# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Subrato Bhattacharya' _publ_contact_author_email BHATT99@YAHOO.COM _publ_section_title ; Novel synthesis of a one-dimensional coordination polymer containing pendent hydrosulfide groups ; loop_ _publ_author_name 'Subrato Bhattacharya' 'Jyotsna Chaturvedi' 'Munirathinam Nethaji' # Attachment 'mn30a_m2.cif' data_mn30a_m _database_code_depnum_ccdc_archive 'CCDC 725580' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'dimethyl(hydrosulfido)tin thioacetate' _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 O2 S Sn' _chemical_formula_sum 'C4 H10 O2 S Sn' _chemical_formula_weight 240.87 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' 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 ORTHORHOMBIC _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 9.310(3) _cell_length_b 7.671(3) _cell_length_c 11.045(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 788.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 456 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.50 _exptl_crystal_description RECTANGULAR _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 3.428 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.4897 _exptl_absorpt_correction_T_max 0.5806 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD' _diffrn_measurement_method OMEGA _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6144 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1019 _reflns_number_gt 882 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER SMART APEX CCD' _computing_cell_refinement 'BRUKER SMART APEX CCD' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-III _computing_publication_material 'WINGX V1.80.01' _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^ > 2\s(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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+2.0519P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1019 _refine_ls_number_parameters 57 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.004 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 -0.0394(5) 0.5073(5) 0.2657(4) 0.0525(10) Uani 1 1 d . . . H1A H 0.0215 0.5073 0.1956 0.079 Uiso 1 1 calc R . . H1B H 0.0057 0.5726 0.3294 0.079 Uiso 1 1 calc R . . H1C H -0.1300 0.5599 0.2458 0.079 Uiso 1 1 calc R . . C2 C 0.2075(5) 0.2500 0.4233(4) 0.0402(11) Uani 1 2 d S . . C3 C 0.3314(6) 0.2500 0.5079(5) 0.0586(16) Uani 1 2 d SD . . H3A H 0.292(6) 0.2500 0.593(4) 0.09(2) Uiso 1 2 d SD . . H3B H 0.400(4) 0.146(6) 0.502(5) 0.15(2) Uiso 1 1 d D . . O1 O 0.2250(4) 0.2500 0.3105(3) 0.0498(9) Uani 1 2 d S . . O2 O 0.0817(3) 0.2500 0.4685(3) 0.0449(9) Uani 1 2 d S . . H1 H -0.235(10) 0.2500 0.578(3) 0.42(10) Uiso 1 2 d SD . . S1 S -0.25373(14) 0.2500 0.47493(12) 0.0513(3) Uani 1 2 d SD . . Sn1 Sn -0.07312(3) 0.2500 0.32344(3) 0.03307(9) Uani 1 2 d SD . . 