# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_shelxl1 _database_code_depnum_ccdc_archive 'CCDC 891289' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H40 Cl2 O2 Sn' _chemical_formula_sum 'C28 H40 Cl2 O2 Sn' _chemical_formula_weight 598.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn 0.0259 5.4591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8030(4) _cell_length_b 10.6301(4) _cell_length_c 20.1254(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.781(3) _cell_angle_gamma 90.00 _cell_volume 2879.78(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8654 _cell_measurement_theta_min 3.2761 _cell_measurement_theta_max 67.1383 _exptl_crystal_description squares _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 8.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78973 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4223 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18841 _diffrn_reflns_av_R_equivalents 0.1705 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 67.00 _reflns_number_total 5134 _reflns_number_gt 4325 _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^)+(0.0815P)^2^+12.1096P] 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 5134 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1530 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 C1 C 0.2167(5) 0.3738(5) 0.9761(3) 0.0194(13) Uani 1 1 d . . . C2 C 0.1445(4) 0.3468(5) 0.9181(3) 0.0183(12) Uani 1 1 d . . . H2 H 0.0779 0.3580 0.9188 0.022 Uiso 1 1 calc R . . C3 C 0.1697(4) 0.3034(5) 0.8592(3) 0.0184(12) Uani 1 1 d . . . C4 C 0.2714(4) 0.2900(5) 0.8609(3) 0.0173(12) Uani 1 1 d . . . C5 C 0.3463(4) 0.3098(5) 0.9198(3) 0.0175(12) Uani 1 1 d . . . C6 C 0.3157(4) 0.3552(5) 0.9767(3) 0.0181(12) Uani 1 1 d . . . H6 H 0.3632 0.3734 1.0161 0.022 Uiso 1 1 calc R . . C7 C 0.4565(4) 0.2849(6) 0.9210(3) 0.0189(12) Uani 1 1 d . . . C8 C 0.4718(5) 0.1493(6) 0.8982(4) 0.0275(14) Uani 1 1 d . . . H8A H 0.4478 0.0910 0.9273 0.041 Uiso 1 1 calc R . . H8B H 0.5412 0.1347 0.9011 0.041 Uiso 1 1 calc R . . H8C H 0.4359 0.1377 0.8520 0.041 Uiso 1 1 calc R . . C9 C 0.4941(5) 0.3801(6) 0.8749(3) 0.0263(14) Uani 1 1 d . . . H9A H 0.4845 0.4640 0.8899 0.039 Uiso 1 1 calc R . . H9B H 0.4578 0.3696 0.8288 0.039 Uiso 1 1 calc R . . H9C H 0.5636 0.3661 0.8774 0.039 Uiso 1 1 calc R . . C10 C 0.5222(5) 0.2979(7) 0.9931(3) 0.0282(14) Uani 1 1 d . . . H10A H 0.5001 0.2398 1.0231 0.042 Uiso 1 1 calc R . . H10B H 0.5175 0.3822 1.0093 0.042 Uiso 1 1 calc R . . H10C H 0.5899 0.2798 0.9920 0.042 Uiso 1 1 calc R . . C11 C 0.0884(5) 0.2718(6) 0.7952(3) 0.0222(13) Uani 1 1 d . . . C12 C -0.0157(5) 0.2896(7) 0.8087(3) 0.0305(16) Uani 1 1 d . . . H12A H -0.0646 0.2694 0.7682 0.046 Uiso 1 1 calc R . . H12B H -0.0239 0.3754 0.8212 0.046 Uiso 1 1 calc R . . H12C H -0.0239 0.2350 0.8450 0.046 Uiso 1 1 calc R . . C13 C 0.0947(5) 0.3614(6) 0.7363(3) 0.0253(14) Uani 1 1 d . . . H13A H 0.1589 0.3537 0.7256 0.038 Uiso 1 1 calc R . . H13B H 0.0851 0.4464 0.7496 0.038 Uiso 1 1 calc R . . H13C H 0.0442 0.3399 0.6970 0.038 Uiso 1 1 calc R . . C14 C 0.0959(5) 0.1333(6) 0.7738(3) 0.0275(14) Uani 1 1 d . . . H14A H 0.1604 0.1183 0.7648 0.041 Uiso 1 1 calc R . . H14B H 0.0458 0.1165 0.7334 0.041 Uiso 1 1 calc R . . H14C H 0.0862 0.0790 0.8099 0.041 Uiso 1 1 calc R . . C15 C 0.2149(4) 0.6226(5) 1.1044(3) 0.0183(12) Uani 1 1 d . . . C16 C 0.2004(4) 0.7229(6) 1.0596(3) 0.0221(13) Uani 1 1 d . . . H16 H 0.1729 0.7088 1.0137 0.027 Uiso 1 1 calc R . . C17 C 0.2267(5) 0.8463(5) 1.0823(3) 0.0169(12) Uani 1 1 d . . . C18 C 0.2696(5) 0.8619(5) 1.1513(3) 0.0204(13) Uani 1 1 d . . . C19 C 0.2856(4) 0.7603(6) 1.1984(3) 0.0192(12) Uani 1 1 d . . . C20 C 0.2566(4) 0.6426(5) 1.1733(3) 0.0168(12) Uani 1 1 d . . . H20 H 0.2650 0.5745 1.2030 0.020 Uiso 1 1 calc R . . C21 C 0.3370(5) 0.7785(6) 1.2744(3) 0.0232(13) Uani 1 1 d . . . C22 C 0.3422(6) 0.6548(7) 1.3139(3) 0.0365(18) Uani 1 1 d . . . H22A H 0.2762 0.6233 1.3110 0.055 Uiso 1 1 calc R . . H22B H 0.3738 0.6690 1.3608 0.055 Uiso 1 1 calc R . . H22C H 0.3798 0.5943 1.2946 0.055 Uiso 1 1 calc R . . C23 C 0.4445(5) 0.8226(7) 1.2797(3) 0.0295(15) Uani 1 1 d . . . H23A H 0.4443 0.9004 1.2554 0.044 Uiso 1 1 calc R . . H23B H 0.4800 0.7600 1.2602 0.044 Uiso 1 1 calc R . . H23C H 0.4763 0.8349 1.3267 0.044 Uiso 1 1 calc R . . C24 C 0.2809(5) 0.8736(7) 1.3100(3) 0.0272(14) Uani 1 1 d . . . H24A H 0.2764 0.9529 1.2867 0.041 Uiso 1 1 calc R . . H24B H 0.3160 0.8845 1.3564 0.041 Uiso 1 1 calc R . . H24C H 0.2153 0.8425 1.3090 0.041 Uiso 1 1 calc R . . C25 C 0.2035(5) 0.9570(6) 1.0311(3) 0.0209(13) Uani 1 1 d . . . C26 C 0.2994(5) 1.0281(6) 1.0253(4) 0.0280(15) Uani 1 1 d . . . H26A H 0.3327 1.0581 1.0694 0.042 Uiso 1 1 calc R . . H26B H 0.2824 1.0981 0.9948 0.042 Uiso 1 1 calc R . . H26C H 0.3426 0.9721 1.0080 0.042 Uiso 1 1 calc R . . C27 C 0.1282(5) 1.0459(6) 1.0527(3) 0.0237(13) Uani 1 1 d . . . H27A H 0.1549 1.0761 1.0980 0.036 Uiso 1 1 calc R . . H27B H 0.0675 1.0013 1.0518 0.036 Uiso 1 1 calc R . . H27C H 0.1153 1.1158 1.0218 0.036 Uiso 1 1 calc R . . C28 C 0.1558(6) 0.9117(6) 0.9588(3) 0.0275(14) Uani 1 1 d . . . H28A H 0.2003 0.8551 0.9433 0.041 Uiso 1 1 calc R . . H28B H 0.1426 0.9828 0.9287 0.041 Uiso 1 1 calc R . . H28C H 0.0947 0.8690 0.9593 0.041 Uiso 1 1 calc R . . O1 O 0.3043(3) 0.2557(4) 0.8039(2) 0.0237(9) Uani 1 1 d . . . O2 O 0.3000(3) 0.9785(4) 1.1780(2) 0.0237(9) Uani 1 1 d . . . Cl1 Cl 0.28295(11) 0.31272(13) 1.15147(7) 0.0218(3) Uani 1 1 d . . . Cl2 Cl 0.02055(11) 0.37913(14) 1.07112(8) 0.0227(3) Uani 1 1 d . . . Sn Sn 0.18304(3) 0.43956(3) 1.066929(18) 0.01556(16) 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 C1 0.025(3) 0.015(3) 0.021(3) -0.001(2) 0.010(3) -0.001(2) C2 0.011(3) 0.020(3) 0.025(3) -0.001(2) 0.008(2) -0.001(2) C3 0.015(3) 0.021(3) 0.018(3) 0.000(2) 0.002(2) -0.003(2) C4 0.017(3) 0.016(3) 0.019(3) 0.001(2) 0.003(2) 0.001(2) C5 0.010(3) 0.021(3) 0.021(3) 0.002(2) 0.003(2) 0.001(2) C6 0.011(3) 0.020(3) 0.020(3) 0.000(2) -0.002(2) -0.002(2) C7 0.010(3) 0.026(3) 0.021(3) -0.003(2) 0.004(2) 0.001(2) C8 0.023(4) 0.030(3) 0.030(3) -0.002(3) 0.006(3) 0.006(3) C9 0.016(3) 0.035(3) 0.031(4) 0.001(3) 0.011(3) 0.000(3) C10 0.018(3) 0.042(4) 0.023(3) -0.002(3) 0.001(3) 0.001(3) C11 0.017(3) 0.033(3) 0.015(3) -0.002(3) 0.000(2) -0.001(3) C12 0.016(3) 0.052(4) 0.020(3) -0.008(3) -0.002(3) -0.009(3) C13 0.023(3) 0.032(3) 0.020(3) 0.000(3) 0.004(3) 0.003(3) C14 0.031(4) 0.031(3) 0.019(3) -0.004(3) 0.003(3) -0.007(3) C15 0.010(3) 0.021(3) 0.022(3) 0.004(2) 0.002(2) 0.001(2) C16 0.015(3) 0.032(3) 0.019(3) -0.005(3) 0.002(2) 0.000(3) C17 0.016(3) 0.018(3) 0.017(3) -0.002(2) 0.005(2) -0.003(2) C18 0.015(3) 0.017(3) 0.029(3) -0.007(2) 0.006(3) -0.001(2) C19 0.015(3) 0.020(3) 0.022(3) -0.001(2) 0.003(2) 0.003(2) C20 0.015(3) 0.021(3) 0.015(3) 0.003(2) 0.003(2) 0.000(2) C21 0.023(3) 0.027(3) 0.018(3) -0.002(2) 0.002(3) 0.001(3) C22 0.055(5) 0.031(4) 0.017(3) -0.001(3) -0.007(3) -0.003(3) C23 0.015(3) 0.043(4) 0.027(3) -0.008(3) -0.002(3) 0.006(3) C24 0.024(4) 0.036(3) 0.021(3) -0.008(3) 0.003(3) 0.001(3) C25 0.017(3) 0.024(3) 0.021(3) 0.000(2) 0.003(2) 0.000(3) C26 0.029(4) 0.024(3) 0.033(4) 0.005(3) 0.012(3) 0.001(3) C27 0.014(3) 0.028(3) 0.026(3) -0.003(3) -0.001(3) 0.004(3) C28 0.034(4) 0.026(3) 0.020(3) 0.003(3) 0.002(3) 0.004(3) O1 0.017(2) 0.036(2) 0.019(2) -0.0061(19) 0.0065(17) 0.003(2) O2 0.024(2) 0.021(2) 0.023(2) -0.0051(18) 0.0002(18) -0.0035(19) Cl1 0.0215(8) 0.0240(7) 0.0193(7) 0.0030(6) 0.0031(5) 0.0029(6) Cl2 0.0132(7) 0.0274(7) 0.0278(7) -0.0009(6) 0.0052(6) -0.0039(6) Sn 0.0138(2) 0.0184(2) 0.0149(2) -0.00137(14) 0.00400(16) -0.00077(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.379(8) . ? C1 C2 1.387(9) . ? C1 Sn 2.102(6) . ? C2 C3 1.387(8) . ? C2 H2 0.9300 . ? C3 C4 1.404(8) . ? C3 C11 1.546(8) . ? C4 O1 1.372(7) . ? C4 C5 1.406(8) . ? C5 C6 1.391(8) . ? C5 C7 1.539(8) . ? C6 H6 0.9300 . ? C7 C10 1.538(8) . ? C7 C9 1.538(8) . ? C7 C8 1.542(8) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.532(8) . ? C11 C13 1.538(9) . ? C11 C14 1.544(9) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.382(9) . ? C15 C20 1.395(8) . ? C15 Sn 2.097(6) . ? C16 C17 1.410(8) . ? C16 H16 0.9300 . ? C17 C18 1.393(9) . ? C17 C25 1.550(8) . ? C18 O2 1.378(7) . ? C18 C19 1.421(9) . ? C19 C20 1.376(8) . ? C19 C21 1.550(8) . ? C20 H20 0.9300 . ? C21 C22 1.530(9) . ? C21 C23 1.538(9) . ? C21 C24 1.542(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C28 1.535(9) . ? C25 C27 1.537(8) . ? C25 C26 1.551(9) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? Cl1 Sn 2.3615(14) . ? Cl2 Sn 2.3524(14) . ? 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 C6 C1 C2 120.3(5) . . ? C6 C1 Sn 116.7(4) . . ? C2 C1 Sn 123.0(4) . . ? C1 C2 C3 121.3(5) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C2 C3 C4 116.8(5) . . ? C2 C3 C11 120.7(5) . . ? C4 C3 C11 122.4(5) . . ? O1 C4 C3 121.3(5) . . ? O1 C4 C5 115.3(5) . . ? C3 C4 C5 123.4(5) . . ? C6 C5 C4 116.5(5) . . ? C6 C5 C7 121.7(5) . . ? C4 C5 C7 121.8(5) . . ? C1 C6 C5 121.5(5) . . ? C1 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C10 C7 C9 107.6(5) . . ? C10 C7 C5 111.9(5) . . ? C9 C7 C5 110.0(5) . . ? C10 C7 C8 105.9(5) . . ? C9 C7 C8 110.4(5) . . ? C5 C7 C8 110.8(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 106.0(5) . . ? C12 C11 C14 106.9(5) . . ? C13 C11 C14 110.9(5) . . ? C12 C11 C3 111.3(5) . . ? C13 C11 C3 110.6(5) . . ? C14 C11 C3 111.0(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 119.9(6) . . ? C16 C15 Sn 119.6(4) . . ? C20 C15 Sn 120.4(4) . . ? C15 C16 C17 121.1(6) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 117.1(5) . . ? C18 C17 C25 123.5(5) . . ? C16 C17 C25 119.3(5) . . ? O2 C18 C17 121.4(5) . . ? O2 C18 C19 115.7(5) . . ? C17 C18 C19 122.9(5) . . ? C20 C19 C18 117.2(5) . . ? C20 C19 C21 120.6(5) . . ? C18 C19 C21 122.2(5) . . ? C19 C20 C15 121.7(5) . . ? C19 C20 H20 119.1 . . ? C15 C20 H20 119.1 . . ? C22 C21 C23 107.0(6) . . ? C22 C21 C24 107.0(5) . . ? C23 C21 C24 110.2(5) . . ? C22 C21 C19 111.3(5) . . ? C23 C21 C19 109.3(5) . . ? C24 C21 C19 111.9(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C27 106.6(5) . . ? C28 C25 C17 112.0(5) . . ? C27 C25 C17 109.3(5) . . ? C28 C25 C26 106.0(5) . . ? C27 C25 C26 111.3(5) . . ? C17 C25 C26 111.5(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C15 Sn C1 123.5(2) . . ? C15 Sn Cl2 111.47(16) . . ? C1 Sn Cl2 109.64(18) . . ? C15 Sn Cl1 103.19(17) . . ? C1 Sn Cl1 103.33(17) . . ? Cl2 Sn Cl1 103.16(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.868 _refine_diff_density_min -1.439 _refine_diff_density_rms 0.153 data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 891290' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 N4 O2 S2 Sn' _chemical_formula_sum 'C36 H48 N4 O2 S2 Sn' _chemical_formula_weight 751.