# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name V.Chandrasekhar P.Singh _publ_contact_author_name 'Vadapalli Chandrasekhar' _publ_contact_author_email VC@IITK.AC.IN data_20marb _database_code_depnum_ccdc_archive 'CCDC 766494' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'organotin sulfonate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H32 N2 O8 S2 Sn' _chemical_formula_weight 707.37 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 'C2/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 25.099(5) _cell_length_b 15.666(5) _cell_length_c 19.433(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 129.327(5) _cell_angle_gamma 90.000(5) _cell_volume 5911(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5826 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.56 _exptl_crystal_description 'block like' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 1.058 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.899 _exptl_absorpt_correction_T_max 0.963 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16015 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5781 _reflns_number_gt 4792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The similar ADP restraint SIMU (66) and the rigid bond restraint "DELU" (14) have been applied to the carbon atoms of the n-butyl chains. ; _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^)+(0.0791P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5781 _refine_ls_number_parameters 394 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.756882(12) 0.307442(15) 0.225337(15) 0.03221(12) Uani 1 1 d . . . S1 S 0.82182(6) 0.17680(6) 0.40826(7) 0.0415(2) Uani 1 1 d . . . S2 S 0.90185(4) 0.42086(6) 0.28577(6) 0.0345(2) Uani 1 1 d . . . O1 O 0.66232(13) 0.22763(16) 0.16033(17) 0.0395(6) Uani 1 1 d . . . O2 O 0.69999(12) 0.34498(16) 0.08425(17) 0.0396(6) Uani 1 1 d . . . O3 O 0.81259(15) 0.25959(16) 0.36531(18) 0.0447(7) Uani 1 1 d . . . O4 O 0.79791(17) 0.10618(17) 0.3471(2) 0.0549(8) Uani 1 1 d . . . O5 O 0.89110(17) 0.1676(2) 0.4899(2) 0.0615(9) Uani 1 1 d . . . O6 O 0.83895(13) 0.40829(17) 0.27624(18) 0.0435(6) Uani 1 1 d . . . O7 O 0.88734(16) 0.46297(18) 0.20990(18) 0.0532(8) Uani 1 1 d . . . O8 O 0.94049(14) 0.34311(17) 0.31172(19) 0.0456(7) Uani 1 1 d . . . N1 N 0.64680(16) 0.17806(18) 0.0937(2) 0.0348(7) Uani 1 1 d . . . N2 N 0.63350(15) 0.36506(19) 0.0349(2) 0.0367(7) Uani 1 1 d . . . C1 C 0.8120(2) 0.2145(2) 0.2127(3) 0.0380(8) Uani 1 1 d U B . H1A H 0.8601 0.2182 0.2652 0.046 Uiso 1 1 calc R . . H1B H 0.7957 0.1586 0.2134 0.046 Uiso 1 1 calc R . . C2 C 0.8080(3) 0.2191(3) 0.1318(3) 0.0567(12) Uani 1 1 d U . . H2A H 0.7610 0.2077 0.0792 0.068 Uiso 1 1 calc R A 1 H2B H 0.8194 0.2767 0.1266 0.068 Uiso 1 1 calc R A 1 C3 C 0.8549(9) 0.1580(11) 0.1341(10) 0.071(3) Uani 0.72(4) 1 d PU B 1 H3A H 0.8577 0.1743 0.0883 0.085 Uiso 0.72(4) 1 calc PR B 1 H3B H 0.9006 0.1636 0.1910 0.085 Uiso 0.72(4) 1 calc PR B 1 C3A C 0.832(2) 0.123(4) 0.122(2) 0.073(7) Uani 0.28(4) 1 d PU B 2 H3A1 H 0.8181 0.0767 0.1411 0.088 Uiso 0.28(4) 1 calc PR B 2 H3A2 H 0.8156 0.1117 0.0624 0.088 Uiso 0.28(4) 1 calc PR B 2 C4 C 0.8347(9) 0.0693(8) 0.1212(12) 0.103(5) Uani 0.527(15) 1 d PU B 1 H4A H 0.8060 0.0606 0.1372 0.155 Uiso 0.527(15) 1 calc PR B 1 H4B H 0.8751 0.0343 0.1580 0.155 Uiso 0.527(15) 1 calc PR B 1 H4C H 0.8098 0.0542 0.0599 0.155 Uiso 0.527(15) 1 calc PR B 1 C4A C 0.9149(8) 0.1388(12) 0.1920(11) 