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 0.063(2) 0.0388(18) 0.055(2) -0.0004(18) 0.0014(19) -0.0046(18) C2 0.036(2) 0.042(2) 0.043(3) 0.000 -0.005(2) 0.000 C3 0.040(3) 0.088(4) 0.047(3) 0.000 -0.009(2) 0.000 O1 0.0373(18) 0.075(3) 0.0368(18) 0.000 0.0026(15) 0.000 O2 0.0329(18) 0.067(2) 0.0352(17) 0.000 -0.0003(14) 0.000 S1 0.0368(6) 0.0762(9) 0.0408(6) 0.000 0.0139(5) 0.000 Sn1 0.03029(16) 0.03773(16) 0.03118(16) 0.000 0.00328(12) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Sn1 2.098(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.257(6) . ? C2 O2 1.273(6) . ? C2 C3 1.483(7) . ? C3 H3A 1.01(4) . ? C3 H3B 1.03(3) . ? O1 Sn1 2.392(3) 6_656 ? O2 Sn1 2.155(3) . ? S1 Sn1 2.3721(14) . ? S1 H1 1.15(4) . ? Sn1 C1 2.098(4) 7_565 ? Sn1 O1 2.392(3) 6_556 ? 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 Sn1 C1 H1A 109.5 . . ? Sn1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sn1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 O2 120.5(4) . . ? O1 C2 C3 121.6(5) . . ? O2 C2 C3 117.9(4) . . ? C2 C3 H3A 108(3) . . ? C2 C3 H3B 116(3) . . ? H3A C3 H3B 107(3) . . ? C2 O1 Sn1 135.7(3) . 6_656 ? C2 O2 Sn1 108.9(3) . . ? Sn1 S1 H1 126(4) . . ? C1 Sn1 C1 140.4(2) 7_565 . ? C1 Sn1 O2 97.22(12) 7_565 . ? C1 Sn1 O2 97.22(12) . . ? C1 Sn1 S1 108.68(12) 7_565 . ? C1 Sn1 S1 108.68(12) . . ? O2 Sn1 S1 87.13(9) . . ? C1 Sn1 O1 85.96(12) 7_565 6_556 ? C1 Sn1 O1 85.96(12) . 6_556 ? O2 Sn1 O1 170.20(12) . 6_556 ? S1 Sn1 O1 83.08(9) . 6_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C2 O1 Sn1 180.0 . . . 6_656 ? C3 C2 O1 Sn1 0.0 . . . 6_656 ? O1 C2 O2 Sn1 0.0 . . . . ? C3 C2 O2 Sn1 180.0 . . . . ? C2 O2 Sn1 C1 71.53(12) . . . 7_565 ? C2 O2 Sn1 C1 -71.53(12) . . . . ? C2 O2 Sn1 S1 180.0 . . . . ? C2 O2 Sn1 O1 180.0 . . . 6_556 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.661 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.111 # Attachment 'ebhu127m1.cif' data_ebhu127m _database_code_depnum_ccdc_archive 'CCDC 725581' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'dimethyltin bis-thiobenzoate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 O2 S2 Sn' _chemical_formula_weight 423.11 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.546(3) _cell_length_b 14.516(4) _cell_length_c 12.049(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.702(4) _cell_angle_gamma 90.00 _cell_volume 1757.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6647 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 26.14 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1458 _exptl_absorpt_coefficient_mu 1.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.622 _exptl_absorpt_correction_T_max 0.689 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8835 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.03 _reflns_number_total 3300 _reflns_number_gt 3135 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0312P)^2^+1.1758P] 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 3300 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.300 _refine_ls_restrained_S_all 1.300 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 0.2597(5) -0.0760(3) 0.0970(4) 0.0648(12) Uani 1 1 d . . . H1A H 0.3050 -0.1223 0.1516 0.097 Uiso 1 1 calc R . . H1B H 0.3156 -0.0564 0.0517 0.097 Uiso 1 1 calc R . . H1C H 0.1784 -0.1011 0.0463 0.097 Uiso 1 1 calc R . . Sn Sn 0.21580(3) 0.03791(2) 0.18808(2) 0.04779(12) Uani 1 1 d . . . S1 S 0.10952(11) -0.01728(9) 0.33442(9) 0.0584(3) Uani 1 1 d . . . S2 S 0.42438(11) 0.07533(10) 0.34609(9) 0.0607(3) Uani 1 1 d . . . O1 O -0.0346(3) -0.0333(2) 