 Si41 N41 Sn1 133.79(15) . . . . ? O11 Sn1 N41 Si42 -137.32(12) . . . . ? O51 Sn1 N41 Si42 122.24(12) . . . . ? O11 Sn1 N41 Si41 42.87(13) . . . . ? O51 Sn1 N41 Si41 -57.57(13) . . . . ? C81 Si81 N81 Si82 -49.0(2) . . . . ? C82 Si81 N81 Si82 72.97(19) . . . . ? C83 Si81 N81 Si82 -169.29(15) . . . . ? C81 Si81 N81 Sn2 130.95(15) . . . . ? C82 Si81 N81 Sn2 -107.07(16) . . . . ? C83 Si81 N81 Sn2 10.66(17) . . . . ? C84 Si82 N81 Si81 75.06(18) . . . . ? C85 Si82 N81 Si81 -163.11(14) . . . . ? C86 Si82 N81 Si81 -43.47(18) . . . . ? C84 Si82 N81 Sn2 -104.89(16) . . . . ? C85 Si82 N81 Sn2 16.94(18) . . . . ? C86 Si82 N81 Sn2 136.58(15) . . . . ? O12 Sn2 N81 Si81 -142.35(11) . . . . ? O52 Sn2 N81 Si81 117.72(11) . . . . ? O12 Sn2 N81 Si82 37.60(13) . . . . ? O52 Sn2 N81 Si82 -62.33(13) . . . . ? C16 C11 C12 C13 -0.4(3) . . . . ? C17 C11 C12 C13 179.1(2) . . . . ? C16 C11 C12 C21 -179.7(2) . . . . ? C17 C11 C12 C21 -0.1(3) . . . . ? C11 C12 C13 C14 -0.2(4) . . . . ? C21 C12 C13 C14 179.1(2) . . . . ? C12 C13 C14 C15 0.7(4) . . . . ? C13 C14 C15 C16 -0.5(4) . . . . ? C14 C15 C16 C11 -0.1(4) . . . . ? C14 C15 C16 C31 176.1(2) . . . . ? C12 C11 C16 C15 0.6(3) . . . . ? C17 C11 C16 C15 -179.0(2) . . . . ? C12 C11 C16 C31 -175.5(2) . . . . ? C17 C11 C16 C31 4.9(3) . . . . ? Sn2 O12 C17 O11 49.7(3) . . . . ? Sn2 O12 C17 C11 -129.58(19) . . . . ? Sn1 O11 C17 O12 44.8(3) . . . . ? Sn1 O11 C17 C11 -135.96(18) . . . . ? C12 C11 C17 O12 68.6(3) . . . . ? C16 C11 C17 O12 -111.8(3) . . . . ? C12 C11 C17 O11 -110.7(3) . . . . ? C16 C11 C17 O11 68.8(3) . . . . ? C13 C12 C21 C22 -91.9(3) . . . . ? C11 C12 C21 C22 87.3(3) . . . . ? C13 C12 C21 C26 85.4(3) . . . . ? C11 C12 C21 C26 -95.4(3) . . . . ? C26 C21 C22 C23 3.8(4) . . . . ? C12 C21 C22 C23 -179.0(2) . . . . ? C26 C21 C22 C27 -175.3(3) . . . . ? C12 C21 C22 C27 2.0(4) . . . . ? C21 C22 C23 C24 -2.8(5) . . . . ? C27 C22 C23 C24 176.2(3) . . . . ? C22 C23 C24 C25 -0.8(5) . . . . ? C22 C23 C24 C28 177.2(3) . . . . ? C23 C24 C25 C26 3.6(5) . . . . ? C28 C24 C25 C26 -174.5(3) . . . . ? C24 C25 C26 C21 -2.6(4) . . . . ? C24 C25 C26 C29 175.6(3) . . . . ? C22 C21 C26 C25 -1.2(4) . . . . ? C12 C21 C26 C25 -178.5(2) . . . . ? C22 C21 C26 C29 -179.4(2) . . . . ? C12 C21 C26 C29 3.4(4) . . . . ? C15 C16 C31 C36 83.8(3) . . . . ? C11 C16 C31 C36 -100.1(3) . . . . ? C15 C16 C31 C32 -93.5(3) . . . . ? C11 C16 C31 C32 82.6(3) . . . . ? C36 C31 C32 C33 1.3(4) . . . . ? C16 C31 C32 C33 178.6(2) . . . . ? C36 C31 C32 C37 -176.6(3) . . . . ? C16 C31 C32 C37 0.7(4) . . . . ? C31 C32 C33 C34 -1.6(4) . . . . ? C37 C32 C33 C34 176.3(3) . . . . ? C32 C33 C34 C35 0.1(5) . . . . ? C32 C33 C34 C38 -179.0(3) . . . . ? C33 C34 C35 C36 1.8(5) . . . . ? C38 C34 C35 C36 -179.2(3) . . . . ? C34 C35 C36 C31 -2.0(4) . . . . ? C34 C35 C36 C39 178.6(3) . . . . ? C32 C31 C36 C35 0.5(4) . . . . ? C16 C31 C36 C35 -176.8(2) . . . . ? C32 C31 C36 C39 179.8(2) . . . . ? C16 C31 C36 C39 2.5(4) . . . . ? C56 C51 C52 C53 -0.3(4) . . . . ? C57 C51 C52 C53 179.8(2) . . . . ? C56 C51 C52 C61 177.2(2) . . . . ? C57 C51 C52 C61 -2.6(4) . . . . ? C51 C52 C53 C54 -0.5(4) . . . . ? C61 C52 C53 C54 -178.1(3) . . . . ? C52 C53 C54 C55 1.0(5) . . . . ? C53 C54 C55 C56 -0.7(5) . . . . ? C52 C51 C56 C55 0.6(4) . . . . ? C57 C51 C56 C55 -179.6(3) . . . . ? C52 C51 C56 C71 -179.3(3) . . . . ? C57 C51 C56 C71 0.6(4) . . . . ? C54 C55 C56 C51 -0.1(5) . . . . ? C54 C55 C56 C71 179.8(3) . . . . ? Sn1 O51 C57 O52 -43.0(4) . . . . ? Sn1 O51 C57 C51 136.0(2) . . . . ? Sn2 O52 C57 O51 -47.8(4) . . . . ? Sn2 O52 C57 C51 133.1(2) . . . . ? C56 C51 C57 O51 -86.0(3) . . . . ? C52 C51 C57 O51 93.8(3) . . . . ? C56 C51 C57 O52 93.0(3) . . . . ? C52 C51 C57 O52 -87.1(3) . . . . ? C51 C52 C61 C66 90.8(3) . . . . ? C53 C52 C61 C66 -91.7(3) . . . . ? C51 C52 C61 C62 -92.3(3) . . . . ? C53 C52 C61 C62 85.2(3) . . . . ? C66 C61 C62 C63 -1.1(4) . . . . ? C52 C61 C62 C63 -178.1(3) . . . . ? C66 C61 C62 C67 179.2(3) . . . . ? C52 C61 C62 C67 2.2(4) . . . . ? C61 C62 C63 C64 -0.5(5) . . . . ? C67 C62 C63 C64 179.2(3) . . . . ? C62 C63 C64 C65 1.3(5) . . . . ? C62 C63 C64 C68 -178.8(3) . . . . ? C63 C64 C65 C66 -0.5(5) . . . . ? C68 C64 C65 C66 179.6(3) . . . . ? C64 C65 C66 C61 -1.1(5) . . . . ? C64 C65 C66 C69 177.2(3) . . . . ? C62 C61 C66 C65 1.9(4) . . . . ? C52 C61 C66 C65 178.8(3) . . . . ? C62 C61 C66 C69 -176.4(3) . . . . ? C52 C61 C66 C69 0.5(4) . . . . ? C51 C56 C71 C76 88.8(3) . . . . ? C55 C56 C71 C76 -91.1(3) . . . . ? C51 C56 C71 C72 -90.9(3) . . . . ? C55 C56 C71 C72 89.2(3) . . . . ? C76 C71 C72 C73 -1.7(4) . . . . ? C56 C71 C72 C73 178.0(3) . . . . ? C76 C71 C72 C77 179.2(3) . . . . ? C56 C71 C72 C77 -1.1(4) . . . . ? C71 C72 C73 C74 -0.3(4) . . . . ? C77 C72 C73 C74 178.8(3) . . . . ? C72 C73 C74 C75 1.5(5) . . . . ? C72 C73 C74 C78 -178.4(3) . . . . ? C73 C74 C75 C76 -0.7(5) . . . . ? C78 C74 C75 C76 179.2(3) . . . . ? C74 C75 C76 C71 -1.2(4) . . . . ? C74 C75 C76 C79 178.7(3) . . . . ? C72 C71 C76 C75 2.4(4) . . . . ? C56 C71 C76 C75 -177.3(2) . . . . ? C72 C71 C76 C79 -177.5(3) . . . . ? C56 C71 C76 C79 2.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.448 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.072 #===END # CHEMICAL DATA data_6 _database_code_depnum_ccdc_archive 'CCDC 618669' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H94 Cl4 N2 O4 Si4 Sn2' _chemical_formula_weight 1470.97 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.8023(6) _cell_length_b 12.5695(9) _cell_length_c 14.2170(10) _cell_angle_alpha 67.446(3) _cell_angle_beta 65.690(2) _cell_angle_gamma 76.473(3) _cell_volume 1767.