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn 0.0259 5.4591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.2953(4) _cell_length_b 24.9586(8) _cell_length_c 30.4963(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7075.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 6727 _cell_measurement_theta_min 3.5388 _cell_measurement_theta_max 67.1121 _exptl_crystal_description rectangle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 7.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.52633 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4223 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12737 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 66.99 _reflns_number_total 6043 _reflns_number_gt 5750 _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^)+(0.0996P)^2^+12.1372P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.025(7) _refine_ls_number_reflns 6043 _refine_ls_number_parameters 413 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.1365 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _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 C1 C -0.3027(6) 1.3011(2) 0.21136(17) 0.0160(11) Uani 1 1 d . . . C2 C -0.5313(6) 1.2864(3) 0.1893(2) 0.0268(14) Uani 1 1 d . . . H2 H -0.6215 1.2988 0.1809 0.032 Uiso 1 1 calc R . . C3 C -0.5087(8) 1.2317(3) 0.19099(19) 0.0326(16) Uani 1 1 d . . . H3 H -0.5805 1.2075 0.1835 0.039 Uiso 1 1 calc R . . C4 C -0.3726(8) 1.2147(3) 0.2045(2) 0.0254(13) Uani 1 1 d . . . H4 H -0.3535 1.1782 0.2059 0.030 Uiso 1 1 calc R . . C5 C 0.6109(6) 1.1073(3) 0.05050(19) 0.0182(12) Uani 1 1 d . . . C6 C 0.8401(6) 1.1364(2) 0.06070(19) 0.0206(12) Uani 1 1 d . . . H6 H 0.9387 1.1328 0.0564 0.025 Uiso 1 1 calc R . . C7 C 0.7910(7) 1.1793(3) 0.0846(2) 0.0247(14) Uani 1 1 d . . . H7 H 0.8539 1.2037 0.0973 0.030 Uiso 1 1 calc R . . C8 C 0.6428(7) 1.1845(2) 0.08870(19) 0.0204(13) Uani 1 1 d . . . H8 H 0.6063 1.2137 0.1040 0.024 Uiso 1 1 calc R . . C9 C 0.0811(6) 1.2387(2) 0.19293(17) 0.0120(10) Uani 1 1 d U . . C10 C 0.1165(6) 1.1840(2) 0.19365(18) 0.0141(11) Uani 1 1 d . . . H10 H 0.1058 1.1651 0.2197 0.017 Uiso 1 1 calc R . . C11 C 0.1672(5) 1.1568(2) 0.15653(18) 0.0148(11) Uani 1 1 d . . . C12 C 0.1906(6) 1.1881(2) 0.11802(18) 0.0151(11) Uani 1 1 d U . . C13 C 0.0993(5) 1.2671(2) 0.15405(17) 0.0133(11) Uani 1 1 d . . . H13 H 0.0728 1.3030 0.1533 0.016 Uiso 1 1 calc R . . C14 C 0.1552(6) 1.2439(2) 0.11646(19) 0.0142(11) Uani 1 1 d . . . C15 C 0.1782(6) 1.2767(2) 0.07389(17) 0.0150(10) Uani 1 1 d . . . C16 C 0.0832(7) 1.2563(2) 0.0368(2) 0.0218(13) Uani 1 1 d . . . H16A H 0.1042 1.2192 0.0313 0.033 Uiso 1 1 calc R . . H16B H 0.1015 1.2767 0.0107 0.033 Uiso 1 1 calc R . . H16C H -0.0161 1.2600 0.0449 0.033 Uiso 1 1 calc R . . C17 C 0.1422(7) 1.3360(2) 0.08190(19) 0.0187(12) Uani 1 1 d . . . H17A H 0.0436 1.3392 0.0909 0.028 Uiso 1 1 calc R . . H17B H 0.1568 1.3559 0.0553 0.028 Uiso 1 1 calc R . . H17C H 0.2036 1.3500 0.1045 0.028 Uiso 1 1 calc R . . C18 C 0.3366(6) 1.2752(3) 0.0597(2) 0.0251(13) Uani 1 1 d . . . H18A H 0.3649 1.2388 0.0543 0.038 Uiso 1 1 calc R . . H18B H 0.3954 1.2901 0.0826 0.038 Uiso 1 1 calc R . . H18C H 0.3485 1.2959 0.0334 0.038 Uiso 1 1 calc R . . C19 C 0.1958(6) 1.0957(2) 0.15813(18) 0.0165(11) Uani 1 1 d . . . C20 C 0.1484(6) 1.0722(2) 0.20219(19) 0.0190(12) Uani 1 1 d . . . H20A H 0.2000 1.0895 0.2255 0.028 Uiso 1 1 calc R . . H20B H 0.1686 1.0344 0.2027 0.028 Uiso 1 1 calc R . . H20C H 0.0470 1.0778 0.2060 0.028 Uiso 1 1 calc R . . C21 C 0.1123(6) 1.0677(2) 0.12187(19) 0.0210(12) Uani 1 1 d . . . H21A H 0.1406 1.0821 0.0940 0.031 Uiso 1 1 calc R . . H21B H 0.0111 1.0734 0.1261 0.031 Uiso 1 1 calc R . . H21C H 0.1324 1.0300 0.1226 0.031 Uiso 1 1 calc R . . C22 C 0.3564(6) 1.0837(2) 0.1530(2) 0.0196(12) Uani 1 1 d . . . H22A H 0.4090 1.1014 0.1759 0.029 Uiso 1 1 calc R . . H22B H 0.3890 1.0964 0.1250 0.029 Uiso 1 1 calc R . . H22C H 0.3718 1.0457 0.1550 0.029 Uiso 1 1 calc R . . C23 C 0.8003(6) 0.9658(2) 0.05306(18) 0.0139(11) Uani 1 1 d U . . C24 C 0.7514(6) 0.9728(2) 0.09506(19) 0.0148(11) Uani 1 1 d . . . H24 H 0.6614 0.9882 0.0994 0.018 Uiso 1 1 calc R . . C25 C 0.8325(6) 0.9576(2) 0.13137(17) 0.0134(10) Uani 1 1 d . . . C26 C 0.9684(6) 0.9356(2) 0.12426(18) 0.0141(11) Uani 1 1 d . . . C27 C 1.0199(6) 0.9255(2) 0.08081(18) 0.0138(11) Uani 1 1 d . . . C28 C 0.9330(6) 0.9425(2) 0.04593(18) 0.0134(11) Uani 1 1 d . . . H28 H 0.9655 0.9380 0.0173 0.016 Uiso 1 1 calc R . . C29 C 1.1684(6) 0.9007(2) 0.07126(17) 0.0140(11) Uani 1 1 d . . . C30 C 1.2880(6) 0.9410(3) 0.0822(2) 0.0225(13) Uani 1 1 d . . . H30A H 1.3800 0.9251 0.0760 0.034 Uiso 1 1 calc R . . H30B H 1.2829 0.9503 0.1127 0.034 Uiso 1 1 calc R . . H30C H 1.2760 0.9726 0.0646 0.034 Uiso 1 1 calc R . . C31 C 1.1823(7) 0.8845(3) 0.0222(2) 0.0256(13) Uani 1 1 d . . . H31A H 1.2755 0.8691 0.0171 0.038 Uiso 1 1 calc R . . H31B H 1.1704 0.9156 0.0041 0.038 Uiso 1 1 calc R . . H31C H 1.1094 0.8586 0.0151 0.038 Uiso 1 1 calc R . . C32 C 1.1945(6) 0.8487(3) 0.0977(2) 0.0234(13) Uani 1 1 d . . . H32A H 1.2878 0.8346 0.0907 0.035 Uiso 1 1 calc R . . H32B H 1.1222 0.8227 0.0902 0.035 Uiso 1 1 calc R . . H32C H 1.1895 0.8564 0.1285 0.035 Uiso 1 1 calc R . . C33 C 0.7608(6) 0.9683(2) 0.1766(2) 0.0182(12) Uani 1 1 d . . . C34 C 0.8489(6) 0.9542(3) 0.21686(18) 0.0210(12) Uani 1 1 d . . . H34A H 0.9377 0.9739 0.2163 0.031 Uiso 1 1 calc R . . H34B H 0.8690 0.9165 0.2169 0.031 Uiso 1 1 calc R . . H34C H 0.7958 0.9634 0.2428 0.031 Uiso 1 1 calc R . . C35 C 0.6183(6) 0.9378(3) 0.17872(18) 0.0185(12) Uani 1 1 d . . . H35A H 0.5609 0.9466 0.1536 0.028 Uiso 1 1 calc R . . H35B H 0.5675 0.9476 0.2049 0.028 Uiso 1 1 calc R . . H35C H 0.6370 0.8999 0.1790 0.028 Uiso 1 1 calc R . . C36 C 0.7250(6) 1.0297(3) 0.1805(2) 0.0223(13) Uani 1 1 d . . . H36A H 0.6684 1.0406 0.1557 0.033 Uiso 1 1 calc R . . H36B H 0.8129 1.0499 0.1811 0.033 Uiso 1 1 calc R . . H36C H 0.6720 1.0361 0.2070 0.033 Uiso 1 1 calc R . . N1 N -0.2705(5) 1.2489(2) 0.21518(16) 0.0193(10) Uani 1 1 d . . . N2 N -0.4289(5) 1.3225(2) 0.19926(17) 0.0236(12) Uani 1 1 d . . . N3 N 0.7516(5) 1.0992(2) 0.04319(16) 0.0182(10) Uani 1 1 d . . . N4 N 0.5505(5) 1.1491(2) 0.07148(16) 0.0169(10) Uani 1 1 d . . . O1 O 0.2391(4) 1.16415(17) 0.08039(13) 0.0159(8) Uani 1 1 d D . . O2 O 1.0659(4) 0.92667(18) 0.15725(13) 0.0180(8) Uani 1 1 d D . . S2 S -0.16573(14) 1.34691(6) 0.22474(4) 0.0171(3) Uani 1 1 d . . . S3 S 0.49395(15) 1.05728(5) 0.03089(4) 0.0172(3) Uani 1 1 d . . . Sn1 Sn 0.0000 1.276446(18) 0.2500 0.01102(14) Uani 1 2 d S . . Sn2 Sn 0.68445(5) 1.0000 0.0000 0.01169(14) Uani 1 2 d S . . H1 H 0.328(5) 1.152(3) 0.085(2) 0.014 Uiso 1 1 d D . . H20 H 1.051(7) 0.901(2) 0.1775(19) 0.014 Uiso 1 1 d 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 C1 0.011(2) 0.026(3) 0.011(3) 0.006(2) -0.003(2) 0.001(2) C2 0.013(3) 0.046(4) 0.021(3) 0.001(3) -0.005(2) -0.009(3) C3 0.025(3) 0.063(5) 0.009(3) -0.003(3) 0.002(2) -0.019(4) C4 0.038(3) 0.023(3) 0.015(3) 0.000(2) 0.007(3) -0.007(3) C5 0.012(3) 0.031(3) 0.012(3) 0.008(2) 0.005(2) 0.001(2) C6 0.014(3) 0.024(3) 0.024(3) 0.007(2) 0.004(2) -0.002(2) C7 0.023(3) 0.024(3) 0.027(3) -0.002(3) -0.002(3) -0.005(2) C8 0.030(3) 0.017(3) 0.014(3) -0.003(2) 0.005(3) -0.005(2) C9 0.013(2) 0.014(2) 0.009(2) -0.0095(19) -0.0019(18) -0.0007(18) C10 0.011(2) 0.022(3) 0.009(3) 0.004(2) 0.001(2) 0.000(2) C11 0.010(2) 0.019(3) 0.015(3) 0.006(2) -0.003(2) -0.002(2) C12 0.005(2) 0.025(3) 0.016(2) 0.002(2) -0.0028(19) -0.002(2) C13 0.012(2) 0.016(3) 0.013(2) -0.004(2) 0.0039(19) -0.002(2) C14 0.011(3) 0.011(3) 0.021(3) 0.000(2) -0.005(2) -0.0076(19) C15 0.013(2) 0.018(3) 0.013(2) 0.001(2) 0.000(2) -0.002(2) C16 0.030(3) 0.013(3) 0.022(3) 0.009(2) -0.004(2) -0.004(2) C17 0.033(3) 0.007(3) 0.016(3) 0.001(2) -0.003(2) -0.003(2) C18 0.019(3) 0.036(4) 0.021(3) 0.009(3) 0.010(2) 0.000(3) C19 0.016(3) 0.017(3) 0.016(3) 0.002(2) 0.005(2) 0.001(2) C20 0.028(3) 0.011(2) 0.018(3) 0.004(2) 0.004(2) 0.003(2) C21 0.022(3) 0.020(3) 0.021(3) -0.005(2) -0.001(2) -0.003(2) C22 0.020(3) 0.015(3) 0.024(3) 0.005(2) 0.005(2) 0.005(2) C23 0.018(2) 0.008(2) 0.015(2) 0.0080(19) -0.002(2) -0.0016(19) C24 0.010(2) 0.020(3) 0.015(3) -0.001(2) 0.0004(19) -0.004(2) C25 0.015(3) 0.010(2) 0.014(3) 0.001(2) 0.000(2) -0.0023(19) C26 0.016(3) 0.012(3) 0.015(3) 0.004(2) -0.004(2) -0.0026(20) C27 0.013(3) 0.013(2) 0.015(3) -0.004(2) 0.000(2) -0.008(2) C28 0.012(2) 0.017(3) 0.011(2) 0.000(2) 0.001(2) -0.004(2) C29 0.016(3) 0.012(3) 0.015(3) 0.005(2) 0.002(2) 0.001(2) C30 0.010(3) 0.034(3) 0.023(3) -0.005(3) 0.000(2) -0.001(2) C31 0.017(3) 0.035(4) 0.025(3) -0.008(3) 0.000(3) 