0.1190(3) 0.0650(9) Uani 1 1 d . . . C3 C -0.0350(4) -0.0431(3) 0.2203(3) 0.0486(9) Uani 1 1 d . . . O2 O 0.4180(3) 0.1142(2) 0.1347(2) 0.0628(8) Uani 1 1 d . . . C11 C 0.6275(4) 0.1492(3) 0.2691(3) 0.0477(9) Uani 1 1 d . . . C16 C 0.7131(4) 0.1465(3) 0.3823(4) 0.0532(10) Uani 1 1 d . . . H16 H 0.6829 0.1240 0.4420 0.064 Uiso 1 1 calc R . . C5 C -0.1628(4) -0.0762(3) 0.3605(4) 0.0534(10) Uani 1 1 d . . . H5 H -0.0931 -0.0528 0.4212 0.064 Uiso 1 1 calc R . . C4 C -0.1526(4) -0.0783(3) 0.2489(3) 0.0479(9) Uani 1 1 d . . . C10 C 0.4886(4) 0.1152(3) 0.2367(3) 0.0492(9) Uani 1 1 d . . . C6 C -0.2760(5) -0.1086(3) 0.3825(4) 0.0649(12) Uani 1 1 d . . . H6 H -0.2820 -0.1070 0.4579 0.078 Uiso 1 1 calc R . . C15 C 0.8418(4) 0.1768(3) 0.4068(4) 0.0598(11) Uani 1 1 d . . . H15 H 0.8987 0.1741 0.4828 0.072 Uiso 1 1 calc R . . C2 C 0.1179(4) 0.1625(3) 0.1232(4) 0.0598(11) Uani 1 1 d . . . H2A H 0.1133 0.2005 0.1870 0.090 Uiso 1 1 calc R . . H2B H 0.0295 0.1494 0.0738 0.090 Uiso 1 1 calc R . . H2C H 0.1665 0.1943 0.0791 0.090 Uiso 1 1 calc R . . C14 C 0.8868(5) 0.2109(3) 0.3198(5) 0.0686(13) Uani 1 1 d . . . H14 H 0.9740 0.2319 0.3370 0.082 Uiso 1 1 calc R . . C9 C -0.2588(4) -0.1135(4) 0.1597(4) 0.0679(13) Uani 1 1 d . . . H9 H -0.2545 -0.1145 0.0838 0.081 Uiso 1 1 calc R . . C8 C -0.3698(5) -0.1466(4) 0.1832(5) 0.0781(15) Uani 1 1 d . . . H8 H -0.4390 -0.1719 0.1235 0.094 Uiso 1 1 calc R . . C13 C 0.8043(5) 0.2143(4) 0.2075(4) 0.0769(15) Uani 1 1 d . . . H13 H 0.8353 0.2374 0.1486 0.092 Uiso 1 1 calc R . . C12 C 0.6752(5) 0.1833(4) 0.1822(4) 0.0656(13) Uani 1 1 d . . . H12 H 0.6194 0.1854 0.1058 0.079 Uiso 1 1 calc R . . C7 C -0.3795(5) -0.1429(4) 0.2935(5) 0.0728(14) Uani 1 1 d . . . H7 H -0.4563 -0.1637 0.3082 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.062(3) 0.061(3) 0.072(3) -0.009(2) 0.021(2) 0.004(2) Sn 0.04239(17) 0.0526(2) 0.04883(17) 0.00160(12) 0.01450(12) -0.00112(12) S1 0.0463(6) 0.0810(9) 0.0473(5) 0.0036(5) 0.0131(4) -0.0104(5) S2 0.0471(6) 0.0844(9) 0.0504(5) 0.0025(5) 0.0144(4) -0.0091(6) O1 0.0599(18) 0.085(2) 0.0509(17) 0.0033(15) 0.0182(14) -0.0125(16) C3 0.046(2) 0.049(3) 0.050(2) 0.0015(17) 0.0140(17) 0.0011(17) O2 0.0525(16) 0.084(2) 0.0480(15) 0.0009(14) 0.0089(13) -0.0055(16) C11 0.040(2) 0.051(3) 0.055(2) -0.0003(18) 0.0171(16) 0.0042(17) C16 0.050(2) 0.055(3) 0.054(2) 0.0038(19) 0.0131(17) -0.0022(19) C5 0.048(2) 0.054(3) 0.059(2) -0.007(2) 0.0184(18) -0.003(2) C4 0.045(2) 0.044(2) 0.053(2) 0.0024(18) 0.0142(17) 0.0019(18) C10 0.047(2) 0.053(3) 0.047(2) 0.0001(17) 0.0124(16) 0.0036(19) C6 0.064(3) 0.066(3) 0.075(3) -0.006(2) 0.037(2) -0.003(2) C15 0.044(2) 0.063(3) 0.066(3) -0.005(2) 0.0068(19) -0.001(2) C2 0.052(2) 0.054(3) 0.072(3) 0.001(2) 0.017(2) 0.001(2) C14 0.049(2) 0.071(3) 0.090(3) -0.014(3) 0.028(2) -0.008(2) C9 0.056(3) 0.087(4) 0.056(2) 0.003(2) 0.010(2) -0.011(3) C8 0.047(3) 0.094(4) 0.085(3) -0.006(3) 0.007(2) -0.015(3) C13 0.062(3) 0.108(4) 0.072(3) -0.003(3) 0.037(2) -0.011(3) C12 0.056(3) 0.091(4) 0.051(2) -0.002(2) 0.0178(19) -0.004(3) C7 0.051(3) 0.068(3) 0.106(4) -0.005(3) 0.032(3) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 Sn 2.112(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? Sn C2 2.111(4) . ? Sn