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.125 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.971 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9647 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6182 _reflns_number_gt 5588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+10.5254P] 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 6182 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1769 _refine_ls_wR_factor_gt 0.1723 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.15758(4) 0.93555(3) -0.13115(3) 0.02711(16) Uani 1 1 d . . . Si1 Si 0.21159(16) 0.82028(14) -0.31643(13) 0.0297(4) Uani 1 1 d . . . Si2 Si -0.04900(15) 0.93233(14) -0.23794(14) 0.0295(4) Uani 1 1 d . . . O1 O 0.0256(4) 0.8220(3) 0.0201(3) 0.0297(9) Uani 1 1 d . . . O2 O 0.0313(4) 1.0962(3) -0.1493(3) 0.0313(9) Uani 1 1 d . . . N1 N 0.0991(5) 0.8912(4) -0.2307(4) 0.0278(10) Uani 1 1 d . . . C1 C -0.0061(5) 0.8177(5) 0.1173(5) 0.0254(12) Uani 1 1 d . . . C2 C -0.0164(5) 0.6998(5) 0.2052(5) 0.0256(11) Uani 1 1 d . . . C3 C -0.1320(5) 0.6714(5) 0.2891(5) 0.0275(12) Uani 1 1 d . . . C4 C -0.1392(6) 0.5662(5) 0.3733(5) 0.0299(12) Uani 1 1 d . . . H4A H -0.2176 0.5474 0.4299 0.036 Uiso 1 1 calc R . . C5 C -0.0344(6) 0.4879(5) 0.3765(5) 0.0297(12) Uani 1 1 d . . . C6 C 0.0782(6) 0.5164(5) 0.2908(5) 0.0304(13) Uani 1 1 d . . . H6A H 0.1502 0.4634 0.2914 0.037 Uiso 1 1 calc R . . C7 C 0.0893(6) 0.6206(5) 0.2034(5) 0.0278(12) Uani 1 1 d . . . C8 C -0.0435(6) 0.3762(5) 0.4697(5) 0.0356(14) Uani 1 1 d . . . H8A H 0.0386 0.3320 0.4578 0.053 Uiso 1 1 calc R . . H8B H -0.1036 0.3308 0.4740 0.053 Uiso 1 1 calc R . . H8C H -0.0712 0.3930 0.5381 0.053 Uiso 1 1 calc R . . C10 C 0.2126(5) 0.6381(5) 0.1113(5) 0.0298(12) Uani 1 1 d . . . C11 C 0.2383(6) 0.5921(5) 0.0283(5) 0.0340(13) Uani 1 1 d . . . C12 C 0.3559(7) 0.6006(6) -0.0528(5) 0.0432(16) Uani 1 1 d . . . H12A H 0.3736 0.5690 -0.1088 0.052 Uiso 1 1 calc R . . C13 C 0.4488(6) 0.6535(6) -0.0556(6) 0.0446(17) Uani 1 1 d . . . C14 C 0.4206(6) 0.6990(6) 0.0274(6) 0.0442(16) Uani 1 1 d . . . H14A H 0.4825 0.7359 0.0270 0.053 Uiso 1 1 calc R . . C15 C 0.3046(6) 0.6920(5) 0.1107(6) 0.0372(14) Uani 1 1 d . . . C16 C 0.1412(7) 0.5333(7) 0.0284(6) 0.0463(17) Uani 1 1 d . . . H16A H 0.0646 0.5353 0.0913 0.070 Uiso 1 1 calc R . . H16B H 0.1722 0.4527 0.0328 0.070 Uiso 1 1 calc R . . H16C H 0.1235 0.5734 -0.0390 0.070 Uiso 1 1 calc R . . C17 C 0.5758(7) 0.6597(8) -0.1446(7) 0.058(2) Uani 1 1 d . . . H17A H 0.5776 0.6238 -0.1954 0.086 Uiso 1 1 calc R . . H17B H 0.6393 0.6184 -0.1122 0.086 Uiso 1 1 calc R . . H17C H 0.5933 0.7408 -0.1838 0.086 Uiso 1 1 calc R . . C18 C 0.2787(7) 0.7392(7) 0.2003(7) 0.0509(18) Uani 1 1 d . . . H18A H 0.3526 0.7734 0.1872 0.076 Uiso 1 1 calc R . . H18B H 0.2585 0.6765 0.2704 0.076 Uiso 1 1 calc R . . H18C H 0.2079 0.7986 0.2020 0.076 Uiso 1 1 calc R . . C20 C -0.2480(5) 0.7484(5) 0.2834(5) 0.0295(12) Uani 1 1 d . . . C21 C -0.2927(6) 0.7561(5) 0.2020(5) 0.0321(13) Uani 1 1 d . . . C22 C -0.3951(6) 0.8343(6) 0.1905(6) 0.0379(14) Uani 1 1 d . . . H22A H -0.4229 0.8427 0.1339 0.045 Uiso 1 1 calc R . . C23 C -0.4580(6) 0.9006(5) 0.2590(6) 0.0385(15) Uani 1 1 d . . . C24 C -0.4172(6) 0.8843(5) 0.3432(6) 0.0358(14) Uani 1 1 d . . . H24A H -0.4628 0.9248 0.3939 0.043 Uiso 1 1 calc R . . C25 C -0.3132(6) 0.8116(5) 0.3556(5) 0.0316(13) Uani 1 1 d . . . C26 C -0.2362(7) 0.6773(6) 0.1341(6) 0.0401(15) Uani 1 1 d . . . H26A H -0.2791 0.6951 0.0829 0.060 Uiso 1 1 calc R . . H26B H -0.2453 0.5968 0.1818 0.060 Uiso 1 1 calc R . . H26C H -0.1474 0.6886 0.0933 0.060 Uiso 1 1 calc R . . C27 C -0.5655(7) 0.9881(7) 0.2422(7) 0.0505(18) Uani 1 1 d . . . H27A H -0.5801 0.9878 0.1792 0.076 Uiso 1 1 calc R . . H27B H -0.5456 1.0652 0.2289 0.076 Uiso 1 1 calc R . . H27C H -0.6408 0.9682 0.3074 0.076 Uiso 1 1 calc R . . C28 C -0.2686(6) 0.8041(6) 0.4438(6) 0.0393(15) Uani 1 1 d . . . H28A H -0.3253 0.8541 0.4858 0.059 Uiso 1 1 calc R . . H28B H -0.1843 0.8294 0.4103 0.059 Uiso 1 1 calc R . . H28C H -0.2674 0.7240 0.4926 0.059 Uiso 1 1 calc R . . C31 C 0.3702(6) 0.8215(6) -0.3174(6) 0.0394(15) Uani 1 1 d . . . H31A H 0.3880 0.9016 -0.3388 0.059 Uiso 1 1 calc R . . H31B H 0.4329 0.7849 -0.3696 0.059 Uiso 1 1 calc R . . H31C H 0.3729 0.7787 -0.2443 0.059 Uiso 1 1 calc R . . C32 C 0.1865(7) 0.6643(6) -0.2744(6) 0.0432(16) Uani 1 1 d . . . H32A H 0.1042 0.6588 -0.2727 0.065 Uiso 1 1 calc R . . H32B H 0.1910 0.6234 -0.2017 0.065 Uiso 1 1 calc R . . H32C H 0.2512 0.6292 -0.3269 0.065 Uiso 1 1 calc R . . C33 C 0.2221(7) 0.8906(6) -0.4617(5) 0.0423(16) Uani 1 1 d . . . H33A H 0.2341 0.9727 -0.4852 0.064 Uiso 1 1 calc R . . H33B H 0.1448 0.8833 -0.4679 0.064 Uiso 1 1 calc R . . H33C H 0.2929 0.8527 -0.5080 0.064 Uiso 1 1 calc R . . C41 C -0.0510(6) 1.0742(6) -0.3467(5) 0.0359(14) Uani 1 1 d . . . H41A H -0.0250 1.1327 -0.3316 0.054 Uiso 1 1 calc R . . H41B H -0.1357 1.0975 -0.3482 0.054 Uiso 1 1 calc R . . H41C H 0.0065 1.0673 -0.4175 0.054 Uiso 1 1 calc R . . C42 C -0.1003(7) 0.8249(7) -0.2723(7) 0.0493(18) Uani 1 1 d . . . H42A H -0.0392 0.8156 -0.3413 0.074 Uiso 1 1 calc R . . H42B H -0.1820 0.8531 -0.2796 0.074 Uiso 1 1 calc R . . H42C H -0.1063 0.7502 -0.2140 0.074 Uiso 