0.005(3) C32 0.012(3) 0.029(3) 0.029(3) 0.004(3) 0.001(2) 0.004(2) C33 0.016(3) 0.023(3) 0.015(3) -0.003(2) 0.005(2) -0.003(2) C34 0.020(3) 0.031(3) 0.011(3) 0.002(2) 0.002(2) 0.003(2) C35 0.016(3) 0.030(3) 0.009(3) -0.001(2) -0.001(2) -0.007(2) C36 0.020(3) 0.027(3) 0.020(3) -0.004(2) 0.001(2) 0.003(2) N1 0.015(2) 0.025(3) 0.018(2) 0.001(2) 0.0006(19) -0.0097(19) N2 0.014(2) 0.041(3) 0.016(3) -0.001(2) 0.002(2) 0.003(2) N3 0.015(2) 0.022(3) 0.018(2) 0.004(2) 0.0013(19) 0.0035(19) N4 0.020(2) 0.018(2) 0.013(2) -0.0002(19) -0.0004(19) 0.0021(19) O1 0.0153(19) 0.018(2) 0.014(2) -0.0026(16) 0.0033(15) 0.0025(16) O2 0.0161(18) 0.025(2) 0.0127(19) 0.0001(16) -0.0050(16) 0.0026(17) S2 0.0120(6) 0.0189(6) 0.0205(7) 0.0004(5) -0.0037(5) 0.0005(5) S3 0.0126(6) 0.0203(6) 0.0188(6) -0.0035(5) 0.0010(5) 0.0006(6) Sn1 0.0103(2) 0.0126(2) 0.0102(2) 0.000 0.00143(18) 0.000 Sn2 0.0101(2) 0.0146(2) 0.0103(2) 0.00149(19) 0.000 0.000 _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 C1 N2 1.340(8) . ? C1 N1 1.342(8) . ? C1 S2 1.758(6) . ? C2 N2 1.345(8) . ? C2 C3 1.381(11) . ? C2 H2 0.9300 . ? C3 C4 1.396(10) . ? C3 H3 0.9300 . ? C4 N1 1.319(8) . ? C4 H4 0.9300 . ? C5 N3 1.342(8) . ? C5 N4 1.347(8) . ? C5 S3 1.760(6) . ? C6 N3 1.351(8) . ? C6 C7 1.372(9) . ? C6 H6 0.9300 . ? C7 C8 1.390(10) . ? C7 H7 0.9300 . ? C8 N4 1.338(8) . ? C8 H8 0.9300 . ? C9 C13 1.391(8) . ? C9 C10 1.405(8) . ? C9 Sn1 2.117(5) . ? C10 C11 1.402(8) . ? C10 H10 0.9300 . ? C11 C12 1.426(8) . ? C11 C19 1.548(8) . ? C12 O1 1.370(7) . ? C12 C14 1.434(8) . ? C13 C14 1.385(8) . ? C13 H13 0.9300 . ? C14 C15 1.549(7) . ? C15 C16 1.524(8) . ? C15 C18 1.534(7) . ? C15 C17 1.538(8) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C21 1.521(8) . ? C19 C22 1.530(8) . ? C19 C20 1.531(7) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.371(8) . ? C23 C28 1.381(8) . ? C23 Sn2 2.123(5) . ? C24 C25 1.392(8) . ? C24 H24 0.9300 . ? C25 C26 1.395(8) . ? C25 C33 1.556(8) . ? C26 O2 1.372(7) . ? C26 C27 1.431(8) . ? C27 C28 1.402(8) . ? C27 C29 1.541(8) . ? C28 H28 0.9300 . ? C29 C30 1.536(8) . ? C29 C32 1.546(8) . ? C29 C31 1.556(8) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.517(8) . ? C33 C35 1.529(8) . ? C33 C36 1.573(8) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? O1 H1 0.89(4) . ? O2 H20 0.90(4) . ? S2 Sn1 2.4616(13) . ? S3 Sn2 2.4630(14) . ? Sn1 C9 2.117(5) 3 ? Sn1 S2 2.4615(14) 3 ? Sn2 C23 2.123(5) 4_575 ? Sn2 S3 2.4629(14) 4_575 ? 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 C1 N1 127.2(5) . . ? N2 C1 S2 116.1(5) . . ? N1 C1 S2 116.7(4) . . ? N2 C2 C3 123.1(6) . . ? N2 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? C2 C3 C4 116.7(6) . . ? C2 C3 H3 121.7 . . ? C4 C3 H3 121.7 . . ? N1 C4 C3 121.9(6) . . ? N1 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? N3 C5 N4 127.0(6) . . ? N3 C5 S3 116.1(5) . . ? N4 C5 S3 117.0(4) . . ? N3 C6 C7 122.9(5) . . ? N3 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C6 C7 C8 116.8(6) . . ? C6 C7 H7 121.6 . . ? C8 C7 H7 121.6 . . ? N4 C8 C7 122.6(6) . . ? N4 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C13 C9 C10 118.7(5) . . ? C13 C9 Sn1 121.1(4) . . ? C10 C9 Sn1 120.2(4) . . ? C11 C10 C9 122.5(5) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 C12 116.8(5) . . ? C10 C11 C19 120.6(5) . . ? C12 C11 C19 122.6(5) . . ? O1 C12 C11 120.1(5) . . ? O1 C12 C14 118.1(5) . . ? C11 C12 C14 121.7(5) . . ? C14 C13 C9 122.6(5) . . ? C14 C13 H13 118.7 . . ? C9 C13 H13 118.7 . . ? C13 C14 C12 117.7(5) . . ? C13 C14 C15 121.7(5) . . ? C12 C14 C15 120.6(5) . . ? C16 C15 C18 109.8(5) . . ? C16 C15 C17 108.3(5) . . ? C18 C15 C17 106.1(5) . . ? C16 C15 C14 111.5(4) . . ? C18 C15 C14 110.8(5) . . ? C17 C15 C14 110.2(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C22 109.5(5) . . ? C21 C19 C20 108.4(5) . . ? C22 C19 C20 107.1(5) . . ? C21 C19 C11 110.0(5) . . ? C22 C19 C11 110.9(5) . . ? C20 C19 C11 110.9(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 119.8(5) . . ? C24 C23 Sn2 119.5(4) . . ? C28 C23 Sn2 120.2(4) . . ? C23 C24 C25 121.9(5) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C24 C25 C26 118.3(5) . . ? C24 C25 C33 115.3(5) . . ? C26 C25 C33 126.4(5) . . ? O2 C26 C25 123.2(5) . . ? O2 C26 C27 115.4(5) . . ? C25 C26 C27 121.1(5) . . ? C28 C27 C26 117.2(5) . . ? C28 C27 C29 119.6(5) . . ? C26 C27 C29 123.1(5) . . ? C23 C28 C27 121.5(5) . . ? C23 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C30 C29 C27 110.2(4) . . ? C30 C29 C32 108.9(5) . . ? C27 C29 C32 112.3(4) . . ? C30 C29 C31 108.6(5) . . ? C27 C29 C31 111.1(4) . . ? C32 C29 C31 105.6(5) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C35 108.6(5) . . ? C34 C33 C25 116.5(5) . . ? C35 C33 C25 108.9(5) . . ? C34 C33 C36 106.2(5) . . ? C35 C33 C36 107.4(5) . . ? C25 C33 C36 108.9(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C4 N1 C1 116.5(5) . . ? C1 N2 C2 114.5(6) . . ? C5 N3 C6 115.2(5) . . ? C8 N4 C5 115.5(5) . . ? C12 O1 H1 109(4) . . ? C26 O2 H20 121(4) . . ? C1 S2 Sn1 93.53(19) . . ? C5 S3 Sn2 95.6(2) . . ? C9 Sn1 C9 127.2(3) 3 . ? C9 Sn1 S2 106.45(16) 3 3 ? C9 Sn1 S2 110.61(15) . 3 ? C9 Sn1 S2 110.61(14) 3 . ? C9 Sn1 S2 106.45(16) . . ? S2 Sn1 S2 88.81(6) 3 . ? C23 Sn2 C23 119.0(3) 4_575 . ? C23 Sn2 S3 107.87(16) 4_575 4_575 ? C23 Sn2 S3 114.99(14) . 4_575 ? C23 Sn2 S3 114.99(14) 4_575 . ? C23 Sn2 S3 107.87(16) . . ? S3 Sn2 S3 88.07(7) 4_575 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.028 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.157 data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 891291' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H52 N4 O2 S2 Sn' _chemical_formula_sum 'C38 H52 N4 O2 S2 Sn' _chemical_formula_weight 779.69 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8406(2) _cell_length_b 19.1873(4) _cell_length_c 18.7686(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.944(2) _cell_angle_gamma 90.00 _cell_volume 3882.92(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12499 _cell_measurement_theta_min 2.9276 _cell_measurement_theta_max 28.5473 _exptl_crystal_description polyhedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80860 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4223 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29129 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6787 _reflns_number_gt 5589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis RED' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND (Brandenburg, 2006) MERCURY (Bruno et al. 2002) ; _computing_publication_material 'WINGX (Farrugia, 1999)' _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^)+(0.0414P)^2^+2.0042P] 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 6787 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 C1 C 0.4789(3) 0.12389(15) 0.31633(17) 0.0173(7) Uani 1 1 d . . . C2 C 0.5737(3) 0.11092(15) 0.37002(16) 0.0187(7) Uani 1 1 d . . . H2 H 0.6512 0.0988 0.3568 0.022 Uiso 1 1 calc R . . C3 C 0.5589(3) 0.11515(15) 0.44284(16) 0.0164(7) Uani 1 1 d . . . C4 C 0.4402(3) 0.13466(15) 0.46016(16) 0.0171(7) Uani 1 1 d . . . C5 C 0.3399(3) 0.14809(16) 0.40797(16) 0.0182(7) Uani 1 1 d . . . C6 C 0.3628(3) 0.14129(16) 0.33627(17) 0.0208(7) Uani 1 1 d . . . H6 H 0.2979 0.1487 0.3006 0.025 Uiso 1 1 calc R . . C7 C 0.2116(3) 0.17163(17) 0.42761(17) 0.0225(7) Uani 1 1 d . . . C8 C 0.1558(3) 0.11933(19) 0.47746(19) 0.0309(9) Uani 1 1 d . . . H8A H 0.0763 0.1359 0.4884 0.046 Uiso 1 1 calc R . . H8B H 0.2101 0.1146 0.5209 0.046 Uiso 1 1 calc R . . H8C H 0.1461 0.0749 0.4541 0.046 Uiso 1 1 calc R . . C9 C 0.2254(3) 0.24356(18) 0.46308(19) 0.0325(9) Uani 1 1 d . . . H9A H 0.1462 0.2589 0.4757 0.049 Uiso 1 1 calc R . . H9B H 0.2558 0.2762 0.4303 0.049 Uiso 1 1 calc R . . H9C H 0.2829 0.2406 0.5055 0.049 Uiso 1 1 calc R . . C10 C 0.1180(3) 0.1788(2) 0.36097(18) 0.0322(9) Uani 1 1 d . . . H10A H 0.0394 0.1935 0.3750 0.048 Uiso 1 1 calc R . . H10B H 0.1086 0.1347 0.3369 0.048 Uiso 1 1 calc R . . H10C H 0.1474 0.2128 0.3292 0.048 Uiso 1 1 calc R . . C11 C 0.6684(3) 0.10073(17) 0.49947(16) 0.0197(7) Uani 1 1 d . . . C12 C 0.7036(3) 0.16786(17) 0.54156(17) 0.0259(8) Uani 1 1 d . . . H12A H 0.6332 0.1844 0.5637 0.039 Uiso 1 1 calc R . . H12B H 0.7289 0.2028 0.5094 0.039 Uiso 1 1 calc R . . H12C H 0.7707 0.1583 0.5778 0.039 Uiso 1 1 calc R . . C13 C 0.6391(3) 0.04058(16) 0.54959(17) 0.0218(7) Uani 1 1 d . . . H13A H 0.5664 0.0519 0.5724 0.033 Uiso 1 1 calc R . . H13B H 0.7080 0.0338 0.5854 0.033 Uiso 1 1 calc R . . H13C H 0.6245 -0.0014 0.5222 0.033 Uiso 1 1 calc R . . C14 C 0.7853(3) 0.07740(18) 0.46607(18) 0.0247(8) Uani 1 1 d . . . H14A H 0.8511 0.0689 0.5034 0.037 Uiso 1 1 calc R . . H14B H 0.8100 0.1133 0.4349 0.037 Uiso 1 1 calc R . . H14C H 0.7678 0.0354 0.4391 0.037 Uiso 1 1 calc R . . C15 C 0.6990(3) 0.08665(16) 0.19813(16) 0.0176(7) Uani 1 1 d . . . C16 C 0.7820(3) 0.12346(16) 0.16053(16) 0.0188(7) Uani 1 1 d . . . H16 H 0.7561 0.1648 0.1378 0.023 Uiso 1 1 calc R . . C17 C 0.9027(3) 0.10027(16) 0.15590(16) 0.0184(7) Uani 1 1 d . . . C18 C 0.9395(3) 0.03861(16) 0.19274(16) 0.0191(7) Uani 1 1 d . . . C19 C 0.8577(3) -0.00071(16) 0.23045(16) 0.0188(7) Uani 1 1 d . . . C20 C 0.7383(3) 0.02513(16) 0.23211(15) 0.0182(7) Uani 1 1 d . . . H20 H 0.6826 0.0003 0.2569 0.022 Uiso 1 1 calc R . . C21 C 0.9893(3) 0.14070(17) 0.10961(18) 0.0230(8) Uani 1 1 d . . . C22 C 0.9223(3) 0.20383(18) 0.0733(2) 0.0320(9) Uani 1 1 d . . . H22A H 0.9775 0.2280 0.0450 0.048 Uiso 1 1 calc R . . H22B H 0.8966 0.2347 0.1092 0.048 Uiso 1 1 calc R . . H22C H 0.8508 0.1882 0.0430 0.048 Uiso 1 1 calc R . . C23 C 1.0254(4) 0.09330(19) 0.04886(19) 0.0325(9) Uani 1 1 d . . . H23A H 1.0791 0.1183 0.0203 0.049 Uiso 1 1 calc R . . H23B H 0.9520 0.0792 0.0194 