S1 2.4918(12) . ? Sn S2 2.4923(12) . ? S1 C3 1.755(4) . ? S2 C10 1.753(4) . ? O1 C3 1.230(5) . ? C3 C4 1.475(6) . ? O2 C10 1.229(4) . ? C11 C12 1.385(6) . ? C11 C16 1.388(5) . ? C11 C10 1.481(5) . ? C16 C15 1.371(6) . ? C16 H16 0.9300 . ? C5 C4 1.381(5) . ? C5 C6 1.382(6) . ? C5 H5 0.9300 . ? C4 C9 1.393(6) . ? C6 C7 1.370(7) . ? C6 H6 0.9300 . ? C15 C14 1.369(6) . ? C15 H15 0.9300 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C14 C13 1.369(7) . ? C14 H14 0.9300 . ? C9 C8 1.373(7) . ? C9 H9 0.9300 . ? C8 C7 1.364(7) . ? C8 H8 0.9300 . ? C13 C12 1.377(6) . ? C13 H13 0.9300 . ? C12 H12 0.9300 . ? C7 H7 0.9300 . ? 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 Sn C1 H1A 109.5 . . ? Sn C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sn C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 Sn C1 129.62(19) . . ? C2 Sn S1 105.26(13) . . ? C1 Sn S1 109.44(14) . . ? C2 Sn S2 108.35(13) . . ? C1 Sn S2 106.60(13) . . ? S1 Sn S2 90.68(4) . . ? C3 S1 Sn 89.13(14) . . ? C10 S2 Sn 87.17(13) . . ? O1 C3 C4 121.9(4) . . ? O1 C3 S1 119.2(3) . . ? C4 C3 S1 118.9(3) . . ? C12 C11 C16 118.4(4) . . ? C12 C11 C10 118.5(4) . . ? C16 C11 C10 123.1(4) . . ? C15 C16 C11 120.6(4) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C4 C9 118.4(4) . . ? C5 C4 C3 122.7(4) . . ? C9 C4 C3 118.9(4) . . ? O2 C10 C11 121.2(4) . . ? O2 C10 S2 119.6(3) . . ? C11 C10 S2 119.3(3) . . ? C7 C6 C5 120.2(4) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C16 C15 C14 120.1(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? Sn C2 H2A 109.5 . . ? Sn C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sn C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C8 C9 C4 120.4(5) . . ? C8 C9 H9 119.8 . . ? C4 C9 H9 119.8 . . ? C7 C8 C9 120.5(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C14 C13 C12 119.7(5) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C12 C11 120.8(4) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C8 C7 C6 119.9(4) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Sn S1 C3 71.05(19) . . . . ? C1 Sn S1 C3 -71.82(19) . . . . ? S2 Sn S1 C3 -179.71(14) . . . . ? C2 Sn S2 C10 -72.3(2) . . . . ? C1 Sn S2 C10 70.8(2) . . . . ? S1 Sn S2 C10 -178.61(15) . . . . ? Sn S1 C3 O1 4.5(3) . . . . ? Sn S1 C3 C4 -177.0(3) . . . . ? C12 C11 C16 C15 -0.2(7) . . . . ? C10 C11 C16 C15 178.3(4) . . . . ? C6 C5 C4 C9 0.2(7) . . . . ? C6 C5 C4 C3 178.9(4) . . . . ? O1 C3 C4 C5 -169.5(4) . . . . ? S1 C3 C4 C5 12.0(6) . . . . ? O1 C3 C4 C9 9.3(7) . . . . ? S1 C3 C4 C9 -169.2(4) . . . . ? C12 C11 C10 O2 2.4(6) . . . . ? C16 C11 C10 O2 -176.1(4) . . . . ? C12 C11 C10 S2 -177.8(3) . . . . ? C16 C11 C10 S2 3.6(6) . . . . ? Sn S2 C10 O2 2.1(4) . . . . ? Sn S2 C10 C11 -177.6(3) . . . . ? C4 C5 C6 C7 -0.2(7) . . . . ? C11 C16 C15 C14 0.7(7) . . . . ? C16 C15 C14 C13 -0.6(8) . . . . ? C5 C4 C9 C8 -1.1(7) . . . . ? C3 C4 C9 C8 -179.9(5) . . . . ? C4 C9 C8 C7 2.1(9) . . . . ? C15 C14 C13 C12 0.1(8) . . . . ? C14 C13 C12 C11 0.3(8) . . . . ? C16 C11 C12 C13 -0.3(7) . . . . ? C10 C11 C12 C13 -178.9(5) . . . . ? C9 C8 C7 C6 -2.1(9) . . . . ? C5 C6 C7 C8 1.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.363 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.078