1 1 calc R . . C43 C -0.1724(6) 0.9414(6) -0.1061(5) 0.0388(15) Uani 1 1 d . . . H43A H -0.1520 0.9968 -0.0834 0.058 Uiso 1 1 calc R . . H43B H -0.1768 0.8651 -0.0502 0.058 Uiso 1 1 calc R . . H43C H -0.2532 0.9672 -0.1156 0.058 Uiso 1 1 calc R . . C101 C 0.4900(10) 0.531(2) 0.385(2) 0.225(14) Uani 1 1 d . . . H10A H 0.5592 0.5688 0.3190 0.270 Uiso 1 1 calc R . . H10B H 0.5282 0.4746 0.4372 0.270 Uiso 1 1 calc R . . Cl1 Cl 0.4277(5) 0.4596(4) 0.3506(4) 0.1426(17) Uani 1 1 d . . . Cl2 Cl 0.4041(4) 0.6332(4) 0.4408(4) 0.1247(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0293(2) 0.0272(2) 0.0272(2) -0.01055(17) -0.01384(17) 0.00313(16) Si1 0.0334(9) 0.0282(8) 0.0293(8) -0.0132(7) -0.0139(7) 0.0054(6) Si2 0.0305(8) 0.0295(8) 0.0312(9) -0.0106(7) -0.0158(7) 0.0027(6) O1 0.034(2) 0.027(2) 0.028(2) -0.0081(17) -0.0141(18) 0.0020(16) O2 0.040(2) 0.023(2) 0.037(2) -0.0106(17) -0.0224(19) 0.0062(17) N1 0.032(3) 0.029(3) 0.027(2) -0.013(2) -0.016(2) 0.005(2) C1 0.022(3) 0.027(3) 0.027(3) -0.009(2) -0.011(2) 0.003(2) C2 0.030(3) 0.023(3) 0.028(3) -0.012(2) -0.013(2) 0.003(2) C3 0.032(3) 0.026(3) 0.029(3) -0.012(2) -0.014(2) 0.001(2) C4 0.035(3) 0.027(3) 0.029(3) -0.008(2) -0.013(3) -0.004(2) C5 0.040(3) 0.025(3) 0.028(3) -0.010(2) -0.017(3) 0.001(2) C6 0.037(3) 0.024(3) 0.034(3) -0.011(2) -0.018(3) 0.005(2) C7 0.033(3) 0.025(3) 0.029(3) -0.011(2) -0.016(2) 0.004(2) C8 0.045(4) 0.027(3) 0.031(3) -0.006(3) -0.016(3) -0.001(3) C10 0.027(3) 0.025(3) 0.030(3) -0.003(2) -0.014(2) 0.008(2) C11 0.035(3) 0.027(3) 0.035(3) -0.010(3) -0.014(3) 0.006(2) C12 0.049(4) 0.038(4) 0.030(3) -0.011(3) -0.011(3) 0.012(3) C13 0.033(3) 0.039(4) 0.039(4) 0.003(3) -0.012(3) 0.007(3) C14 0.030(3) 0.041(4) 0.051(4) -0.005(3) -0.016(3) 0.002(3) C15 0.034(3) 0.032(3) 0.044(4) -0.008(3) -0.020(3) 0.004(3) C16 0.056(4) 0.048(4) 0.040(4) -0.026(3) -0.013(3) -0.002(3) C17 0.037(4) 0.059(5) 0.050(5) -0.003(4) -0.011(3) 0.009(3) C18 0.044(4) 0.061(5) 0.061(5) -0.027(4) -0.024(4) -0.004(3) C20 0.027(3) 0.027(3) 0.034(3) -0.008(2) -0.012(2) -0.003(2) C21 0.031(3) 0.030(3) 0.037(3) -0.010(3) -0.016(3) -0.001(2) C22 0.036(3) 0.038(4) 0.045(4) -0.010(3) -0.024(3) -0.001(3) C23 0.027(3) 0.028(3) 0.052(4) -0.006(3) -0.014(3) 0.001(2) C24 0.029(3) 0.032(3) 0.044(4) -0.017(3) -0.008(3) 0.000(2) C25 0.030(3) 0.029(3) 0.036(3) -0.009(3) -0.012(3) -0.004(2) C26 0.048(4) 0.038(4) 0.048(4) -0.020(3) -0.027(3) 0.001(3) C27 0.035(4) 0.050(4) 0.059(5) -0.014(4) -0.023(3) 0.013(3) C28 0.038(3) 0.041(4) 0.043(4) -0.021(3) -0.014(3) 0.000(3) C31 0.030(3) 0.039(4) 0.049(4) -0.024(3) -0.011(3) 0.007(3) C32 0.055(4) 0.031(3) 0.051(4) -0.019(3) -0.024(3) 0.005(3) C33 0.050(4) 0.044(4) 0.033(3) -0.018(3) -0.014(3) 0.004(3) C41 0.036(3) 0.042(4) 0.030(3) -0.010(3) -0.019(3) 0.006(3) C42 0.043(4) 0.051(4) 0.070(5) -0.031(4) -0.029(4) 0.004(3) C43 0.029(3) 0.046(4) 0.036(3) -0.010(3) -0.013(3) 0.003(3) C101 0.022(5) 0.23(2) 0.43(4) -0.23(3) 0.021(11) 0.003(8) Cl1 0.144(4) 0.113(3) 0.130(3) -0.050(3) -0.014(3) 0.012(3) Cl2 0.136(3) 0.114(3) 0.124(3) -0.056(2) -0.019(2) -0.033(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N1 2.093(5) . ? Sn1 O2 2.208(4) . ? Sn1 O1 2.240(4) . ? Si1 N1 1.729(5) . ? Si1 C31 1.871(7) . ? Si1 C33 1.872(7) . ? Si1 C32 1.875(7) . ? Si2 N1 1.737(5) . ? Si2 C41 1.862(6) . ? Si2 C43 1.867(7) . ? Si2 C42 1.887(7) . ? O1 C1 1.257(7) . ? O2 C1 1.259(7) 2_575 ? C1 O2 1.259(7) 2_575 ? C1 C2 1.520(8) . ? C2 C7 1.401(8) . ? C2 C3 1.404(8) . ? C3 C4 1.394(8) . ? C3 C20 1.493(8) . ? C4 C5 1.394(8) . ? C5 C6 1.390(9) . ? C5 C8 1.506(8) . ? C6 C7 1.406(8) . ? C7 C10 1.497(8) . ? C10 C11 1.401(9) . ? C10 C15 1.404(9) . ? C11 C12 1.388(10) . ? C11 C16 1.501(10) . ? C12 C13 1.389(11) . ? C13 C14 1.391(11) . ? C13 C17 1.507(10) . ? C14 C15 1.388(10) . ? C15 C18 1.498(10) . ? C20 C25 1.401(9) . ? C20 C21 1.422(9) . ? C21 C22 1.392(9) . ? C21 C26 1.500(9) . ? C22 C23 1.390(10) . ? C23 C24 1.394(10) . ? C23 C27 1.508(9) . ? C24 C25 1.380(9) . ? C25 C28 1.513(9) . ? C101 Cl1 1.591(19) . ? C101 Cl2 1.676(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 O2 89.53(17) . . ? N1 Sn1 O1 91.53(17) . . ? O2 Sn1 O1 98.15(15) . . ? N1 Si1 C31 110.9(3) . . ? N1 Si1 C33 112.6(3) . . ? C31 Si1 C33 105.7(3) . . ? N1 Si1 C32 113.0(3) . . ? C31 Si1 C32 106.2(3) . . ? C33 Si1 C32 108.0(3) . . ? N1 Si2 C41 110.4(3) . . ? N1 Si2 C43 113.0(3) . . ? C41 Si2 C43 109.2(3) . . ? N1 Si2 C42 111.9(3) . . ? C41 Si2 C42 107.0(3) . . ? C43 Si2 C42 105.0(4) . . ? C1 O1 Sn1 128.6(4) . . ? C1 O2 Sn1 135.8(4) 2_575 . ? Si1 N1 Si2 120.3(3) . . ? Si1 N1 Sn1 116.1(3) . . ? Si2 N1 Sn1 123.3(3) . . ? O1 C1 O2 125.4(5) . 2_575 ? O1 C1 C2 118.5(5) . . ? O2 C1 C2 116.1(5) 2_575 . ? C7 C2 C3 120.2(5) . . ? C7 C2 C1 120.1(5) . . ? C3 C2 C1 119.7(5) . . ? C4 C3 C2 119.5(5) . . ? C4 C3 C20 120.1(5) . . ? C2 C3 C20 120.3(5) . . ? C5 C4 C3 121.7(6) . . ? C6 C5 C4 117.8(5) . . ? C6 C5 C8 121.3(5) . . ? C4 C5 C8 120.9(6) . . ? C5 C6 C7 122.4(5) . . ? C2 C7 C6 118.3(5) . . ? C2 C7 C10 123.8(5) . . ? C6 C7 C10 117.8(5) . . ? C11 C10 C15 120.0(6) . . ? C11 C10 C7 118.5(5) . . ? C15 C10 C7 121.4(6) . . ? C12 C11 C10 118.5(6) . . ? C12 C11 C16 120.8(6) . . ? C10 C11 C16 120.6(6) . . ? C11 C12 C13 122.8(7) . . ? C12 C13 C14 117.5(6) . . ? C12 C13 C17 121.1(7) . . ? C14 C13 C17 121.4(7) . . ? C15 C14 C13 121.9(7) . . ? C14 C15 C10 119.3(6) . . ? C14 C15 C18 120.4(6) . . ? C10 C15 C18 120.3(6) . . ? C25 C20 C21 119.8(5) . . ? C25 C20 C3 122.2(5) . . ? C21 C20 C3 118.0(5) . . ? C22 C21 C20 118.4(6) . . ? C22 C21 C26 120.3(6) . . ? C20 C21 C26 121.1(5) . . ? C23 C22 C21 122.2(6) . . ? C22 C23 C24 117.7(6) . . ? C22 C23 C27 121.2(7) . . ? C24 C23 C27 121.1(6) . . ? C25 C24 C23 122.5(6) . . ? C24 C25 C20 119.1(6) . . ? C24 C25 C28 119.9(6) . . ? C20 C25 C28 121.0(5) . . ? Cl1 C101 Cl2 120.5(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.861 _refine_diff_density_min -2.046 _refine_diff_density_rms 0.148 #===END # CHEMICAL DATA data_8_CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 618670' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H36 Cl2 N O2 Si Sn' _chemical_formula_weight 648.