0.049 Uiso 1 1 calc R . . H23C H 1.0677 0.0528 0.0690 0.049 Uiso 1 1 calc R . . C24 C 1.1032(3) 0.16984(18) 0.15521(19) 0.0312(9) Uani 1 1 d . . . H24A H 1.1547 0.1944 0.1250 0.047 Uiso 1 1 calc R . . H24B H 1.1494 0.1322 0.1787 0.047 Uiso 1 1 calc R . . H24C H 1.0768 0.2012 0.1905 0.047 Uiso 1 1 calc R . . C25 C 0.8973(3) -0.07051(17) 0.26822(17) 0.0243(8) Uani 1 1 d . . . C26 C 0.7906(4) -0.10379(18) 0.3034(2) 0.0329(9) Uani 1 1 d . . . H26A H 0.7635 -0.0724 0.3385 0.049 Uiso 1 1 calc R . . H26B H 0.8184 -0.1465 0.3263 0.049 Uiso 1 1 calc R . . H26C H 0.7230 -0.1133 0.2675 0.049 Uiso 1 1 calc R . . C27 C 1.0046(4) -0.0574(2) 0.32773(19) 0.0368(9) Uani 1 1 d . . . H27A H 1.0734 -0.0368 0.3071 0.055 Uiso 1 1 calc R . . H27B H 1.0300 -0.1009 0.3500 0.055 Uiso 1 1 calc R . . H27C H 0.9769 -0.0265 0.3630 0.055 Uiso 1 1 calc R . . C28 C 0.9375(4) -0.12279(17) 0.2131(2) 0.0323(9) Uani 1 1 d . . . H28A H 1.0046 -0.1034 0.1900 0.048 Uiso 1 1 calc R . . H28B H 0.8688 -0.1324 0.1780 0.048 Uiso 1 1 calc R . . H28C H 0.9642 -0.1653 0.2370 0.048 Uiso 1 1 calc R . . C29 C 0.3751(3) 0.04718(16) 0.06800(17) 0.0201(7) Uani 1 1 d . . . C30 C 0.3006(3) 0.02392(18) -0.04596(18) 0.0286(8) Uani 1 1 d . . . H30 H 0.2468 0.0003 -0.0795 0.034 Uiso 1 1 calc R . . C31 C 0.3821(3) 0.07034(17) -0.06967(17) 0.0240(8) Uani 1 1 d . . . H31 H 0.3824 0.0791 -0.1184 0.029 Uiso 1 1 calc R . . C32 C 0.4637(3) 0.10392(16) -0.02063(17) 0.0225(8) Uani 1 1 d . . . C33 C 0.5595(4) 0.1550(2) -0.04034(18) 0.0342(9) Uani 1 1 d . . . H33A H 0.6061 0.1720 0.0024 0.051 Uiso 1 1 calc R . . H33B H 0.5192 0.1933 -0.0661 0.051 Uiso 1 1 calc R . . H33C H 0.6145 0.1323 -0.0699 0.051 Uiso 1 1 calc R . . C34 C 0.5426(3) 0.28150(16) 0.19475(16) 0.0191(7) Uani 1 1 d . . . C35 C 0.7014(3) 0.29253(17) 0.28465(17) 0.0220(7) Uani 1 1 d . . . C36 C 0.6986(3) 0.36377(17) 0.27490(17) 0.0254(8) Uani 1 1 d . . . H36 H 0.7511 0.3931 0.3034 0.030 Uiso 1 1 calc R . . C37 C 0.6151(3) 0.38971(17) 0.22135(17) 0.0249(8) Uani 1 1 d . . . H37 H 0.6138 0.4376 0.2137 0.030 Uiso 1 1 calc R . . C38 C 0.7885(3) 0.25697(19) 0.3403(2) 0.0341(9) Uani 1 1 d . . . H38A H 0.7750 0.2075 0.3378 0.051 Uiso 1 1 calc R . . H38B H 0.7740 0.2735 0.3869 0.051 Uiso 1 1 calc R . . H38C H 0.8725 0.2670 0.3318 0.051 Uiso 1 1 calc R . . N1 N 0.2946(3) 0.01080(14) 0.02412(14) 0.0252(6) Uani 1 1 d . . . N2 N 0.4608(3) 0.09195(14) 0.05002(14) 0.0219(6) Uani 1 1 d . . . N3 N 0.5357(3) 0.35025(14) 0.17962(14) 0.0236(6) Uani 1 1 d . . . N4 N 0.6221(2) 0.25137(13) 0.24455(13) 0.0185(6) Uani 1 1 d . . . O1 O 0.4120(2) 0.14181(12) 0.52968(11) 0.0242(5) Uani 1 1 d . . . H1 H 0.4738 0.1333 0.5573 0.036 Uiso 1 1 calc R . . O2 O 1.0576(2) 0.01244(12) 0.19368(12) 0.0272(6) Uani 1 1 d . . . H2A H 1.0987 0.0379 0.1701 0.041 Uiso 1 1 calc R . . S1 S 0.36574(8) 0.03477(4) 0.16059(4) 0.02081(19) Uani 1 1 d . . . S2 S 0.44203(8) 0.22638(4) 0.14261(4) 0.0248(2) Uani 1 1 d . . . Sn1 Sn 0.51748(2) 0.123279(11) 0.208169(11) 0.01641(8) 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 C1 0.0164(17) 0.0174(16) 0.0184(16) -0.0030(12) 0.0035(14) -0.0002(13) C2 0.0134(17) 0.0217(18) 0.0217(17) -0.0001(13) 0.0048(14) -0.0022(13) C3 0.0127(17) 0.0175(17) 0.0189(17) 0.0008(12) 0.0015(13) -0.0011(13) C4 0.0200(18) 0.0168(17) 0.0144(16) 0.0012(12) 0.0011(14) -0.0009(13) C5 0.0174(18) 0.0165(16) 0.0210(17) -0.0017(12) 0.0027(14) -0.0004(13) C6 0.0201(19) 0.0234(18) 0.0186(17) 0.0028(13) 0.0004(14) -0.0010(14) C7 0.0164(18) 0.0304(19) 0.0214(17) 0.0004(14) 0.0049(14) 0.0032(14) C8 0.0171(19) 0.043(2) 0.033(2) 0.0061(16) 0.0069(16) 0.0023(16) C9 0.028(2) 0.037(2) 0.033(2) -0.0073(16) 0.0041(17) 0.0103(17) C10 0.020(2) 0.049(2) 0.028(2) 0.0018(16) 0.0032(16) 0.0116(17) C11 0.0144(18) 0.0250(18) 0.0189(17) 0.0009(13) -0.0020(14) -0.0025(14) C12 0.026(2) 0.028(2) 0.0220(18) 0.0016(14) -0.0019(15) -0.0066(15) C13 0.0200(18) 0.0218(18) 0.0226(17) 0.0004(13) -0.0014(14) 0.0007(14) C14 0.0142(18) 0.0297(19) 0.0294(19) 0.0043(14) -0.0017(15) 0.0013(14) C15 0.0110(17) 0.0254(18) 0.0159(16) -0.0026(13) -0.0004(13) 0.0022(13) C16 0.0187(18) 0.0179(17) 0.0194(17) 0.0006(13) -0.0002(14) 0.0016(13) C17 0.0176(18) 0.0189(17) 0.0192(17) -0.0006(13) 0.0040(14) -0.0020(13) C18 0.0118(17) 0.0233(18) 0.0220(17) -0.0064(13) 0.0006(14) 0.0016(13) C19 0.0180(18) 0.0210(17) 0.0171(16) -0.0012(12) 0.0008(14) 0.0012(13) C20 0.0158(17) 0.0228(17) 0.0156(16) -0.0008(12) 0.0006(13) -0.0028(14) C21 0.0165(18) 0.0247(19) 0.0289(19) 0.0051(14) 0.0077(15) 0.0003(14) C22 0.021(2) 0.034(2) 0.043(2) 0.0124(17) 0.0130(18) 0.0015(16) C23 0.031(2) 0.034(2) 0.036(2) 0.0078(16) 0.0209(18) 0.0050(17) C24 0.0182(19) 0.027(2) 0.049(2) 0.0034(16) 0.0067(17) -0.0012(15) C25 0.0233(19) 0.0227(18) 0.0266(18) 0.0040(14) 0.0007(15) 0.0023(15) C26 0.036(2) 0.029(2) 0.036(2) 0.0154(16) 0.0098(18) 0.0051(17) C27 0.038(2) 0.038(2) 0.032(2) 0.0073(17) -0.0074(18) 0.0054(18) C28 0.033(2) 0.0200(18) 0.045(2) 0.0007(15) 0.0082(18) 0.0038(16) C29 0.0180(18) 0.0173(17) 0.0251(18) -0.0028(13) 0.0027(14) 0.0036(14) C30 0.022(2) 0.038(2) 0.0245(19) -0.0127(15) -0.0035(15) -0.0010(16) C31 0.026(2) 0.0275(19) 0.0183(17) -0.0044(14) 0.0017(15) 0.0031(15) C32 0.026(2) 0.0219(18) 0.0200(18) -0.0005(13) 0.0025(15) 0.0069(15) C33 0.041(2) 0.040(2) 0.0231(19) 0.0024(16) 0.0078(18) -0.0106(18) C34 0.0196(18) 0.0236(18) 0.0149(16) -0.0005(13) 0.0053(14) 0.0000(14) C35 0.0188(19) 0.0263(19) 0.0215(17) 0.0004(14) 0.0046(15) 0.0005(14) C36 0.026(2) 0.028(2) 0.0215(18) -0.0024(14) 0.0004(15) -0.0027(15) C37 0.036(2) 0.0202(18) 0.0193(18) -0.0027(13) 0.0040(16) -0.0015(15) C38 0.029(2) 0.029(2) 0.042(2) 0.0063(16) -0.0090(18) -0.0025(17) N1 0.0224(16) 0.0274(16) 0.0258(16) -0.0046(12) 0.0025(13) 0.0021(13) N2 0.0187(16) 0.0250(15) 0.0221(15) -0.0021(11) 0.0035(12) -0.0011(12) N3 0.0269(17) 0.0227(15) 0.0210(15) 0.0015(12) 0.0024(13) 0.0016(13) N4 0.0161(15) 0.0218(15) 0.0178(14) -0.0008(11) 0.0032(12) 0.0001(11) O1 0.0204(13) 0.0370(14) 0.0149(12) -0.0008(9) 0.0010(10) 0.0041(10) O2 0.0141(13) 0.0273(13) 0.0418(14) 0.0083(11) 0.0100(11) 0.0039(10) S1 0.0194(5) 0.0223(4) 0.0209(4) 0.0025(3) 0.0028(3) -0.0020(3) S2 0.0293(5) 0.0225(5) 0.0209(4) 0.0030(3) -0.0053(4) -0.0030(4) Sn1 0.01247(13) 0.02225(13) 0.01484(13) 0.00167(8) 0.00301(9) 0.00079(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.385(4) . ? C1 C6 1.390(4) . ? C1 Sn1 2.115(3) . ? C2 C3 1.395(4) . ? C2 H2 0.9300 . ? C3 C4 1.410(4) . ? C3 C11 1.534(4) . ? C4 O1 1.377(3) . ? C4 C5 1.410(4) . ? C5 C6 1.400(4) . ? C5 C7 1.543(4) . ? C6 H6 0.9300 . ? C7 C10 1.533(5) . ? C7 C9 1.533(5) . ? C7 C8 1.538(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C14 1.537(4) . ? C11 C13 1.543(4) . ? C11 C12 1.538(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.387(4) . ? C15 C16 1.392(4) . ? C15 Sn1 2.116(3) . ? C16 C17 1.393(4) . ? C16 H16 0.9300 . ? C17 C18 1.407(4) . ? C17 C21 1.552(4) . ? C18 O2 1.373(4) . ? C18 C19 1.410(4) . ? C19 C20 1.390(4) . ? C19 C25 1.555(4) . ? C20 H20 0.9300 . ? C21 C24 1.533(5) . ? C21 C22 1.536(5) . ? C21 C23 1.540(5) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C28 1.536(5) . ? C25 C26 1.530(5) . ? C25 C27 1.547(5) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N2 1.334(4) . ? C29 N1 1.333(4) . ? C29 S1 1.767(3) . ? C30 N1 1.347(4) . ? C30 C31 1.362(5) . ? C30 H30 0.9300 . ? C31 C32 1.370(5) . ? C31 H31 0.9300 . ? C32 N2 1.349(4) . ? C32 C33 1.502(5) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 N4 1.336(4) . ? C34 N3 1.350(4) . ? C34 S2 1.745(3) . ? C35 N4 1.340(4) . ? C35 C36 1.379(4) . ? C35 C38 1.498(5) . ? C36 C37 1.374(5) . ? C36 H36 0.9300 . ? C37 N3 1.337(4) . ? C37 H37 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? O1 H1 0.8200 . ? O2 H2A 0.8200 . ? S1 Sn1 2.4664(8) . ? S2 Sn1 2.4265(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.1(3) . . ? C2 C1 Sn1 119.5(2) . . ? C6 C1 Sn1 122.3(2) . . ? C1 C2 C3 123.4(3) . . ? C1 C2 H2 118.3 . . ? C3 C2 H2 118.3 . . ? C2 C3 C4 116.2(3) . . ? C2 C3 C11 120.6(3) . . ? C4 C3 C11 123.2(3) . . ? O1 C4 C5 114.2(3) . . ? O1 C4 C3 122.8(3) . . ? C5 C4 C3 123.0(3) . . ? C6 C5 C4 116.7(3) . . ? C6 C5 C7 120.7(3) . . ? C4 C5 C7 122.5(3) . . ? C1 C6 C5 122.5(3) . . ? C1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C10 C7 C9 107.5(3) . . ? C10 C7 C8 106.6(3) . . ? C9 C7 C8 110.5(3) . . ? C10 C7 C5 111.6(3) . . ? C9 C7 C5 108.5(3) . . ? C8 C7 C5 112.0(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C3 112.4(2) . . ? C14 C11 C13 105.2(3) . . ? C3 C11 C13 111.3(3) . . ? C14 C11 C12 106.4(3) . . ? C3 C11 C12 109.7(3) . . ? C13 C11 C12 111.7(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 118.8(3) . . ? C20 C15 Sn1 119.0(2) . . ? C16 C15 Sn1 122.2(2) . . ? C15 C16 C17 122.0(3) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C16 C17 C18 117.3(3) . . ? C16 C17 C21 120.1(3) . . ? C18 C17 C21 122.5(3) . . ? O2 C18 C19 115.6(3) . . ? O2 C18 C17 122.0(3) . . ? C19 C18 C17 122.4(3) . . ? C20 C19 C18 117.2(3) . . ? C20 C19 C25 120.7(3) . . ? C18 C19 C25 122.1(3) . . ? C15 C20 C19 122.4(3) . . ? C15 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C24 C21 C22 106.1(3) . . ? C24 C21 C23 112.1(3) . . ? C22 C21 C23 106.4(3) . . ? C24 C21 C17 111.7(3) . . ? C22 C21 C17 110.9(3) . . ? C23 C21 C17 109.5(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C26 107.3(3) . . ? C28 C25 C27 110.4(3) . . ? C26 C25 C27 107.5(3) . . ? C28 C25 C19 109.9(3) . . ? C26 C25 C19 111.8(3) . . ? C27 C25 C19 109.9(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 N1 127.5(3) . . ? N2 C29 S1 116.6(2) . . ? N1 C29 S1 115.9(2) . . ? N1 C30 C31 122.7(3) . . ? N1 C30 H30 118.7 . . ? C31 C30 H30 118.7 . . ? C30 C31 C32 118.9(3) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? N2 C32 C31 120.1(3) . . ? N2 C32 C33 116.1(3) . . ? C31 C32 C33 123.8(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 N3 126.0(3) . . ? N4 C34 S2 116.8(2) . . ? N3 C34 S2 117.2(2) . . ? N4 C35 C36 120.4(3) . . ? N4 C35 C38 116.4(3) . . ? C36 C35 C38 123.2(3) . . ? C37 C36 C35 117.4(3) . . ? C37 C36 H36 121.3 . . ? C35 C36 H36 121.3 . . ? N3 C37 C36 124.0(3) . . ? N3 C37 H37 118.0 . . ? C36 C37 H37 118.0 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C29 N1 C30 114.3(3) . . ? C29 N2 C32 116.5(3) . . ? C37 N3 C34 114.3(3) . . ? C34 N4 C35 117.9(3) . . ? C4 O1 H1 109.5 . . ? C18 O2 H2A 109.5 . . ? C29 S1 Sn1 99.16(11) . . ? C34 S2 Sn1 92.96(11) . . ? C1 Sn1 C15 111.43(12) . . ? C1 Sn1 S2 113.11(8) . . ? C15 Sn1 S2 119.56(9) . . ? C1 Sn1 S1 99.24(9) . . ? C15 Sn1 S1 109.31(9) . . ? S2 Sn1 S1 101.57(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.571 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.082 data_shelxl4 _database_code_depnum_ccdc_archive 'CCDC 891292' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H41 Cl N O2 S Sn, C33 H44 Cl N O2 S Sn' _chemical_formula_sum 'C66 H85 Cl2 N2 O4 S2 Sn2' _chemical_formula_weight 1342.