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.5733(6) _cell_length_b 11.8229(6) _cell_length_c 13.8362(7) _cell_angle_alpha 67.2930(10) _cell_angle_beta 79.9680(10) _cell_angle_gamma 89.7190(10) _cell_volume 1567.46(14) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max .45 _exptl_crystal_size_mid .45 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 662 _exptl_absorpt_coefficient_mu 1.048 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11645 _diffrn_reflns_av_R_equivalents 0.0135 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5513 _reflns_number_gt 5062 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+3.2215P] 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 5513 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 -0.00684(2) 0.12677(2) 0.52924(2) 0.03560(12) Uani 1 1 d . . . Si1 Si 0.15899(11) -0.11503(11) 0.66540(10) 0.0404(3) Uani 1 1 d . . . O1 O 0.1929(3) 0.1661(3) 0.4547(2) 0.0392(6) Uani 1 1 d . . . O2 O 0.0935(3) 0.3246(3) 0.3630(2) 0.0434(7) Uani 1 1 d . . . N1 N 0.0519(3) -0.0626(2) 0.5847(2) 0.0231(6) Uani 1 1 d . . . C1 C 0.3241(4) 0.3394(4) 0.3264(3) 0.0338(8) Uani 1 1 d . . . C2 C 0.3848(4) 0.4049(4) 0.3737(3) 0.0362(8) Uani 1 1 d . . . C3 C 0.5065(4) 0.4614(4) 0.3242(4) 0.0476(11) Uani 1 1 d . . . H3A H 0.5484 0.5053 0.3549 0.057 Uiso 1 1 calc R . . C4 C 0.5667(4) 0.4538(5) 0.2301(4) 0.0538(12) Uani 1 1 d . . . H4A H 0.6497 0.4915 0.1976 0.065 Uiso 1 1 calc R . . C5 C 0.5055(4) 0.3910(5) 0.1834(4) 0.0507(11) Uani 1 1 d . . . H5A H 0.5472 0.3871 0.1191 0.061 Uiso 1 1 calc R . . C6 C 0.3827(4) 0.3332(4) 0.2303(3) 0.0387(9) Uani 1 1 d . . . C7 C 0.1939(4) 0.2749(4) 0.3827(3) 0.0332(8) Uani 1 1 d . . . C8 C 0.3151(4) 0.4114(4) 0.4753(3) 0.0362(9) Uani 1 1 d . . . C9 C 0.2260(4) 0.4998(4) 0.4714(3) 0.0394(9) Uani 1 1 d . . . C10 C 0.1511(4) 0.4954(4) 0.5665(4) 0.0432(10) Uani 1 1 d . . . H10A H 0.0903 0.5543 0.5642 0.052 Uiso 1 1 calc R . . C11 C 0.1640(4) 0.4066(4) 0.6643(3) 0.0409(9) Uani 1 1 d . . . C12 C 0.2571(4) 0.3235(4) 0.6664(3) 0.0407(9) Uani 1 1 d . . . H12A H 0.2688 0.2647 0.7326 0.049 Uiso 1 1 calc R . . C13 C 0.3340(4) 0.3242(4) 0.5737(3) 0.0376(9) Uiso 1 1 d . . . C14 C 0.4352(5) 0.2335(5) 0.5798(4) 0.0537(12) Uani 1 1 d . . . H14A H 0.4341 0.1807 0.6538 0.080 Uiso 1 1 calc R . . H14B H 0.5191 0.2772 0.5483 0.080 Uiso 1 1 calc R . . H14C H 0.4178 0.1838 0.5412 0.080 Uiso 1 1 calc R . . C15 C 0.0766(5) 0.3994(5) 0.7660(4) 0.0556(12) Uani 1 1 d . . . H15A H 0.0995 0.3324 0.8263 0.083 Uiso 1 1 calc R . . H15B H -0.0121 0.3851 0.7618 0.083 Uiso 1 1 calc R . . H15C H 0.0866 0.4761 0.7750 0.083 Uiso 1 1 calc R . . C16 C 0.2083(5) 0.5982(4) 0.3669(4) 0.0535(11) Uani 1 1 d . . . H16A H 0.1426 0.6508 0.3801 0.080 Uiso 1 1 calc R . . H16B H 0.1819 0.5602 0.3221 0.080 Uiso 1 1 calc R . . H16C H 0.2889 0.6470 0.3312 0.080 Uiso 1 1 calc R . . C17 C 0.3160(4) 0.2687(4) 0.1768(3) 0.0390(9) Uani 1 1 d . . . C18 C 0.2424(4) 0.3353(4) 0.1015(3) 0.0440(10) Uani 1 1 d . . . C19 C 0.1832(5) 0.2744(5) 0.0513(4) 0.0527(11) Uani 1 1 d . . . H19A H 0.1347 0.3193 0.0000 0.063 Uiso 1 1 calc R . . C20 C 0.1928(5) 0.1511(5) 0.0736(4) 0.0547(12) Uani 1 1 d . . . C21 C 0.2643(5) 0.0863(5) 0.1505(4) 0.0551(12) Uani 1 1 d . . . H21A H 0.2705 0.0015 0.1682 0.066 Uiso 1 1 calc R . . C22 C 0.3268(5) 0.1426(4) 0.2018(4) 0.0465(10) Uani 1 1 d . . . C23 C 0.4077(6) 0.0686(5) 0.2809(5) 0.0680(15) Uani 1 1 d . . . H23A H 0.4030 -0.0162 0.2880 0.102 Uiso 1 1 calc R . . H23B H 0.3756 0.0724 0.3496 0.102 Uiso 1 1 calc R . . H23C H 0.4964 0.1021 0.2560 0.102 Uiso 1 1 calc R . . C24 C 0.1282(7) 0.0876(7) 0.0173(5) 0.0788(18) Uani 1 1 d . . . H24A H 0.0827 0.1466 -0.0331 0.118 Uiso 1 1 calc R . . H24B H 0.0677 0.0222 0.0692 0.118 Uiso 1 1 calc R . . H24C H 0.1928 0.0534 -0.0206 0.118 Uiso 1 1 calc R . . C25 C 0.2224(6) 0.4681(5) 0.0777(4) 0.0593(13) Uani 1 1 d . . . H25A H 0.1687 0.4982 0.0241 0.089 Uiso 1 1 calc R . . H25B H 0.3050 0.5150 0.0514 0.089 Uiso 1 1 calc R . . H25C H 0.1806 0.4771 0.1423 0.089 Uiso 1 1 calc R . . C102 C 0.1638(6) -0.0104(5) 0.7362(5) 0.0657(14) Uani 1 1 d . . . H10B H 0.0798 -0.0140 0.7791 0.099 Uiso 1 1 calc R . . H10C H 0.1869 0.0730 0.6845 0.099 Uiso 1 1 calc R . . H10D H 0.2272 -0.0356 0.7820 0.099 Uiso 1 1 calc R . . C103 C 0.1104(5) -0.2729(5) 0.7626(5) 0.0649(14) Uani 1 1 d . . . H10E H 0.0276 -0.2740 0.8063 0.097 Uiso 1 1 calc R . . H10F H 0.1742 -0.3015 0.8077 0.097 Uiso 1 1 calc R . . H10G H 0.1037 -0.3263 0.7250 0.097 Uiso 1 1 calc R . . C104 C 0.3172(5) -0.1149(6) 0.5837(4) 0.0622(14) Uani 1 1 d . . . H10H H 0.3112 -0.1708 0.5484 0.093 Uiso 1 1 calc R . . H10I H 0.3809 -0.1411 0.6292 0.093 Uiso 1 1 calc R . . H10J H 0.3426 -0.0325 0.5305 0.093 Uiso 1 1 calc R . . Cl1 Cl 0.5005(2) 0.8323(2) 0.13638(18) 0.1042(6) Uiso 1 1 d . . . Cl3 Cl 0.3247(3) 0.8020(3) 0.0089(2) 0.1238(8) Uiso 1 1 d . . . C501 C 0.4578(8) 0.7514(8) 0.0663(6) 0.095(2) Uiso 1 1 d . . . H50B H 0.4402 0.6647 0.1144 0.114 Uiso 1 1 calc R . . H50C H 0.5309 0.7566 0.0100 0.114 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 0.02771(16) 0.03589(17) 0.04439(18) -0.01921(13) -0.00146(11) 0.00074(11) Si1 0.0327(6) 0.0425(6) 0.0451(6) -0.0144(5) -0.0112(5) -0.0004(5) O1 0.0298(14) 0.0356(15) 0.0503(16) -0.0161(13) -0.0038(12) -0.0036(11) O2 0.0287(15) 0.0458(16) 0.0555(18) -0.0201(14) -0.0063(13) 0.0015(12) N1 0.0173(13) 0.0206(13) 0.0316(15) -0.0097(11) -0.0064(11) -0.0016(10) C1 0.0271(19) 0.035(2) 0.041(2) -0.0171(17) -0.0039(16) -0.0020(15) C2 0.031(2) 0.038(2) 0.045(2) -0.0223(18) -0.0053(16) -0.0011(16) C3 0.036(2) 0.048(2) 0.064(3) -0.030(2) -0.004(2) -0.0104(19) C4 0.034(2) 0.062(3) 0.065(3) -0.030(2) 0.006(2) -0.016(2) C5 0.040(2) 0.063(3) 0.048(2) -0.029(2) 0.0106(19) -0.010(2) C6 0.034(2) 0.041(2) 0.045(2) -0.0220(18) -0.0038(17) -0.0022(17) C7 0.030(2) 0.036(2) 0.040(2) -0.0223(17) -0.0044(16) -0.0035(16) C8 0.0288(19) 0.040(2) 0.048(2) -0.0265(18) -0.0062(17) -0.0059(16) C9 0.040(2) 0.038(2) 0.045(2) -0.0207(18) -0.0079(18) 0.0010(17) C10 0.043(2) 0.041(2) 0.052(2) -0.026(2) -0.0087(19) 0.0069(18) C11 0.039(2) 0.045(2) 0.046(2) -0.0262(19) -0.0076(18) 0.0003(18) C12 0.044(2) 0.040(2) 0.043(2) -0.0195(18) -0.0149(18) -0.0003(18) C14 0.049(3) 0.059(3) 0.062(3) -0.031(2) -0.018(2) 0.018(2) C15 0.055(3) 0.067(3) 0.048(3) -0.028(2) -0.005(2) 0.007(2) C16 0.061(3) 0.048(3) 0.049(3) -0.018(2) -0.007(2) 0.010(2) C17 0.035(2) 0.048(2) 0.038(2) -0.0234(18) -0.0010(17) -0.0017(17) C18 0.046(2) 0.051(3) 0.035(2) -0.0181(19) -0.0013(18) 0.0014(19) C19 0.054(3) 0.068(3) 0.042(2) -0.025(2) -0.015(2) 0.007(2) C20 0.053(3) 0.072(3) 0.053(3) -0.039(3) -0.011(2) -0.003(2) C21 0.067(3) 0.051(3) 0.063(3) -0.038(2) -0.015(2) 0.005(2) C22 0.049(3) 0.051(3) 0.049(2) -0.028(2) -0.011(2) 0.006(2) C23 0.088(4) 0.064(3) 0.074(4) -0.040(3) -0.040(3) 0.029(3) C24 0.084(4) 0.100(5) 0.078(4) -0.058(4) -0.025(3) -0.007(4) C25 0.072(3) 0.051(3) 0.049(3) -0.014(2) -0.008(2) 0.003(2) C102 0.075(4) 0.068(3) 0.064(3) -0.032(3) -0.026(3) 0.002(3) C103 0.058(3) 0.052(3) 0.071(3) -0.005(3) -0.022(3) -0.001(2) C104 0.038(3) 0.084(4) 0.064(3) -0.026(3) -0.014(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N1 2.116(3) 2_556 ? Sn1 O1 2.149(3) . ? Sn1 N1 2.194(3) . ? Sn1 O2 2.628(3) . ? Sn1 Sn1 3.3896(5) 2_556 ? Si1 N1 1.677(3) . ? Si1 C103 1.840(5) . ? Si1 C104 1.849(5) . ? Si1 C102 1.857(5) . ? O1 C7 1.286(5) . ? O2 C7 1.231(5) . ? N1 Sn1 2.116(3) 2_556 ? C1 C6 1.396(6) . ? C1 C2 1.407(5) . ? C1 C7 1.503(5) . ? C2 C3 1.385(6) . ? C2 C8 1.499(6) . ? C3 C4 1.383(7) . ? C3 H3A 0.9400 . ? C4 C5 1.381(7) . ? C4 H4A 0.9400 . ? C5 C6 1.395(6) . ? C5 H5A 0.9400 . ? C6 C17 1.499(6) . ? C8 C9 1.396(6) . ? C8 C13 1.402(6) . ? C9 C10 1.395(6) . ? C9 C16 1.508(6) . ? C10 C11 1.385(6) . ? C10 H10A 0.9400 . ? C11 C12 1.384(6) . ? C11 C15 1.515(6) . ? C12 C13 1.391(6) . ? C12 H12A 0.9400 . ? C13 C14 1.501(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.398(6) . ? C17 C22 1.403(6) . ? C18 C19 1.391(7) . ? C18 C25 1.496(7) . ? C19 C20 1.375(8) . ? C19 H19A 0.9400 . ? C20 C21 1.392(7) . ? C20 C24 1.510(7) . ? C21 C22 1.384(6) . ? C21 H21A 0.9400 . ? C22 C23 1.508(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C102 H10B 0.9700 . ? C102 H10C 0.9700 . ? C102 H10D 0.9700 . ? C103 H10E 0.9700 . ? C103 H10F 0.9700 . ? C103 H10G 0.9700 . ? C104 H10H 0.9700 . ? C104 H10I 0.9700 . ? C104 H10J 0.9700 . ? Cl1 C501 1.712(8) . ? Cl3 C501 1.727(8) . ? C501 H50B 0.9800 . ? C501 H50C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 O1 92.72(11) 2_556 . ? N1 Sn1 N1 76.28(11) 2_556 . ? O1 Sn1 N1 81.98(10) . . ? N1 Sn1 O2 84.98(10) 2_556 . ? O1 Sn1 O2 53.66(10) . . ? N1 Sn1 O2 130.86(10) . . ? N1 Sn1 Sn1 38.96(7) 2_556 2_556 ? O1 Sn1 Sn1 86.52(7) . 2_556 ? N1 Sn1 Sn1 37.32(7) . 2_556 ? O2 Sn1 Sn1 111.64(7) . 2_556 ? N1 Si1 C103 111.0(2) . . ? N1 Si1 C104 108.8(2) . . ? C103 Si1 C104 108.7(3) . . ? N1 Si1 C102 106.7(2) . . ? C103 Si1 C102 109.8(3) . . ? C104 Si1 C102 111.8(3) . . ? C7 O1 Sn1 102.6(2) . . ? C7 O2 Sn1 81.6(2) . . ? Si1 N1 Sn1 128.02(16) . 2_556 ? Si1 N1 Sn1 123.99(15) . . ? Sn1 N1 Sn1 103.72(11) 2_556 . ? C6 C1 C2 121.3(4) . . ? C6 C1 C7 120.4(3) . . ? C2 C1 C7 118.3(3) . . ? C3 C2 C1 118.7(4) . . ? C3 C2 C8 122.5(4) . . ? C1 C2 C8 118.8(3) . . ? C4 C3 C2 120.5(4) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C1 118.0(4) . . ? C5 C6 C17 120.4(4) . . ? C1 C6 C17 121.6(4) . . ? O2 C7 O1 121.6(4) . . ? O2 C7 C1 122.0(4) . . ? O1 C7 C1 116.4(3) . . ? C9 C8 C13 120.4(4) . . ? C9 C8 C2 119.7(4) . . ? C13 C8 C2 119.9(4) . . ? C10 C9 C8 118.9(4) . . ? C10 C9 C16 119.8(4) . . ? C8 C9 C16 121.4(4) . . ? C11 C10 C9 121.7(4) . . ? C11 C10 H10A 119.1 . . ? C9 C10 H10A 119.1 . . ? C12 C11 C10 118.2(4) . . ? C12 C11 C15 121.0(4) . . ? C10 C11 C15 120.8(4) . . ? C11 C12 C13 122.1(4) . . ? C11 C12 H12A 119.0 . . ? C13 C12 H12A 119.0 . . ? C12 C13 C8 118.6(4) . . ? C12 C13 C14 120.3(4) . . ? C8 C13 C14 121.1(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C9 C16 H16A 109.5 . . ? C9 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C9 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 120.0(4) . . ? C18 