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn 0.0259 5.4591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.0304(13) _cell_length_b 11.0367(3) _cell_length_c 33.5317(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.048(3) _cell_angle_gamma 90.00 _cell_volume 13315.2(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100.2(2) _cell_measurement_reflns_used 15076 _cell_measurement_theta_min 3.6979 _cell_measurement_theta_max 67.2519 _exptl_crystal_description rectangle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5544 _exptl_absorpt_coefficient_mu 7.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.48362 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4223 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40974 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 67.00 _reflns_number_total 11863 _reflns_number_gt 10850 _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^)+(0.1110P)^2^+3.9870P] 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 11863 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1406 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.98269(9) 1.1850(3) 0.41672(9) 0.0186(6) Uani 1 1 d . . . C2 C 0.99971(9) 1.0865(3) 0.39931(9) 0.0190(6) Uani 1 1 d . . . H2 H 0.9910 1.0089 0.4043 0.023 Uiso 1 1 calc R . . C3 C 1.02943(9) 1.1004(3) 0.37446(9) 0.0206(7) Uani 1 1 d . . . C4 C 1.04172(10) 1.2198(3) 0.36785(10) 0.0223(7) Uani 1 1 d . . . C5 C 1.02501(10) 1.3222(3) 0.38430(10) 0.0228(7) Uani 1 1 d . . . C6 C 0.99540(10) 1.3011(3) 0.40861(10) 0.0219(7) Uani 1 1 d . . . H6 H 0.9837 1.3671 0.4198 0.026 Uiso 1 1 calc R . . C7 C 1.03895(12) 1.4519(3) 0.37731(13) 0.0344(9) Uani 1 1 d . . . C8 C 1.07876(14) 1.4637(4) 0.39589(17) 0.0510(13) Uani 1 1 d . . . H8A H 1.0946 1.4060 0.3837 0.076 Uiso 1 1 calc R . . H8B H 1.0787 1.4482 0.4241 0.076 Uiso 1 1 calc R . . H8C H 1.0878 1.5441 0.3915 0.076 Uiso 1 1 calc R . . C9 C 1.03752(17) 1.4817(4) 0.33226(14) 0.0512(13) Uani 1 1 d . . . C10 C 1.01501(15) 1.5455(3) 0.39772(15) 0.0455(12) Uani 1 1 d . . . H10A H 1.0243 1.6253 0.3929 0.068 Uiso 1 1 calc R . . H10B H 1.0159 1.5303 0.4259 0.068 Uiso 1 1 calc R . . H10C H 0.9898 1.5395 0.3871 0.068 Uiso 1 1 calc R . . C11 C 1.04811(10) 0.9890(3) 0.35641(10) 0.0236(7) Uani 1 1 d . . . C12 C 1.02930(11) 0.8709(3) 0.36786(11) 0.0285(8) Uani 1 1 d . . . H12A H 1.0037 0.8725 0.3585 0.043 Uiso 1 1 calc R . . H12B H 1.0309 0.8620 0.3964 0.043 Uiso 1 1 calc R . . H12C H 1.0415 0.8038 0.3559 0.043 Uiso 1 1 calc R . . C13 C 1.08900(12) 0.9792(4) 0.37228(13) 0.0367(9) Uani 1 1 d . . . H13A H 1.1021 1.0517 0.3657 0.055 Uiso 1 1 calc R . . H13B H 1.1004 0.9107 0.3603 0.055 Uiso 1 1 calc R . . H13C H 1.0899 0.9692 0.4008 0.055 Uiso 1 1 calc R . . C14 C 1.04530(11) 0.9942(3) 0.31005(10) 0.0282(7) Uani 1 1 d . . . H14A H 1.0568 1.0671 0.3012 0.042 Uiso 1 1 calc R . . H14B H 1.0196 0.9935 0.3008 0.042 Uiso 1 1 calc R . . H14C H 1.0577 0.9252 0.2995 0.042 Uiso 1 1 calc R . . C15 C 0.88206(9) 1.1850(3) 0.43275(9) 0.0195(6) Uani 1 1 d . . . C16 C 0.86226(9) 1.0851(3) 0.41645(9) 0.0181(6) Uani 1 1 d . . . H16 H 0.8720 1.0076 0.4201 0.022 Uiso 1 1 calc R . . C17 C 0.82853(10) 1.0996(3) 0.39497(10) 0.0222(7) Uani 1 1 d . . . C18 C 0.81429(10) 1.2181(3) 0.39067(11) 0.0243(7) Uani 1 1 d . . . C19 C 0.86751(10) 1.2998(3) 0.42781(10) 0.0214(7) Uani 1 1 d . . . H19 H 0.8807 1.3654 0.4386 0.026 Uiso 1 1 calc R . . C20 C 0.83346(10) 1.3202(3) 0.40706(11) 0.0241(7) Uani 1 1 d . . . C21 C 0.81836(11) 1.4511(3) 0.40115(13) 0.0309(9) Uani 1 1 d . . . C22 C 0.78036(13) 1.4651(4) 0.41988(16) 0.0465(11) Uani 1 1 d . . . H22A H 0.7827 1.4431 0.4476 0.070 Uiso 1 1 calc R . . H22B H 0.7625 1.4133 0.4062 0.070 Uiso 1 1 calc R . . H22C H 0.7723 1.5478 0.4175 0.070 Uiso 1 1 calc R . . C23 C 0.84475(13) 1.5422(3) 0.42245(15) 0.0415(11) Uani 1 1 d . . . H23A H 0.8688 1.5368 0.4116 0.062 Uiso 1 1 calc R . . H23B H 0.8468 1.5242 0.4505 0.062 Uiso 1 1 calc R . . H23C H 0.8351 1.6227 0.4186 0.062 Uiso 1 1 calc R . . C24 C 0.81609(13) 1.4852(4) 0.35705(14) 0.0413(10) Uani 1 1 d . . . H24A H 0.8401 1.4757 0.3463 0.062 Uiso 1 1 calc R . . H24B H 0.8082 1.5680 0.3542 0.062 Uiso 1 1 calc R . . H24C H 0.7985 1.4335 0.3429 0.062 Uiso 1 1 calc R . . C25 C 0.80930(10) 0.9903(3) 0.37414(10) 0.0229(7) Uani 1 1 d . . . C26 C 0.76912(10) 0.9738(3) 0.38733(12) 0.0289(8) Uani 1 1 d . . . H26A H 0.7551 1.0463 0.3815 0.043 Uiso 1 1 calc R . . H26B H 0.7696 0.9580 0.4155 0.043 Uiso 1 1 calc R . . H26C H 0.7577 0.9069 0.3731 0.043 Uiso 1 1 calc R . . C27 C 0.80903(12) 1.0074(4) 0.32859(11) 0.0350(9) Uani 1 1 d . . . H27A H 0.7962 1.0811 0.3213 0.053 Uiso 1 1 calc R . . H27B H 0.7966 0.9401 0.3156 0.053 Uiso 1 1 calc R . . H27C H 0.8341 1.0116 0.3204 0.053 Uiso 1 1 calc R . . C28 C 0.82982(11) 0.8725(3) 0.38397(12) 0.0311(8) Uani 1 1 d . . . H28A H 0.8171 0.8064 0.3706 0.047 Uiso 1 1 calc R . . H28B H 0.8306 0.8591 0.4123 0.047 Uiso 1 1 calc R . . H28C H 0.8547 0.8777 0.3753 0.047 Uiso 1 1 calc R . . C29 C 0.94758(10) 0.9235(3) 0.48809(10) 0.0237(7) Uani 1 1 d . . . C30 C 0.93515(10) 0.8568(3) 0.42292(11) 0.0260(7) Uani 1 1 d . . . H30 H 0.9290 0.8746 0.3963 0.031 Uiso 1 1 calc R . . C31 C 0.94043(11) 0.7378(3) 0.43415(12) 0.0319(8) Uani 1 1 d . . . H31 H 0.9378 0.6757 0.4155 0.038 Uiso 1 1 calc R . . C32 C 0.94989(11) 0.7123(3) 0.47427(14) 0.0353(9) Uani 1 1 d . . . H32 H 0.9538 0.6327 0.4826 0.042 Uiso 1 1 calc R . . C33 C 0.95331(10) 0.8063(3) 0.50141(12) 0.0289(8) Uani 1 1 d . . . H33 H 0.9594 0.7909 0.5282 0.035 Uiso 1 1 calc R . . C34 C 0.18752(9) 0.0148(3) 0.37385(9) 0.0212(7) Uani 1 1 d . . . C35 C 0.18308(9) -0.1036(3) 0.38711(10) 0.0211(7) Uani 1 1 d . . . H35 H 0.1848 -0.1666 0.3689 0.025 Uiso 1 1 calc R . . C36 C 0.17614(9) -0.1315(3) 0.42657(10) 0.0228(7) Uani 1 1 d . . . C37 C 0.17400(10) -0.0329(3) 0.45301(10) 0.0238(7) Uani 1 1 d . . . C38 C 0.18583(9) 0.1093(3) 0.40120(10) 0.0212(7) Uani 1 1 d . . . H38 H 0.1892 0.1884 0.3926 0.025 Uiso 1 1 calc R . . C39 C 0.17921(10) 0.0884(3) 0.44108(10) 0.0225(7) Uani 1 1 d . . . C40 C 0.17696(11) 0.1946(3) 0.47089(10) 0.0266(8) Uani 1 1 d . . . C41 C 0.13743(12) 0.2028(4) 0.48560(13) 0.0375(9) Uani 1 1 d . . . H41A H 0.1312 0.1279 0.4981 0.056 Uiso 1 1 calc R . . H41B H 0.1202 0.2181 0.4633 0.056 Uiso 1 1 calc R . . H41C H 0.1362 0.2677 0.5046 0.056 Uiso 1 1 calc R . . C42 C 0.18607(13) 0.3154(3) 0.45137(12) 0.0339(9) Uani 1 1 d . . . H42A H 0.1688 0.3297 0.4290 0.051 Uiso 1 1 calc R . . H42B H 0.2109 0.3127 0.4423 0.051 Uiso 1 1 calc R . . H42C H 0.1842 0.3796 0.4705 0.051 Uiso 1 1 calc R . . C43 C 0.20513(13) 0.1748(4) 0.50646(12) 0.0368(10) Uani 1 1 d . . . H43A H 0.1999 0.0994 0.5193 0.055 Uiso 1 1 calc R . . H43B H 0.2032 0.2400 0.5252 0.055 Uiso 1 1 calc R . . H43C H 0.2298 0.1727 0.4971 0.055 Uiso 1 1 calc R . . C44 C 0.13442(12) -0.2878(4) 0.45729(12) 0.0347(9) Uani 1 1 d . . . H44A H 0.1313 -0.2355 0.4797 0.052 Uiso 1 1 calc R . . H44B H 0.1331 -0.3708 0.4657 0.052 Uiso 1 1 calc R . . H44C H 0.1151 -0.2722 0.4372 0.052 Uiso 1 1 calc R . . C45 C 0.17521(12) -0.3506(3) 0.40446(12) 0.0318(8) Uani 1 1 d . . . H45A H 0.1730 -0.4326 0.4136 0.048 Uiso 1 1 calc R . . H45B H 0.1987 -0.3402 0.3927 0.048 Uiso 1 1 calc R . . H45C H 0.1555 -0.3334 0.3849 0.048 Uiso 1 1 calc R . . C46 C 0.20484(14) -0.2964(4) 0.47030(14) 0.0456(11) Uani 1 1 d . . . H46A H 0.2043 -0.2437 0.4930 0.068 Uiso 1 1 calc R . . H46B H 0.2281 -0.2871 0.4580 0.068 Uiso 1 1 calc R . . H46C H 0.2022 -0.3789 0.4788 0.068 Uiso 1 1 calc R . . C47 C 0.14633(9) 0.0196(3) 0.27074(9) 0.0203(7) Uani 1 1 d . . . C48 C 0.13382(10) -0.0958(3) 0.26092(10) 0.0231(7) Uani 1 1 d . . . H48 H 0.1457 -0.1620 0.2731 0.028 Uiso 1 1 calc R . . C49 C 0.10397(10) -0.1165(3) 0.23342(10) 0.0236(7) Uani 1 1 d . . . C50 C 0.12850(10) 0.1186(3) 0.25302(10) 0.0210(7) Uani 1 1 d . . . H50 H 0.1365 0.1962 0.2601 0.025 Uiso 1 1 calc R . . C51 C 0.08811(10) -0.0135(3) 0.21461(9) 0.0212(7) Uani 1 1 d . . . C52 C 0.09880(9) 0.1053(3) 0.22471(9) 0.0197(7) Uani 1 1 d . . . C53 C 0.08001(10) 0.2186(3) 0.20565(10) 0.0242(7) Uani 1 1 d . . . C54 C 0.03817(11) 0.2199(4) 0.21196(12) 0.0334(8) Uani 1 1 d . . . H54A H 0.0270 0.1478 0.2007 0.050 Uiso 1 1 calc R . . H54B H 0.0271 0.2898 0.1991 0.050 Uiso 1 1 calc R . . H54C H 0.0342 0.2230 0.2400 0.050 Uiso 1 1 calc R . . C55 C 0.08784(11) 0.2243(3) 0.16098(10) 0.0296(8) Uani 1 1 d . . . H55A H 0.0783 0.1527 0.1478 0.044 Uiso 1 1 calc R . . H55B H 0.1142 0.2293 0.1581 0.044 Uiso 1 1 calc R . . H55C H 0.0760 0.2945 0.1492 0.044 Uiso 1 1 calc R . . C56 C 