C17 C6 119.4(4) . . ? C22 C17 C6 120.6(4) . . ? C19 C18 C17 118.5(4) . . ? C19 C18 C25 120.1(4) . . ? C17 C18 C25 121.4(4) . . ? C20 C19 C18 122.8(4) . . ? C20 C19 H19A 118.6 . . ? C18 C19 H19A 118.6 . . ? C19 C20 C21 117.5(4) . . ? C19 C20 C24 121.6(5) . . ? C21 C20 C24 120.9(5) . . ? C22 C21 C20 122.1(5) . . ? C22 C21 H21A 119.0 . . ? C20 C21 H21A 119.0 . . ? C21 C22 C17 119.0(4) . . ? C21 C22 C23 119.6(4) . . ? C17 C22 C23 121.3(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C18 C25 H25A 109.5 . . ? C18 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C18 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C102 H10B 109.5 . . ? Si1 C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? Si1 C102 H10D 109.5 . . ? H10B C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? Si1 C103 H10E 109.5 . . ? Si1 C103 H10F 109.5 . . ? H10E C103 H10F 109.5 . . ? Si1 C103 H10G 109.5 . . ? H10E C103 H10G 109.5 . . ? H10F C103 H10G 109.5 . . ? Si1 C104 H10H 109.5 . . ? Si1 C104 H10I 109.5 . . ? H10H C104 H10I 109.5 . . ? Si1 C104 H10J 109.5 . . ? H10H C104 H10J 109.5 . . ? H10I C104 H10J 109.5 . . ? Cl1 C501 Cl3 114.1(5) . . ? Cl1 C501 H50B 108.7 . . ? Cl3 C501 H50B 108.7 . . ? Cl1 C501 H50C 108.7 . . ? Cl3 C501 H50C 108.7 . . ? H50B C501 H50C 107.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.209 _refine_diff_density_min -1.458 _refine_diff_density_rms 0.089 #===END # CHEMICAL DATA data_8_Et2O _database_code_depnum_ccdc_archive 'CCDC 618671' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H68 N2 O4 Si2 Sn2, C4 H10 O' _chemical_formula_sum 'C60 H78 N2 O5 Si2 Sn2' _chemical_formula_weight 1200.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8922(3) _cell_length_b 11.7957(3) _cell_length_c 12.3240(3) _cell_angle_alpha 77.2409(16) _cell_angle_beta 75.5426(16) _cell_angle_gamma 87.3334(17) _cell_volume 1495.34(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20318 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description chip _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.922 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details 'Shelxtl 6.10 (Bruker-AXS, 2000)' _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_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25297 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.62 _reflns_number_total 6863 _reflns_number_gt 5809 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 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^)+(0.0351P)^2^+1.9364P] 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 SHELXL _refine_ls_extinction_coef 0.0061(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6863 _refine_ls_number_parameters 353 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0920 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si -0.17154(9) 0.98879(8) 0.35128(8) 0.0329(2) Uani 1 1 d . . . Sn1 Sn 0.00339(2) 0.852184(18) 0.534130(18) 0.02740(9) Uani 1 1 d . . . N1 N -0.0551(2) 0.99136(18) 0.41738(18) 0.0161(4) Uani 1 1 d . . . O1 O 0.1997(2) 0.86713(19) 0.43657(19) 0.0314(5) Uani 1 1 d . . . O2 O 0.0958(2) 0.7695(2) 0.3544(2) 0.0339(5) Uani 1 1 d . . . C1 C 0.1966(3) 0.8058(2) 0.3630(3) 0.0261(6) Uani 1 1 d . . . C2 C 0.3222(3) 0.7760(3) 0.2906(3) 0.0287(6) Uani 1 1 d . . . C3 C 0.3828(3) 0.8544(3) 0.1899(3) 0.0343(7) Uani 1 1 d . . . C4 C 0.4983(4) 0.8227(4) 0.1259(3) 0.0472(10) Uani 1 1 d . . . H4 H 0.5402 0.8740 0.0569 0.057 Uiso 1 1 calc R . . C5 C 0.5527(4) 0.7173(4) 0.1619(4) 0.0561(12) Uani 1 1 d . . . H5 H 0.6315 0.6967 0.1172 0.067 Uiso 1 1 calc R . . C6 C 0.4934(4) 0.6418(4) 0.2623(4) 0.0493(10) Uani 1 1 d . . . H6 H 0.5324 0.5701 0.2864 0.059 Uiso 1 1 calc R . . C7 C 0.3778(3) 0.6693(3) 0.3282(3) 0.0347(7) Uani 1 1 d . . . C8 C 0.3239(3) 0.9699(3) 0.1579(3) 0.0333(7) Uani 1 1 d . . . C9 C 0.2289(3) 0.9831(3) 0.0968(3) 0.0354(7) Uani 1 1 d . . . C10 C 0.1697(3) 1.0905(3) 0.0770(3) 0.0405(8) Uani 1 1 d . . . H10 H 0.1058 1.0998 0.0356 0.049 Uiso 1 1 calc R . . C11 C 0.2014(4) 1.1843(3) 0.1160(3) 0.0417(9) Uani 1 1 d . . . C12 C 0.2984(4) 1.1705(3) 0.1723(3) 0.0407(8) Uani 1 1 d . . . H12 H 0.3226 1.2344 0.1978 0.049 Uiso 1 1 calc R . . C13 C 0.3609(3) 1.0659(3) 0.1923(3) 0.0384(8) Uani 1 1 d . . . C14 C 0.1946(4) 0.8830(4) 0.0528(4) 0.0478(9) Uani 1 1 d . . . H14A H 0.1340 0.9089 0.0057 0.072 Uiso 1 1 calc R . . H14B H 0.1561 0.8205 0.1178 0.072 Uiso 1 1 calc R . . H14C H 0.2711 0.8542 0.0063 0.072 Uiso 1 1 calc R . . C15 C 0.1333(4) 1.2991(3) 0.0970(4) 0.0546(11) Uani 1 1 d . . . H15A H 0.0797 1.2982 0.0442 0.082 Uiso 1 1 calc R . . H15B H 0.1958 1.3625 0.0641 0.082 Uiso 1 1 calc R . . H15C H 0.0805 1.3111 0.1705 0.082 Uiso 1 1 calc R . . C16 C 0.4710(4) 1.0562(4) 0.2482(4) 0.0539(10) Uani 1 1 d . . . H16A H 0.5499 1.0466 0.1918 0.081 Uiso 1 1 calc R . . H16B H 0.4578 0.9889 0.3128 0.081 Uiso 1 1 calc R . . H16C H 0.4768 1.1270 0.2760 0.081 Uiso 1 1 calc R . . C17 C 0.3132(3) 0.5939(3) 0.4412(3) 0.0323(7) Uani 1 1 d . . . C18 C 0.2220(4) 0.5117(3) 0.4480(3) 0.0367(8) Uani 1 1 d . . . C19 C 0.1534(4) 0.4531(3) 0.5557(3) 0.0409(8) Uani 1 1 d . . . H19 H 0.0915 0.3969 0.5602 0.049 Uiso 1 1 calc R . . C20 C 0.1731(4) 0.4749(3) 0.6566(3) 0.0391(8) Uani 1 1 d . . . C21 C 0.2668(4) 0.5538(3) 0.6478(3) 0.0374(8) Uani 1 1 d . . . H21 H 0.2829 0.5679 0.7160 0.045 Uiso 1 1 calc R . . C22 C 0.3389(3) 0.6136(3) 0.5417(3) 0.0355(8) Uani 1 1 d . . . C23 C 0.1965(4) 0.4866(4) 0.3410(3) 0.0510(10) Uani 1 1 d . . . H23A H 0.1214 0.4362 0.3618 0.077 Uiso 1 1 calc R . . H23B H 0.2698 0.4475 0.3013 0.077 Uiso 1 1 calc R . . H23C H 0.1816 0.5597 0.2903 0.077 Uiso 1 1 calc R . . C24 C 0.0945(5) 0.4147(4) 0.7724(3) 0.0547(11) Uani 1 1 d . . . H24A H 0.1492 0.3655 0.8152 0.082 Uiso 1 1 calc R . . H24B H 0.0292 0.3664 0.7620 0.082 Uiso 1 1 calc R . . H24C H 0.0540 0.4729 0.8151 0.082 Uiso 1 1 calc R . . C25 C 0.4435(4) 0.6959(3) 0.5366(4) 0.0488(10) Uani 1 1 d . . . H25A H 0.4500 0.6954 0.6146 0.073 Uiso 1 1 calc R . . H25B H 0.4243 0.7747 0.4992 0.073 Uiso 1 1 calc R . . H25C H 0.5242 0.6710 0.4925 0.073 Uiso 1 1 calc R . . C26 C -0.1958(4) 1.1406(3) 0.2791(4) 0.0477(10) Uani 1 1 d . . . H26A H -0.2191 1.1888 0.3364 0.072 Uiso 1 1 calc R . . H26B H -0.2639 1.1425 0.2396 0.072 Uiso 1 1 calc R . . H26C H -0.1172 1.1708 0.2231 0.072 Uiso 1 1 calc R . . C27 C -0.3160(4) 0.9282(5) 0.4603(4) 0.0647(13) Uani 1 1 d . . . H27A H -0.2993 0.8492 0.4990 0.097 Uiso 1 1 calc R . . H27B H -0.3851 0.9261 0.4228 0.097 Uiso 1 1 calc R . . H27C H -0.3403 0.9772 0.5168 0.097 Uiso 1 1 calc R . . C28 C -0.1295(5) 0.8990(4) 0.2434(4) 0.0607(12) Uani 1 1 d . . . H28A H -0.0510 0.9289 0.1871 0.091 Uiso 1 1 calc R . . H28B H -0.1980 0.9015 0.2043 0.091 Uiso 1 1 calc R . . H28C H -0.1170 0.8185 0.2811 0.091 Uiso 1 1 calc R . . C41 C 0.7604(14) 0.3918(9) 0.0252(10) 0.087(3) Uani 0.50 1 d PDU A -1 H41A H 0.7849 0.3221 0.0748 0.131 Uiso 0.50 1 calc PR A -1 H41B H 0.7918 0.4611 0.0416 0.131 Uiso 0.50 1 calc PR A -1 H41C H 0.7971 0.3891 -0.0554 0.131 Uiso 0.50 1 calc PR A -1 C42 C 0.6174(16) 0.3964(17) 0.047(2) 0.089(5) Uani 0.50 1 d PDU A -1 H42A H 0.5867 0.3294 0.0249 0.107 Uiso 0.50 1 calc PR A -1 H42B H 0.5804 0.3895 0.1306 0.107 Uiso 0.50 1 calc PR A -1 O43 O 0.574(2) 0.5033(18) -0.015(2) 0.078(3) Uani 0.50 1 d PDU A -1 C44 C 0.437(3) 0.512(3) 0.005(3) 0.080(5) Uani 0.50 1 d PDU A -1 H44A H 0.3981 0.5178 0.0847 0.096 Uiso 0.50 1 calc PR A -1 H44B H 0.4014 0.4422 -0.0098 0.096 Uiso 0.50 1 calc PR A -1 C45 C 0.4117(19) 0.620(2) -0.079(2) 0.099(6) Uani 0.50 1 d PDU A -1 H45A H 0.3200 0.6301 -0.0690 0.148 Uiso 0.50 1 calc PR A -1 H45B H 0.4510 0.6128 -0.1575 0.148 Uiso 0.50 1 calc PR A -1 H45C H 0.4477 0.6880 -0.0635 0.148 Uiso 0.50 1 calc PR 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 Si1 0.0285(5) 0.0362(5) 0.0370(5) -0.0077(4) -0.0134(4) -0.0016(4) Sn1 0.02419(13) 0.02690(13) 0.02885(13) -0.00396(8) -0.00353(9) -0.00322(8) N1 0.0142(11) 0.0172(10) 0.0185(11) -0.0056(9) -0.0054(9) 0.0012(8) O1 0.0255(11) 0.0330(12) 0.0344(12) -0.0096(10) -0.0029(9) 0.0002(9) O2 0.0244(12) 0.0371(12) 0.0402(13) -0.0099(10) -0.0062(10) -0.0011(9) C1 0.0266(16) 0.0208(13) 0.0276(15) -0.0005(12) -0.0051(12) 0.0015(12) C2 0.0241(15) 0.0308(16) 0.0292(16) -0.0049(13) -0.0046(13) 0.0019(12) C3 0.0265(17) 0.0402(18) 0.0304(16) -0.0005(14) -0.0026(13) 0.0012(14) C4 0.034(2) 0.058(2) 0.0357(19) 0.0017(18) 0.0061(15) 0.0044(17) C5 0.032(2) 0.067(3) 0.052(2) -0.005(2) 0.0101(18) 0.0183(19) C6 0.037(2) 0.049(2) 0.051(2) -0.0021(18) -0.0010(17) 0.0153(17) C7 0.0301(17) 0.0321(16) 0.0385(18) -0.0057(14) -0.0049(14) 0.0045(14) C8 0.0295(17) 0.0372(17) 0.0252(15) 0.0020(13) 0.0007(13) -0.0019(14) C9 0.0332(18) 0.0419(18) 0.0279(16) -0.0028(14) -0.0055(14) -0.0027(15) C10 0.0325(19) 0.050(2) 0.0328(18) 0.0057(16) -0.0093(15) 0.0035(16) C11 0.040(2) 0.0399(19) 0.0356(18) 0.0005(15) -0.0007(16) 0.0026(16) C12 0.039(2) 0.0378(18) 0.0390(19) -0.0035(15) -0.0009(16) -0.0075(15) C13 0.0357(19) 0.0425(19) 0.0317(17) 0.0016(15) -0.0056(15) -0.0069(15) C14 0.047(2) 0.056(2) 0.046(2) -0.0148(19) -0.0186(18) 0.0029(19) C15 0.057(3) 0.040(2) 0.056(3) -0.0015(19) -0.004(2) 0.0067(19) C16 0.048(2) 0.061(3) 0.057(3) -0.011(2) -0.021(2) -0.007(2) C17 0.0272(16) 0.0276(15) 0.0405(18) -0.0051(14) -0.0089(14) 0.0079(13) C18 0.042(2) 0.0265(16) 0.0413(19) -0.0071(14) -0.0101(16) 0.0025(14) C19 0.044(2) 0.0289(17) 0.047(2) -0.0032(15) -0.0110(17) -0.0049(15) C20 0.044(2) 0.0293(16) 0.0400(19) 0.0020(14) -0.0107(16) 0.0014(15) C21 0.042(2) 0.0329(17) 0.0381(18) -0.0028(14) -0.0169(16) 0.0038(15) C22 0.0311(18) 0.0294(16) 0.046(2) -0.0041(14) -0.0142(15) 0.0041(13) C23 0.063(3) 0.049(2) 0.044(2) -0.0155(18) -0.012(2) -0.008(2) C24 0.064(3) 0.047(2) 0.042(2) 0.0045(18) -0.005(2) -0.010(2) C25 0.043(2) 0.046(2) 0.059(2) -0.0048(19) -0.0200(19) -0.0063(18) C26 0.047(2) 0.046(2) 0.055(2) -0.0049(18) -0.027(2) 0.0048(18) C27 0.039(2) 0.085(3) 0.066(3) 0.002(3) -0.016(2) -0.025(2) C28 0.065(3) 0.069(3) 0.070(3) -0.035(2) -0.042(3) 0.016(2) C41 0.140(8) 0.047(5) 0.079(7) -0.005(5) -0.040(8) -0.006(6) C42 0.138(8) 0.043(6) 0.074(11) -0.003(6) -0.009(8) -0.020(6) O43 0.097(5) 0.054(6) 0.076(7) -0.016(5) -0.002(6) -0.013(5) C44 0.102(7) 0.075(11) 0.067(10) -0.024(8) -0.012(9) -0.029(9) C45 0.117(12) 0.118(15) 0.077(13) -0.029(10) -0.047(11) 0.000(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.674(2) . ? Si1 C28 1.837(4) . ? Si1 C27 1.849(4) . ? Si1 C26 1.854(4) . ? Sn1 N1 2.119(2) . ? Sn1 O1 2.169(2) . ? Sn1 N1 2.198(2) 2_576 ? N1 Sn1 2.198(2) 2_576 ? O1 C1 1.286(4) . ? O2 C1 1.234(4) . ? C1 C2 1.509(4) . ? C2 C3 1.404(4) . ? C2 C7 1.406(4) . ? C3 C4 1.391(5) . ? C3 C8 1.494(5) . ? C4 C5 1.383(6) . ? C4 H4 0.9500 . ? C5 C6 1.382(6) . ? C5 H5 0.9500 . ? C6 C7 1.385(5) . ? C6 H6 0.9500 . ? C7 C17 1.499(5) . ? C8 C13 1.401(5) . ? C8 C9 1.408(5) . ? C9 C10 1.395(5) . ? C9 