0.09619(12) 0.3350(3) 0.22412(12) 0.0315(9) Uani 1 1 d . . . H56A H 0.1225 0.3375 0.2208 0.047 Uiso 1 1 calc R . . H56B H 0.0917 0.3370 0.2521 0.047 Uiso 1 1 calc R . . H56C H 0.0846 0.4038 0.2111 0.047 Uiso 1 1 calc R . . C57 C 0.09000(11) -0.2468(3) 0.22459(11) 0.0265(8) Uani 1 1 d . . . C58 C 0.11018(15) -0.3386(3) 0.25229(14) 0.0437(11) Uani 1 1 d . . . H58A H 0.1011 -0.4186 0.2461 0.066 Uiso 1 1 calc R . . H58B H 0.1057 -0.3196 0.2795 0.066 Uiso 1 1 calc R . . H58C H 0.1364 -0.3352 0.2485 0.066 Uiso 1 1 calc R . . C59 C 0.09764(14) -0.2827(3) 0.18139(12) 0.0379(9) Uani 1 1 d . . . H59A H 0.0890 -0.3638 0.1763 0.057 Uiso 1 1 calc R . . H59B H 0.1239 -0.2787 0.1778 0.057 Uiso 1 1 calc R . . H59C H 0.0848 -0.2280 0.1631 0.057 Uiso 1 1 calc R . . C60 C 0.04864(12) -0.2591(4) 0.23132(13) 0.0381(9) Uani 1 1 d . . . H60A H 0.0408 -0.3407 0.2256 0.057 Uiso 1 1 calc R . . H60B H 0.0348 -0.2043 0.2140 0.057 Uiso 1 1 calc R . . H60C H 0.0443 -0.2400 0.2586 0.057 Uiso 1 1 calc R . . C61 C 0.16037(10) 0.3428(3) 0.32560(10) 0.0251(7) Uani 1 1 d . . . H61 H 0.1396 0.3203 0.3391 0.030 Uiso 1 1 calc R . . C62 C 0.16555(11) 0.4627(3) 0.31685(11) 0.0280(8) Uani 1 1 d . . . H62 H 0.1486 0.5207 0.3245 0.034 Uiso 1 1 calc R . . C63 C 0.19662(11) 0.4967(3) 0.29629(11) 0.0294(8) Uani 1 1 d . . . H63 H 0.2007 0.5777 0.2903 0.035 Uiso 1 1 calc R . . C64 C 0.22132(10) 0.4082(3) 0.28495(10) 0.0262(7) Uani 1 1 d . . . H64 H 0.2419 0.4283 0.2707 0.031 Uiso 1 1 calc R . . C65 C 0.21448(10) 0.2886(3) 0.29541(10) 0.0221(7) Uani 1 1 d . . . C66 C 0.17265(11) -0.2635(3) 0.43994(11) 0.0271(8) Uani 1 1 d . . . N1 N 0.93864(8) 0.9481(3) 0.44944(9) 0.0206(6) Uani 1 1 d . . . N2 N 0.18456(8) 0.2564(3) 0.31520(8) 0.0213(6) Uani 1 1 d . . . O1 O 1.07141(8) 1.2410(2) 0.34430(8) 0.0331(6) Uani 1 1 d . . . O2 O 0.78093(8) 1.2283(2) 0.36951(9) 0.0351(6) Uani 1 1 d . . . O3 O 0.16657(9) -0.0502(2) 0.49249(8) 0.0342(6) Uani 1 1 d . . . O4 O 0.06058(7) -0.0356(2) 0.18497(8) 0.0272(6) Uani 1 1 d . . . S1 S 0.95113(2) 1.05376(8) 0.51811(2) 0.02408(19) Uani 1 1 d . . . S2 S 0.24298(2) 0.16394(8) 0.28502(3) 0.0258(2) Uani 1 1 d . . . Cl1 Cl 0.94543(2) 1.36192(7) 0.48919(2) 0.02499(18) Uani 1 1 d . . . Cl2 Cl 0.22394(2) -0.15094(7) 0.29921(2) 0.02604(19) Uani 1 1 d . . . Sn1 Sn 0.938150(6) 1.165785(19) 0.455831(6) 0.01730(10) Uani 1 1 d . . . Sn2 Sn 0.193175(6) 0.041808(19) 0.311934(6) 0.01876(10) 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 C1 0.0185(15) 0.0230(16) 0.0144(15) 0.0005(12) 0.0014(12) 0.0016(12) C2 0.0223(16) 0.0211(16) 0.0137(15) -0.0002(12) 0.0009(12) -0.0002(12) C3 0.0240(16) 0.0239(17) 0.0141(15) -0.0001(12) 0.0012(12) 0.0011(13) C4 0.0246(17) 0.0250(17) 0.0179(16) -0.0012(13) 0.0071(13) -0.0039(13) C5 0.0269(18) 0.0199(17) 0.0218(17) 0.0007(13) 0.0041(14) -0.0026(13) C6 0.0289(17) 0.0206(16) 0.0163(16) 0.0007(13) 0.0026(13) 0.0034(13) C7 0.046(2) 0.0234(19) 0.036(2) -0.0058(15) 0.0232(19) -0.0093(16) C8 0.049(3) 0.042(3) 0.064(3) -0.021(2) 0.025(2) -0.022(2) C9 0.093(4) 0.024(2) 0.040(3) 0.0067(18) 0.032(3) -0.007(2) C10 0.063(3) 0.023(2) 0.054(3) -0.0011(18) 0.034(2) -0.0063(18) C11 0.0284(18) 0.0240(17) 0.0191(17) -0.0019(14) 0.0072(13) 0.0010(14) C12 0.039(2) 0.0239(18) 0.0242(18) -0.0001(14) 0.0138(15) 0.0056(15) C13 0.034(2) 0.041(2) 0.035(2) -0.0039(17) 0.0075(17) 0.0054(17) C14 0.036(2) 0.0276(18) 0.0217(18) -0.0018(14) 0.0082(14) -0.0003(15) C15 0.0184(15) 0.0246(17) 0.0154(15) 0.0030(12) 0.0004(12) 0.0067(13) C16 0.0246(16) 0.0162(15) 0.0136(15) 0.0000(12) 0.0038(12) 0.0000(12) C17 0.0252(17) 0.0253(18) 0.0167(16) 0.0020(13) 0.0057(13) -0.0007(14) C18 0.0225(17) 0.0256(18) 0.0245(18) 0.0050(14) -0.0010(14) -0.0021(14) C19 0.0261(17) 0.0202(16) 0.0182(16) 0.0002(13) 0.0039(13) 0.0004(13) C20 0.0278(18) 0.0187(16) 0.0259(18) 0.0003(13) 0.0010(14) 0.0033(13) C21 0.031(2) 0.0222(19) 0.039(2) 0.0004(15) -0.0093(17) 0.0026(14) C22 0.041(3) 0.039(2) 0.059(3) -0.003(2) -0.001(2) 0.0149(19) C23 0.046(3) 0.0208(19) 0.056(3) -0.0021(17) -0.014(2) 0.0065(16) C24 0.048(2) 0.027(2) 0.048(3) 0.0120(18) -0.014(2) -0.0015(18) C25 0.0257(17) 0.0220(17) 0.0211(18) 0.0012(13) 0.0020(13) -0.0016(14) C26 0.0294(19) 0.0257(18) 0.032(2) 0.0038(15) 0.0042(15) -0.0026(14) C27 0.037(2) 0.045(2) 0.0221(19) -0.0037(17) 0.0012(15) -0.0116(18) C28 0.035(2) 0.0211(18) 0.037(2) -0.0066(15) -0.0042(16) -0.0023(15) C29 0.0233(17) 0.0273(18) 0.0207(18) 0.0052(14) 0.0031(13) -0.0006(14) C30 0.0277(18) 0.0252(17) 0.0254(18) -0.0012(14) 0.0051(14) -0.0023(14) C31 0.032(2) 0.0239(18) 0.040(2) -0.0056(16) 0.0068(16) -0.0020(15) C32 0.029(2) 0.0209(18) 0.055(3) 0.0100(17) 0.0020(18) -0.0013(15) C33 0.0260(18) 0.0290(19) 0.031(2) 0.0099(15) -0.0057(15) -0.0008(15) C34 0.0232(16) 0.0279(17) 0.0127(15) 0.0017(13) 0.0017(12) -0.0005(13) C35 0.0220(16) 0.0244(17) 0.0168(16) -0.0012(13) 0.0010(12) 0.0011(13) C36 0.0216(16) 0.0271(18) 0.0198(17) 0.0005(14) 0.0012(13) -0.0030(13) C37 0.0273(18) 0.0294(19) 0.0150(17) 0.0026(13) 0.0050(13) -0.0051(14) C38 0.0242(16) 0.0192(16) 0.0204(17) 0.0029(13) 0.0046(13) -0.0013(12) C39 0.0279(17) 0.0236(17) 0.0160(16) -0.0014(13) 0.0017(13) -0.0014(13) C40 0.035(2) 0.0273(18) 0.0175(17) -0.0026(14) 0.0057(14) -0.0055(15) C41 0.044(2) 0.035(2) 0.035(2) -0.0068(17) 0.0168(18) -0.0023(18) C42 0.053(3) 0.0249(18) 0.0240(19) -0.0033(15) 0.0063(17) -0.0073(17) C43 0.048(2) 0.040(2) 0.0221(19) -0.0062(16) 0.0000(17) -0.0142(18) C44 0.044(2) 0.033(2) 0.028(2) -0.0018(16) 0.0147(17) -0.0131(17) C45 0.045(2) 0.0215(17) 0.030(2) 0.0026(15) 0.0147(17) -0.0014(15) C46 0.056(3) 0.033(2) 0.046(3) 0.0136(19) -0.011(2) -0.004(2) C47 0.0256(17) 0.0242(16) 0.0113(15) -0.0022(12) 0.0039(12) -0.0022(13) C48 0.0306(18) 0.0213(17) 0.0177(16) 0.0046(13) 0.0042(13) 0.0044(14) C49 0.0331(19) 0.0199(16) 0.0185(16) 0.0009(13) 0.0077(14) -0.0029(14) C50 0.0279(17) 0.0186(16) 0.0171(16) -0.0007(12) 0.0060(13) 0.0012(13) C51 0.0297(18) 0.0234(16) 0.0109(15) 0.0009(12) 0.0031(13) 0.0022(14) C52 0.0269(17) 0.0218(16) 0.0108(15) 0.0010(12) 0.0046(12) -0.0003(13) C53 0.0332(19) 0.0224(17) 0.0165(16) -0.0007(13) -0.0025(14) 0.0025(14) C54 0.036(2) 0.032(2) 0.032(2) 0.0020(16) -0.0012(16) 0.0029(16) C55 0.041(2) 0.0311(19) 0.0168(17) 0.0072(14) -0.0006(14) 0.0017(16) C56 0.046(2) 0.0195(18) 0.028(2) 0.0002(14) -0.0106(17) 0.0060(15) C57 0.038(2) 0.0204(17) 0.0210(18) -0.0007(14) 0.0025(15) -0.0015(15) C58 0.069(3) 0.022(2) 0.039(2) 0.0025(16) -0.009(2) -0.0054(18) C59 0.063(3) 0.0220(19) 0.030(2) -0.0052(15) 0.0096(19) -0.0019(17) C60 0.046(2) 0.027(2) 0.042(2) -0.0063(17) 0.0075(18) -0.0117(17) C61 0.0270(18) 0.0310(19) 0.0172(17) -0.0032(13) 0.0016(13) 0.0011(14) C62 0.034(2) 0.0238(18) 0.0255(19) -0.0024(13) 0.0004(15) 0.0022(14) C63 0.041(2) 0.0193(17) 0.028(2) 0.0023(15) 0.0008(15) -0.0029(15) C64 0.0316(19) 0.0267(18) 0.0208(17) 0.0024(14) 0.0050(14) 0.0001(15) C65 0.0265(17) 0.0238(17) 0.0159(16) -0.0002(13) 0.0010(13) -0.0011(13) C66 0.0320(19) 0.0261(18) 0.0237(18) 0.0062(14) 0.0043(15) -0.0020(15) N1 0.0208(15) 0.0227(15) 0.0185(15) 0.0000(11) 0.0026(11) -0.0005(10) N2 0.0275(14) 0.0237(15) 0.0125(14) -0.0004(11) 0.0000(11) 0.0031(12) O1 0.0350(15) 0.0292(14) 0.0369(15) -0.0046(11) 0.0196(12) -0.0107(11) O2 0.0315(14) 0.0273(14) 0.0447(16) 0.0033(11) -0.0134(12) 0.0000(11) O3 0.0540(18) 0.0347(15) 0.0147(13) 0.0003(10) 0.0086(12) -0.0126(12) O4 0.0308(14) 0.0230(12) 0.0268(14) -0.0037(9) -0.0072(11) -0.0020(10) S1 0.0290(4) 0.0280(4) 0.0152(4) 0.0028(3) 0.0008(3) -0.0006(3) S2 0.0264(4) 0.0257(4) 0.0260(4) 0.0034(3) 0.0092(3) 0.0016(3) Cl1 0.0307(4) 0.0227(4) 0.0219(4) -0.0061(3) 0.0053(3) -0.0021(3) Cl2 0.0329(4) 0.0238(4) 0.0220(4) 0.0012(3) 0.0065(3) 0.0063(3) Sn1 0.02069(15) 0.01852(15) 0.01293(15) -0.00002(7) 0.00316(10) 0.00070(7) Sn2 0.02383(15) 0.01963(15) 0.01300(15) 0.00140(7) 0.00283(10) 0.00130(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.392(5) . ? C1 C6 1.393(5) . ? C1 Sn1 2.136(3) . ? C2 C3 1.400(5) . ? C2 H2 0.9300 . ? C3 C4 1.412(5) . ? C3 C11 1.541(5) . ? C4 O1 1.383(4) . ? C4 C5 1.406(5) . ? C5 C6 1.396(5) . ? C5 C7 1.539(5) . ? C6 H6 0.9300 . ? C7 C10 1.531(5) . ? C7 C8 1.539(7) . ? C7 C9 1.544(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.528(5) . ? C11 C13 1.544(5) . ? C11 C14 1.553(5) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C19 1.377(5) . ? C15 C16 1.408(5) . ? C15 Sn1 2.136(3) . ? C16 C17 1.389(5) . ? C16 H16 0.9300 . ? C17 C18 1.409(5) . ? C17 C25 1.540(5) . ? C18 O2 1.367(4) . ? C18 C20 1.417(5) . ? C19 C20 1.396(5) . ? C19 H19 0.9300 . ? C20 C21 1.553(5) . ? C21 C24 1.524(6) . ? C21 C23 1.534(5) . ? C21 C22 1.544(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C28 1.523(5) . ? C25 C27 1.538(5) . ? C25 C26 1.547(5) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N1 1.346(5) . ? C29 C33 1.381(5) . ? C29 S1 1.755(4) . ? C30 N1 1.345(5) . ? C30 C31 1.377(5) . ? C30 H30 0.9300 . ? C31 C32 1.399(6) . ? C31 H31 0.9300 . ? C32 C33 1.381(6) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.392(5) . ? C34 C38 1.393(5) . ? C34 Sn2 2.118(3) . ? C35 C36 1.394(5) . ? C35 H35 0.9300 . ? C36 C37 1.408(5) . ? C36 C66 1.532(5) . ? C37 O3 1.378(4) . ? C37 C39 1.413(5) . ? C38 C39 1.390(5) . ? C38 H38 0.9300 . ? C39 C40 1.546(5) . ? C40 C42 1.528(5) . ? C40 C41 1.534(5) . ? C40 C43 1.540(6) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C66 1.547(5) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C66 1.536(5) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C66 1.545(5) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C50 1.385(5) . ? C47 C48 1.386(5) . ? C47 Sn2 2.138(3) . ? C48 C49 1.397(5) . ? C48 H48 0.9300 . ? C49 C51 1.406(5) . ? C49 C57 1.547(5) . ? C50 C52 1.400(5) . ? C50 H50 0.9300 . ? C51 O4 1.388(4) . ? C51 C52 1.403(5) . ? C52 C53 1.544(5) . ? C53 C56 1.529(5) . ? C53 C54 1.533(5) . ? C53 C55 1.540(5) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C60 1.525(6) . ? C57 C58 1.532(5) . ? C57 C59 1.541(5) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 N2 1.351(5) . ? C61 C62 1.370(5) . ? C61 H61 0.9300 . ? C62 C63 1.397(6) . ? C62 H62 0.9300 . ? C63 C64 1.388(5) . ? C63 H63 0.9300 . ? C64 C65 1.391(5) . ? C64 H64 0.9300 . ? C65 N2 1.344(5) . ? C65 S2 1.763(4) . ? N1 Sn1 2.413(3) . ? N2 Sn2 2.391(3) . ? S1 Sn1 2.4505(8) . ? S2 Sn2 2.4544(9) . ? Cl1 Sn1 2.4443(8) . ? Cl2 Sn2 2.4467(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.7(3) . . ? C2 C1 Sn1 122.8(2) . . ? C6 C1 Sn1 118.5(2) . . ? C1 C2 C3 122.1(3) . . ? C1 C2 H2 118.9 . . ? C3 C2 H2 118.9 . . ? C2 C3 C4 116.9(3) . . ? C2 C3 C11 120.7(3) . . ? C4 C3 C11 122.4(3) . . ? O1 C4 C5 116.6(3) . . ? O1 C4 C3 120.4(3) . . ? C5 C4 C3 123.0(3) . . ? C6 C5 C4 116.8(3) . . ? C6 C5 C7 120.6(3) . . ? C4 C5 C7 122.5(3) . . ? C1 C6 C5 122.5(3) . . ? C1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C10 C7 C8 107.3(4) . . ? C10 C7 C5 111.3(3) . . ? C8 C7 C5 108.8(4) . . ? C10 C7 C9 107.7(4) . . ? C8 C7 C9 111.1(4) . . ? C5 C7 C9 110.7(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C3 111.9(3) . . ? C12 C11 C13 106.3(3) . . ? C3 C11 C13 110.4(3) . . ? C12 C11 C14 106.1(3) . . ? C3 C11 C14 110.9(3) . . ? C13 C11 C14 111.0(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C19 C15 C16 119.5(3) . . ? C19 C15 Sn1 118.8(2) . . ? C16 C15 Sn1 120.9(2) . . ? C17 C16 C15 121.5(3) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 117.6(3) . . ? C16 C17 C25 120.3(3) . . ? C18 C17 C25 121.9(3) . . ? O2 C18 C17 115.8(3) . . ? O2 C18 C20 122.2(3) . . ? C17 C18 C20 122.0(3) . . ? C15 C19 C20 121.8(3) . . ? C15 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C18 117.5(3) . . ? C19 C20 C21 120.4(3) . . ? C18 C20 C21 122.0(3) . . ? C24 C21 C23 106.8(4) . . ? C24 C21 C22 111.5(4) . . ? C23 C21 C22 106.6(4) . . ? C24 C21 C20 110.8(3) . . ? C23 C21 C20 110.3(3) . . ? C22 C21 C20 110.7(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C27 107.3(3) . . ? C28 C25 C17 111.7(3) . . ? C27 C25 C17 109.5(3) . . ? C28 C25 C26 106.8(3) . . ? C27 C25 C26 110.0(3) . . ? C17 C25 C26 111.6(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N1 C29 C33 121.6(3) . . ? N1 C29 S1 113.2(3) . . ? C33 C29 S1 125.2(3) . . ? N1 C30 C31 121.8(4) . . ? N1 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C30 C31 C32 118.6(4) . . ? C30 C31 H31 120.7 . . ? C32 C31 H31 120.7 . . ? C33 C32 C31 119.4(3) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C29 C33 C32 119.0(4) . . ? C29 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C35 C34 C38 118.9(3) . . ? C35 C34 Sn2 117.7(2) . . ? C38 C34 Sn2 123.4(3) . . ? C34 C35 C36 122.7(3) . . ? C34 C35 H35 118.6 . . ? C36 C35 H35 118.6 . . ? C35 C36 C37 116.4(3) . . ? C35 C36 C66 120.7(3) . . ? C37 C36 C66 122.9(3) . . ? O3 C37 C36 121.2(3) . . ? O3 C37 C39 116.1(3) . . ? C36 C37 C39 122.8(3) . . ? C39 C38 C34 121.7(3) . . ? C39 C38 H38 119.2 . . ? C34 C38 H38 119.2 . . ? C38 C39 C37 117.5(3) . . ? C38 C39 C40 120.9(3) . . ? C37 C39 C40 121.6(3) . . ? C42 C40 C41 108.1(3) . . ? C42 C40 C43 107.9(3) . . ? C41 C40 C43 110.1(3) . . ? C42 C40 C39 111.4(3) . . ? C41 C40 C39 109.5(3) . . ? C43 C40 C39 109.8(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C66 C44 H44A 109.5 . . ? C66 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C66 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C66 C45 H45A 109.5 . . ? C66 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C66 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C66 C46 H46A 109.5 . . ? C66 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C66 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C50 C47 C48 119.1(3) . . ? C50 C47 Sn2 121.3(2) . . ? C48 C47 Sn2 119.6(3) . . ? C47 C48 C49 122.4(3) . . ? C47 C48 H48 118.8 . . ? C49 C48 H48 118.8 . . ? C48 C49 C51 116.4(3) . . ? C48 C49 C57 120.6(3) . . ? C51 C49 C57 123.0(3) . . ? C47 C50 C52 121.9(3) . . ? C47 C50 H50 119.1 . . ? C52 C50 H50 119.1 . . ? O4 C51 C52 120.9(3) . . ? O4 C51 C49 115.9(3) . . ? C52 C51 C49 123.2(3) . . ? C50 C52 C51 116.9(3) . . ? C50 C52 C53 119.9(3) . . ? C51 C52 C53 123.2(3) . . ? C56 C53 C54 107.0(3) . . ? C56 C53 C55 105.9(3) . . ? C54 C53 C55 111.5(3) . . ? C56 C53 C52 111.3(3) . . ? C54 C53 C52 111.3(3) . . ? C55 C53 C52 109.7(3) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C60 C57 C58 106.7(3) . . ? C60 C57 C59 109.9(3) . . ? C58 C57 C59 107.3(3) . . ? C60 C57 C49 111.4(3) . . ? C58 C57 C49 111.1(3) . . ? C59 C57 C49 110.3(3) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N2 C61 C62 122.0(3) . . ? N2 C61 H61 119.0 . . ? C62 C61 H61 119.0 . . ? C61 C62 C63 119.2(3) . . ? C61 C62 H62 120.4 . . ? C63 C62 H62 120.4 . . ? C64 C63 C62 119.2(3) . . ? C64 C63 H63 120.4 . . ? C62 C63 H63 120.4 . . ? C63 C64 C65 118.3(3) . . ? C63 C64 H64 120.9 . . ? C65 C64 H64 120.9 . . ? N2 C65 C64 122.2(3) . . ? N2 C65 S2 112.5(3) . . ? C64 C65 S2 125.3(3) . . ? C36 C66 C45 111.0(3) . . ? C36 C66 C46 110.2(3) . . ? C45 C66 C46 106.8(3) . . ? C36 C66 C44 111.3(3) . . ? C45 C66 C44 105.9(3) . . ? C46 C66 C44 111.3(3) . . ? C30 N1 C29 119.7(3) . . ? C30 N1 Sn1 143.5(2) . . ? C29 N1 Sn1 96.7(2) . . ? C65 N2 C61 119.1(3) . . ? C65 N2 Sn2 97.5(2) . . ? C61 N2 Sn2 143.0(2) . . ? C29 S1 Sn1 85.39(12) . . ? C65 S2 Sn2 84.89(12) . . ? C15 Sn1 C1 119.67(12) . . ? C15 Sn1 N1 94.46(11) . . ? C1 Sn1 N1 92.01(11) . . ? C15 Sn1 Cl1 98.88(9) . . ? C1 Sn1 Cl1 97.31(9) . . ? N1 Sn1 Cl1 157.16(7) . . ? C15 Sn1 S1 119.53(9) . . ? C1 Sn1 S1 117.23(9) . . ? N1 Sn1 S1 64.61(7) . . ? Cl1 Sn1 S1 92.63(3) . . ? C34 Sn2 C47 120.23(12) . . ? C34 Sn2 N2 94.31(12) . . ? C47 Sn2 N2 92.47(11) . . ? C34 Sn2 Cl2 96.69(10) . . ? C47 Sn2 Cl2 97.89(9) . . ? N2 Sn2 Cl2 158.44(8) . . ? C34 Sn2 S2 123.24(10) . . ? C47 Sn2 S2 113.14(9) . . ? N2 Sn2 S2 64.68(7) . . ? Cl2 Sn2 S2 93.81(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.991 _refine_diff_density_min -1.790 _refine_diff_density_rms 0.140 data_shelxl5 _database_code_depnum_ccdc_archive 'CCDC 891293' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H46 Cl N O2 S2 Sn' _chemical_formula_sum 'C35 H46 Cl N O2 S2 Sn' _chemical_formula_weight 730.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn 0.0259 5.4591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0191(4) _cell_length_b 10.1141(3) _cell_length_c 27.4822(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.059(3) _cell_angle_gamma 90.00 _cell_volume 3538.90(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100.7(3) _cell_measurement_reflns_used 6006 _cell_measurement_theta_min 3.2861 _cell_measurement_theta_max 67.2470 _exptl_crystal_description rectangle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 7.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.55788 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4223 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12677 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 66.97 _reflns_number_total 6302 _reflns_number_gt 5556 _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^)+(0.0630P)^2^+0.1753P] 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 6302 _refine_ls_number_parameters 379 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.072 _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 C1 C 0.6972(3) 0.4043(4) 0.17369(12) 0.0272(7) Uani 1 1 d . . . C2 C 0.6538(3) 0.6154(4) 0.18510(12) 0.0259(7) Uani 1 1 d . . . C3 C 0.7603(3) 0.6326(4) 0.18328(12) 0.0256(7) Uani 1 1 d . . . C4 C 0.8065(3) 0.7569(4) 0.18735(13) 0.0306(8) Uani 1 1 d . . . H4 H 0.8765 0.7675 0.1853 0.037 Uiso 1 1 calc R . . C5 C 0.7459(3) 0.8641(4) 0.19445(12) 0.0319(8) Uani 1 1 d . . . H5 H 0.7757 0.9481 0.1977 0.038 Uiso 1 1 calc R . . C6 C 0.6405(3) 0.8488(4) 0.19684(13) 0.0311(8) Uani 1 1 d . . . H6 H 0.6012 0.9226 0.2017 0.037 Uiso 1 1 calc R . . C7 C 0.5939(3) 0.7254(4) 0.19211(14) 0.0326(8) Uani 1 1 d . . . H7 H 0.5236 0.7159 0.1936 0.039 Uiso 1 1 calc R . . C8 C 0.4552(2) 0.3286(3) 0.23782(11) 0.0220(7) Uani 1 1 d . . . C9 C 0.4078(3) 0.2247(4) 0.25751(12) 0.0241(7) Uani 1 1 d . . . H9 H 0.3948 0.1464 0.2395 0.029 Uiso 1 1 calc R . . C10 C 0.3788(3) 0.2337(4) 0.30367(12) 0.0247(7) Uani 1 1 d . . . C11 C 0.4006(3) 0.3534(4) 0.32947(11) 0.0247(7) Uani 1 1 d . . . C12 C 0.4494(3) 0.4617(4) 0.31129(12) 0.0254(7) Uani 1 1 d . . . C13 C 0.4752(2) 0.4455(3) 0.26456(12) 0.0241(7) Uani 1 1 d . . . H13 H 0.5067 0.5152 0.2511 0.029 Uiso 1 1 calc R . . C14 C 0.4691(3) 0.5926(4) 0.33991(12) 0.0274(7) Uani 1 1 d . . . C15 C 0.3644(3) 0.6544(4) 0.34548(13) 0.0308(8) Uani 1 1 d . . . H15A H 0.3778 0.7362 0.3634 0.046 Uiso 1 1 calc R . . H15B H 0.3284 0.5948 0.3634 0.046 Uiso 1 1 calc R . . H15C H 0.3217 0.6710 0.3131 0.046 Uiso 1 1 calc R . . C16 C 0.5425(3) 0.5719(4) 0.39151(13) 0.0364(9) Uani 1 1 d . . . H16A H 0.5534 0.6549 0.4088 0.055 Uiso 1 1 calc R . . H16B H 0.6087 0.5376 0.3872 0.055 Uiso 1 1 calc R . . H16C H 0.5108 0.5104 0.4106 0.055 Uiso 1 1 calc R . . C17 C 0.5239(3) 0.6943(4) 0.31296(15) 0.0329(8) Uani 1 1 d . . . H17A H 0.5343 0.7746 0.3320 0.049 Uiso 1 1 calc R . . H17B H 0.4811 0.7120 0.2807 0.049 Uiso 1 1 calc R . . H17C H 0.5907 0.6602 0.3093 0.049 Uiso 1 1 calc R . . C18 C 0.3193(3) 0.1191(4) 0.32226(12) 0.0281(7) Uani 1 1 d . . . C19 C 0.3104(3) -0.0013(4) 0.28799(13) 0.0308(8) Uani 1 1 d . . . H19A H 0.2732 -0.0705 0.3009 0.046 Uiso 1 1 calc R . . H19B H 0.3794 -0.0316 0.2863 0.046 Uiso 1 1 calc R . . H19C H 0.2730 0.0228 0.2553 0.046 Uiso 1 1 calc R . . C20 C 0.2070(3) 0.1657(4) 0.32285(14) 0.0358(8) Uani 1 1 d . . . H20A H 