C14 1.501(5) . ? C10 C11 1.389(6) . ? C10 H10 0.9500 . ? C11 C12 1.386(6) . ? C11 C15 1.514(5) . ? C12 C13 1.384(5) . ? C12 H12 0.9500 . ? C13 C16 1.514(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.395(5) . ? C17 C22 1.405(5) . ? C18 C19 1.394(5) . ? C18 C23 1.506(5) . ? C19 C20 1.392(5) . ? C19 H19 0.9500 . ? C20 C21 1.382(5) . ? C20 C24 1.507(5) . ? C21 C22 1.397(5) . ? C21 H21 0.9500 . ? C22 C25 1.512(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C41 C42 1.512(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 O43 1.451(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? O43 C44 1.457(9) . ? C44 C45 1.516(10) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C28 111.43(17) . . ? N1 Si1 C27 108.50(17) . . ? C28 Si1 C27 109.2(3) . . ? N1 Si1 C26 107.23(16) . . ? C28 Si1 C26 109.1(2) . . ? C27 Si1 C26 111.4(2) . . ? N1 Sn1 O1 93.17(8) . . ? N1 Sn1 N1 75.94(9) . 2_576 ? O1 Sn1 N1 81.77(8) . 2_576 ? Si1 N1 Sn1 127.00(12) . . ? Si1 N1 Sn1 123.05(12) . 2_576 ? Sn1 N1 Sn1 104.06(9) . 2_576 ? C1 O1 Sn1 100.39(19) . . ? O2 C1 O1 121.6(3) . . ? O2 C1 C2 121.3(3) . . ? O1 C1 C2 117.1(3) . . ? C3 C2 C7 121.2(3) . . ? C3 C2 C1 120.5(3) . . ? C7 C2 C1 118.2(3) . . ? C4 C3 C2 118.3(3) . . ? C4 C3 C8 122.5(3) . . ? C2 C3 C8 119.1(3) . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 120.8(3) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 118.4(3) . . ? C6 C7 C17 123.0(3) . . ? C2 C7 C17 118.5(3) . . ? C13 C8 C9 119.4(3) . . ? C13 C8 C3 119.5(3) . . ? C9 C8 C3 121.0(3) . . ? C10 C9 C8 118.8(3) . . ? C10 C9 C14 121.3(3) . . ? C8 C9 C14 119.9(3) . . ? C11 C10 C9 121.9(3) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C12 C11 C10 118.1(3) . . ? C12 C11 C15 120.6(4) . . ? C10 C11 C15 121.3(4) . . ? C13 C12 C11 121.8(4) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C8 119.7(3) . . ? C12 C13 C16 120.1(4) . . ? C8 C13 C16 120.1(3) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 120.1(3) . . ? C18 C17 C7 121.0(3) . . ? C22 C17 C7 118.7(3) . . ? C19 C18 C17 119.2(3) . . ? C19 C18 C23 120.0(3) . . ? C17 C18 C23 120.8(3) . . ? C20 C19 C18 121.8(4) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C21 C20 C19 118.0(3) . . ? C21 C20 C24 120.7(4) . . ? C19 C20 C24 121.2(4) . . ? C20 C21 C22 122.1(3) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C21 C22 C17 118.7(3) . . ? C21 C22 C25 120.1(3) . . ? C17 C22 C25 121.2(3) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O43 C42 C41 112.2(15) . . ? O43 C42 H42A 109.2 . . ? C41 C42 H42A 109.2 . . ? O43 C42 H42B 109.2 . . ? C41 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C42 O43 C44 113.9(13) . . ? O43 C44 C45 106.0(16) . . ? O43 C44 H44A 110.5 . . ? C45 C44 H44A 110.5 . . ? O43 C44 H44B 110.5 . . ? C45 C44 H44B 110.5 . . ? H44A C44 H44B 108.7 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C28 Si1 N1 Sn1 -69.7(2) . . . . ? C27 Si1 N1 Sn1 50.6(2) . . . . ? C26 Si1 N1 Sn1 170.98(18) . . . . ? C28 Si1 N1 Sn1 141.8(2) . . . 2_576 ? C27 Si1 N1 Sn1 -98.0(2) . . . 2_576 ? C26 Si1 N1 Sn1 22.4(2) . . . 2_576 ? O1 Sn1 N1 Si1 126.11(15) . . . . ? N1 Sn1 N1 Si1 -153.2(2) 2_576 . . . ? O1 Sn1 N1 Sn1 -80.69(10) . . . 2_576 ? N1 Sn1 N1 Sn1 0.0 2_576 . . 2_576 ? N1 Sn1 O1 C1 -84.81(18) . . . . ? N1 Sn1 O1 C1 -160.11(18) 2_576 . . . ? Sn1 O1 C1 O2 8.4(3) . . . . ? Sn1 O1 C1 C2 -169.2(2) . . . . ? O2 C1 C2 C3 97.9(4) . . . . ? O1 C1 C2 C3 -84.5(4) . . . . ? O2 C1 C2 C7 -83.6(4) . . . . ? O1 C1 C2 C7 94.0(4) . . . . ? C7 C2 C3 C4 1.7(5) . . . . ? C1 C2 C3 C4 -179.8(3) . . . . ? C7 C2 C3 C8 -175.9(3) . . . . ? C1 C2 C3 C8 2.6(5) . . . . ? C2 C3 C4 C5 -1.0(6) . . . . ? C8 C3 C4 C5 176.6(4) . . . . ? C3 C4 C5 C6 -0.2(7) . . . . ? C4 C5 C6 C7 0.7(8) . . . . ? C5 C6 C7 C2 0.0(7) . . . . ? C5 C6 C7 C17 -176.2(4) . . . . ? C3 C2 C7 C6 -1.2(6) . . . . ? C1 C2 C7 C6 -179.7(3) . . . . ? C3 C2 C7 C17 175.2(3) . . . . ? C1 C2 C7 C17 -3.3(5) . . . . ? C4 C3 C8 C13 -84.1(5) . . . . ? C2 C3 C8 C13 93.4(4) . . . . ? C4 C3 C8 C9 97.9(4) . . . . ? C2 C3 C8 C9 -84.6(4) . . . . ? C13 C8 C9 C10 -3.1(5) . . . . ? C3 C8 C9 C10 174.9(3) . . . . ? C13 C8 C9 C14 176.0(3) . . . . ? C3 C8 C9 C14 -6.0(5) . . . . ? C8 C9 C10 C11 -0.2(5) . . . . ? C14 C9 C10 C11 -179.3(3) . . . . ? C9 C10 C11 C12 2.5(5) . . . . ? C9 C10 C11 C15 -178.0(3) . . . . ? C10 C11 C12 C13 -1.6(5) . . . . ? C15 C11 C12 C13 179.0(3) . . . . ? C11 C12 C13 C8 -1.7(5) . . . . ? C11 C12 C13 C16 176.6(4) . . . . ? C9 C8 C13 C12 4.0(5) . . . . ? C3 C8 C13 C12 -174.0(3) . . . . ? C9 C8 C13 C16 -174.3(3) . . . . ? C3 C8 C13 C16 7.7(5) . . . . ? C6 C7 C17 C18 -94.4(5) . . . . ? C2 C7 C17 C18 89.3(4) . . . . ? C6 C7 C17 C22 90.4(5) . . . . ? C2 C7 C17 C22 -85.8(4) . . . . ? C22 C17 C18 C19 2.7(5) . . . . ? C7 C17 C18 C19 -172.4(3) . . . . ? C22 C17 C18 C23 -177.9(3) . . . . ? C7 C17 C18 C23 7.0(5) . . . . ? C17 C18 C19 C20 0.2(5) . . . . ? C23 C18 C19 C20 -179.2(3) . . . . ? C18 C19 C20 C21 -2.4(5) . . . . ? C18 C19 C20 C24 177.4(4) . . . . ? C19 C20 C21 C22 1.7(5) . . . . ? C24 C20 C21 C22 -178.1(3) . . . . ? C20 C21 C22 C17 1.1(5) . . . . ? C20 C21 C22 C25 -177.8(3) . . . . ? C18 C17 C22 C21 -3.3(5) . . . . ? C7 C17 C22 C21 171.9(3) . . . . ? C18 C17 C22 C25 175.6(3) . . . . ? C7 C17 C22 C25 -9.2(5) . . . . ? C41 C42 O43 C44 -179.5(14) . . . . ? C42 O43 C44 C45 -173(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.771 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.140 #===END