0.1688 0.0951 0.3343 0.054 Uiso 1 1 calc R . . H20B H 0.1722 0.1909 0.2898 0.054 Uiso 1 1 calc R . . H20C H 0.2099 0.2402 0.3448 0.054 Uiso 1 1 calc R . . C21 C 0.3750(3) 0.0696(4) 0.37451(13) 0.0386(9) Uani 1 1 d . . . H21A H 0.3356 -0.0020 0.3845 0.058 Uiso 1 1 calc R . . H21B H 0.3795 0.1406 0.3981 0.058 Uiso 1 1 calc R . . H21C H 0.4444 0.0395 0.3734 0.058 Uiso 1 1 calc R . . C22 C 0.4028(3) 0.3911(4) 0.09996(12) 0.0299(8) Uani 1 1 d . . . C23 C 0.4228(3) 0.5191(4) 0.08524(13) 0.0340(8) Uani 1 1 d . . . H23 H 0.4765 0.5680 0.1047 0.041 Uiso 1 1 calc R . . C24 C 0.3636(4) 0.5752(4) 0.04174(14) 0.0434(10) Uani 1 1 d . . . C25 C 0.2840(4) 0.4987(5) 0.01336(14) 0.0523(12) Uani 1 1 d . . . C26 C 0.2616(4) 0.3674(5) 0.02612(13) 0.0424(10) Uani 1 1 d . . . C27 C 0.3226(3) 0.3180(4) 0.07037(13) 0.0353(9) Uani 1 1 d . . . H27 H 0.3091 0.2331 0.0804 0.042 Uiso 1 1 calc R . . C28 C 0.1741(4) 0.2840(5) -0.00541(15) 0.0508(12) Uani 1 1 d . . . C29 C 0.1705(4) 0.1443(5) 0.01492(15) 0.0517(11) Uani 1 1 d . . . H29A H 0.2363 0.1009 0.0155 0.078 Uiso 1 1 calc R . . H29B H 0.1149 0.0957 -0.0060 0.078 Uiso 1 1 calc R . . H29C H 0.1579 0.1484 0.0481 0.078 Uiso 1 1 calc R . . C30 C 0.0654(5) 0.3451(7) -0.0058(2) 0.081(2) Uani 1 1 d . . . H30A H 0.0633 0.4338 -0.0185 0.122 Uiso 1 1 calc R . . H30B H 0.0532 0.3465 0.0275 0.122 Uiso 1 1 calc R . . H30C H 0.0120 0.2931 -0.0266 0.122 Uiso 1 1 calc R . . C31 C 0.1907(6) 0.2685(6) -0.05910(17) 0.0755(19) Uani 1 1 d . . . H31A H 0.2584 0.2299 -0.0584 0.113 Uiso 1 1 calc R . . H31B H 0.1871 0.3537 -0.0748 0.113 Uiso 1 1 calc R . . H31C H 0.1371 0.2121 -0.0775 0.113 Uiso 1 1 calc R . . C32 C 0.3899(4) 0.7167(5) 0.02631(16) 0.0494(11) Uani 1 1 d U . . C33 C 0.2942(5) 0.8093(5) 0.0234(2) 0.0655(15) Uani 1 1 d U . . H33A H 0.2351 0.7737 0.0003 0.098 Uiso 1 1 calc R . . H33B H 0.3108 0.8953 0.0124 0.098 Uiso 1 1 calc R . . H33C H 0.2775 0.8164 0.0557 0.098 Uiso 1 1 calc R . . C34 C 0.4251(6) 0.7128(6) -0.0237(2) 0.0750(17) Uani 1 1 d U . . H34A H 0.3710 0.6729 -0.0484 0.113 Uiso 1 1 calc R . . H34B H 0.4884 0.6618 -0.0201 0.113 Uiso 1 1 calc R . . H34C H 0.4378 0.8012 -0.0337 0.113 Uiso 1 1 calc R . . C35 C 0.4799(5) 0.7798(5) 0.0633(2) 0.0601(13) Uani 1 1 d U . . H35A H 0.5415 0.7255 0.0666 0.090 Uiso 1 1 calc R . . H35B H 0.4608 0.7879 0.0951 0.090 Uiso 1 1 calc R . . H35C H 0.4943 0.8659 0.0516 0.090 Uiso 1 1 calc R . . N1 N 0.6204(2) 0.4842(3) 0.17923(11) 0.0293(6) Uani 1 1 d . . . O1 O 0.3729(2) 0.3685(3) 0.37505(9) 0.0346(6) Uani 1 1 d . . . O2 O 0.2205(4) 0.5484(4) -0.02942(12) 0.0825(13) Uani 1 1 d . . . S1 S 0.67169(7) 0.23737(9) 0.16484(3) 0.02995(19) Uani 1 1 d . . . S2 S 0.81657(6) 0.48058(9) 0.17456(3) 0.02829(19) Uani 1 1 d . . . Sn1 Sn 0.488698(17) 0.30308(2) 0.165935(8) 0.02445(9) Uani 1 1 d . . . Cl1 Cl 0.42843(7) 0.07742(9) 0.14989(3) 0.03107(19) 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 C1 0.0303(18) 0.0289(18) 0.0239(15) 0.0041(14) 0.0090(14) 0.0031(15) C2 0.0291(18) 0.0274(18) 0.0222(15) 0.0023(14) 0.0074(13) -0.0012(14) C3 0.0251(17) 0.0301(18) 0.0213(14) 0.0014(14) 0.0044(12) 0.0003(14) C4 0.0259(18) 0.036(2) 0.0285(17) 0.0008(16) 0.0024(14) -0.0040(16) C5 0.0343(19) 0.033(2) 0.0252(16) -0.0029(15) -0.0010(14) -0.0059(16) C6 0.0344(19) 0.0302(19) 0.0284(17) 0.0005(16) 0.0061(15) 0.0070(16) C7 0.0291(19) 0.039(2) 0.0321(18) 0.0010(16) 0.0116(15) 0.0018(16) C8 0.0174(15) 0.0297(17) 0.0195(14) 0.0009(13) 0.0052(12) 0.0044(13) C9 0.0209(16) 0.0277(17) 0.0218(15) 0.0006(14) 0.0001(12) 0.0016(14) C10 0.0185(16) 0.0304(18) 0.0241(15) 0.0037(15) 0.0019(12) 0.0016(14) C11 0.0242(16) 0.0286(18) 0.0202(15) 0.0016(14) 0.0020(12) 0.0004(14) C12 0.0220(16) 0.0278(18) 0.0250(15) 0.0022(14) 0.0017(13) 0.0002(14) C13 0.0217(16) 0.0246(17) 0.0258(15) 0.0031(14) 0.0045(13) -0.0008(13) C14 0.0239(17) 0.0301(18) 0.0271(16) -0.0029(15) 0.0031(14) -0.0039(15) C15 0.0315(19) 0.0326(19) 0.0288(17) -0.0074(15) 0.0077(14) 0.0003(16) C16 0.036(2) 0.038(2) 0.0310(18) -0.0055(17) -0.0042(15) -0.0024(17) C17 0.033(2) 0.030(2) 0.038(2) -0.0032(16) 0.0099(16) -0.0037(15) C18 0.0309(18) 0.0297(18) 0.0226(15) 0.0031(14) 0.0032(14) -0.0029(15) C19 0.0321(18) 0.0265(18) 0.0329(17) 0.0046(15) 0.0047(15) -0.0050(15) C20 0.032(2) 0.044(2) 0.0322(18) 0.0030(17) 0.0093(15) -0.0055(18) C21 0.049(2) 0.036(2) 0.0281(17) 0.0119(17) 0.0008(16) -0.0033(18) C22 0.038(2) 0.0353(19) 0.0187(14) -0.0009(14) 0.0106(14) 0.0077(16) C23 0.049(2) 0.0326(19) 0.0235(16) -0.0007(15) 0.0137(16) 0.0082(17) C24 0.078(3) 0.031(2) 0.0234(17) 0.0006(16) 0.0169(19) 0.014(2) C25 0.086(3) 0.044(2) 0.0223(17) 0.0024(18) 0.000(2) 0.019(3) C26 0.060(3) 0.044(2) 0.0203(17) -0.0023(17) 0.0014(17) 0.010(2) C27 0.047(2) 0.035(2) 0.0240(17) -0.0002(16) 0.0096(16) 0.0098(18) C28 0.066(3) 0.056(3) 0.0239(19) -0.0036(19) -0.0052(19) 0.007(2) C29 0.057(3) 0.060(3) 0.032(2) -0.001(2) -0.0025(19) 0.001(2) C30 0.078(4) 0.092(5) 0.056(3) -0.015(3) -0.026(3) 0.034(4) C31 0.135(6) 0.061(3) 0.026(2) -0.008(2) 0.006(3) -0.018(4) C32 0.078(3) 0.040(2) 0.0349(19) 0.0052(18) 0.022(2) 0.011(2) C33 0.093(3) 0.046(3) 0.056(3) 0.009(2) 0.014(3) 0.016(2) C34 0.120(4) 0.060(3) 0.055(3) 0.011(2) 0.041(3) 0.010(3) C35 0.082(3) 0.044(2) 0.056(2) 0.010(2) 0.020(2) -0.004(2) N1 0.0257(15) 0.0313(16) 0.0342(15) -0.0001(13) 0.0137(12) 0.0006(13) O1 0.0450(15) 0.0388(15) 0.0222(11) -0.0009(11) 0.0125(11) -0.0012(12) O2 0.140(4) 0.054(2) 0.0339(16) 0.0108(16) -0.026(2) 0.014(2) S1 0.0269(4) 0.0283(4) 0.0369(4) -0.0005(4) 0.0119(3) 0.0032(4) S2 0.0240(4) 0.0304(4) 0.0309(4) 0.0016(4) 0.0069(3) 0.0016(3) Sn1 0.02490(14) 0.02557(14) 0.02398(13) 0.00056(8) 0.00763(9) 0.00231(9) Cl1 0.0324(4) 0.0280(4) 0.0322(4) -0.0033(3) 0.0054(3) 0.0009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.319(5) . ? C1 S1 1.728(4) . ? C1 S2 1.731(4) . ? C2 N1 1.395(5) . ? C2 C7 1.395(5) . ? C2 C3 1.408(5) . ? C3 C4 1.388(5) . ? C3 S2 1.741(4) . ? C4 C5 1.379(6) . ? C4 H4 0.9300 . ? C5 C6 1.396(5) . ? C5 H5 0.9300 . ? C6 C7 1.382(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.385(5) . ? C8 C13 1.388(5) . ? C8 Sn1 2.126(3) . ? C9 C10 1.400(5) . ? C9 H9 0.9300 . ? C10 C11 1.402(5) . ? C10 C18 1.539(5) . ? C11 O1 1.382(4) . ? C11 C12 1.409(5) . ? C12 C13 1.403(5) . ? C12 C14 1.534(5) . ? C13 H13 0.9300 . ? C14 C17 1.529(5) . ? C14 C15 1.536(5) . ? C14 C16 1.550(5) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.529(5) . ? C18 C20 1.539(5) . ? C18 C21 1.550(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C27 1.393(6) . ? C22 C23 1.397(5) . ? C22 Sn1 2.117(3) . ? C23 C24 1.400(5) . ? C23 H23 0.9300 . ? C24 C25 1.395(7) . ? C24 C32 1.551(6) . ? C25 O2 1.382(5) . ? C25 C26 1.419(7) . ? C26 C27 1.398(5) . ? C26 C28 1.532(6) . ? C27 H27 0.9300 . ? C28 C29 1.524(7) . ? C28 C30 1.543(7) . ? C28 C31 1.543(6) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C35 1.523(7) . ? C32 C34 1.537(6) . ? C32 C33 1.547(7) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? N1 Sn1 2.483(3) . ? S1 Sn1 2.4796(9) . ? Sn1 Cl1 2.4237(9) . ? 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 C1 S1 119.1(3) . . ? N1 C1 S2 115.2(3) . . ? S1 C1 S2 125.7(2) . . ? N1 C2 C7 127.2(3) . . ? N1 C2 C3 113.5(3) . . ? C7 C2 C3 119.3(3) . . ? C4 C3 C2 121.5(3) . . ? C4 C3 S2 128.5(3) . . ? C2 C3 S2 110.0(3) . . ? C5 C4 C3 118.2(3) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 120.8(4) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C2 119.1(3) . . ? C6 C7 H7 120.5 . . ? C2 C7 H7 120.5 . . ? C9 C8 C13 119.3(3) . . ? C9 C8 Sn1 117.8(2) . . ? C13 C8 Sn1 122.9(2) . . ? C8 C9 C10 122.1(3) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C9 C10 C11 116.7(3) . . ? C9 C10 C18 120.1(3) . . ? C11 C10 C18 123.0(3) . . ? O1 C11 C10 119.3(3) . . ? O1 C11 C12 117.2(3) . . ? C10 C11 C12 123.4(3) . . ? C13 C12 C11 116.5(3) . . ? C13 C12 C14 121.6(3) . . ? C11 C12 C14 121.9(3) . . ? C8 C13 C12 121.9(3) . . ? C8 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C17 C14 C12 112.2(3) . . ? C17 C14 C15 106.7(3) . . ? C12 C14 C15 110.2(3) . . ? C17 C14 C16 105.8(3) . . ? C12 C14 C16 111.0(3) . . ? C15 C14 C16 110.7(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 107.5(3) . . ? C19 C18 C10 111.9(3) . . ? C20 C18 C10 108.5(3) . . ? C19 C18 C21 105.9(3) . . ? C20 C18 C21 110.6(3) . . ? C10 C18 C21 112.3(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 119.0(3) . . ? C27 C22 Sn1 118.3(3) . . ? C23 C22 Sn1 122.7(3) . . ? C22 C23 C24 121.3(4) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C23 117.7(4) . . ? C25 C24 C32 122.7(4) . . ? C23 C24 C32 119.6(4) . . ? O2 C25 C24 121.1(4) . . ? O2 C25 C26 115.7(4) . . ? C24 C25 C26 123.2(4) . . ? C27 C26 C25 116.2(4) . . ? C27 C26 C28 121.0(4) . . ? C25 C26 C28 122.8(4) . . ? C22 C27 C26 122.5(4) . . ? C22 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? C29 C28 C26 112.3(4) . . ? C29 C28 C30 106.0(5) . . ? C26 C28 C30 110.9(4) . . ? C29 C28 C31 106.1(4) . . ? C26 C28 C31 111.1(4) . . ? C30 C28 C31 110.2(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C35 C32 C34 106.0(5) . . ? C35 C32 C33 106.2(4) . . ? C34 C32 C33 110.9(4) . . ? C35 C32 C24 112.8(4) . . ? C34 C32 C24 110.2(4) . . ? C33 C32 C24 110.6(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C1 N1 C2 111.7(3) . . ? C1 N1 Sn1 92.7(2) . . ? C2 N1 Sn1 155.2(2) . . ? C1 S1 Sn1 83.87(12) . . ? C1 S2 C3 89.60(17) . . ? C22 Sn1 C8 124.78(12) . . ? C22 Sn1 Cl1 98.45(11) . . ? C8 Sn1 Cl1 99.31(10) . . ? C22 Sn1 S1 116.06(9) . . ? C8 Sn1 S1 115.35(9) . . ? Cl1 Sn1 S1 91.19(3) . . ? C22 Sn1 N1 92.35(13) . . ? C8 Sn1 N1 92.47(11) . . ? Cl1 Sn1 N1 155.34(7) . . ? S1 Sn1 N1 64.16(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.168 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.091