0.112(7) Uani 0.473(15) 1 d PU B 2 H4A1 H 0.9265 0.1852 0.1713 0.168 Uiso 0.473(15) 1 calc PR B 2 H4A2 H 0.9385 0.0881 0.1965 0.168 Uiso 0.473(15) 1 calc PR B 2 H4A3 H 0.9287 0.1526 0.2494 0.168 Uiso 0.473(15) 1 calc PR B 2 C5 C 0.7128(2) 0.4053(3) 0.2508(3) 0.0575(12) Uani 1 1 d U . . H5A H 0.7440 0.4156 0.3144 0.069 Uiso 1 1 calc R . . H5B H 0.7121 0.4569 0.2227 0.069 Uiso 1 1 calc R . . C6 C 0.6402(4) 0.3938(4) 0.2219(5) 0.098(2) Uani 1 1 d U . . H6A H 0.6220 0.4492 0.2202 0.118 Uiso 1 1 calc R . . H6B H 0.6099 0.3700 0.1624 0.118 Uiso 1 1 calc R . . C7 C 0.6406(5) 0.3429(6) 0.2768(6) 0.125(3) Uani 1 1 d U . . H7A H 0.6747 0.3626 0.3376 0.150 Uiso 1 1 calc R . . H7B H 0.6526 0.2853 0.2729 0.150 Uiso 1 1 calc R . . C8 C 0.5656(5) 0.3436(7) 0.2501(9) 0.186(5) Uani 1 1 d U . . H8A H 0.5600 0.3949 0.2719 0.279 Uiso 1 1 calc R . . H8B H 0.5609 0.2949 0.2759 0.279 Uiso 1 1 calc R . . H8C H 0.5311 0.3413 0.1865 0.279 Uiso 1 1 calc R . . C9 C 0.66615(19) 0.0964(2) 0.1096(3) 0.0420(9) Uani 1 1 d . . . H9 H 0.6900 0.0741 0.1665 0.050 Uiso 1 1 calc R . . C10 C 0.6507(2) 0.0458(2) 0.0419(3) 0.0503(11) Uani 1 1 d . . . H10 H 0.6638 -0.0113 0.0529 0.060 Uiso 1 1 calc R . . C11 C 0.6161(2) 0.0780(2) -0.0424(3) 0.0448(10) Uani 1 1 d . . . H11 H 0.6076 0.0441 -0.0877 0.054 Uiso 1 1 calc R . . C12 C 0.59430(19) 0.1617(3) -0.0583(3) 0.0426(9) Uani 1 1 d . . . H12 H 0.5691 0.1841 -0.1154 0.051 Uiso 1 1 calc R . . C13 C 0.60993(18) 0.2121(2) 0.0106(2) 0.0351(8) Uani 1 1 d . . . C14 C 0.58612(19) 0.3017(2) -0.0036(3) 0.0355(8) Uani 1 1 d . . . C15 C 0.5176(2) 0.3221(3) -0.0575(3) 0.0500(11) Uani 1 1 d . . . H15 H 0.4846 0.2791 -0.0839 0.060 Uiso 1 1 calc R . . C16 C 0.4974(2) 0.4067(3) -0.0728(3) 0.0606(13) Uani 1 1 d . . . H16 H 0.4510 0.4210 -0.1081 0.073 Uiso 1 1 calc R . . C17 C 0.5468(2) 0.4693(3) -0.0350(3) 0.0550(11) Uani 1 1 d . . . H17 H 0.5340 0.5264 -0.0465 0.066 Uiso 1 1 calc R . . C18 C 0.6154(2) 0.4470(2) 0.0199(3) 0.0465(10) Uani 1 1 d . . . H18 H 0.6490 0.4893 0.0465 0.056 Uiso 1 1 calc R . . C19 C 0.95219(17) 0.4929(2) 0.3774(2) 0.0332(8) Uani 1 1 d . . . C20 C 0.97925(17) 0.4699(2) 0.4649(2) 0.0321(8) Uani 1 1 d . . . C21 C 0.96584(18) 0.3901(2) 0.4860(2) 0.0366(8) Uani 1 1 d . . . H21 H 0.9369 0.3511 0.4407 0.044 Uiso 1 1 calc R . . C22 C 0.9944(2) 0.3695(2) 0.5709(3) 0.0437(9) Uani 1 1 d . . . H22 H 0.9865 0.3158 0.5833 0.052 Uiso 1 1 calc R . . C23 C 1.03572(19) 0.4282(2) 0.6402(3) 0.0394(9) Uani 1 1 d . . . H23 H 1.0549 0.4135 0.6981 0.047 Uiso 1 1 calc R . . C24 C 0.7661(2) 0.1833(2) 0.4349(3) 0.0377(9) Uani 1 1 d . . . C25 C 0.77420(19) 0.2487(2) 0.4920(2) 0.0364(8) Uani 1 1 d . . . C26 C 0.8279(2) 0.3091(2) 0.5345(3) 0.0440(10) Uani 1 1 d . . . H26 H 0.8604 0.3069 0.5259 0.053 Uiso 1 1 calc R . . C27 C 0.8330(2) 0.3703(3) 0.5878(3) 0.0521(11) Uani 1 1 d . . . H27 H 0.8683 0.4103 0.6142 0.062 Uiso 1 1 calc R . . C28 C 0.7863(2) 0.3741(3) 0.6036(3) 0.0478(10) Uani 1 1 d . . . H28 H 0.7908 0.4163 0.6407 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.03260(17) 0.03442(17) 0.03001(18) -0.00527(9) 0.02003(14) -0.00305(9) S1 0.0559(6) 0.0365(5) 0.0416(6) 0.0026(4) 0.0353(5) 0.0053(4) S2 0.0320(5) 0.0352(5) 0.0294(5) -0.0004(3) 0.0163(4) -0.0004(4) O1 0.0412(14) 0.0434(14) 0.0378(15) -0.0081(12) 0.0268(13) -0.0082(12) O2 0.0331(14) 0.0435(14) 0.0366(14) -0.0014(11) 0.0195(12) -0.0042(11) O3 0.0692(18) 0.0353(14) 0.0430(16) -0.0037(11) 0.0419(15) -0.0037(13) O4 0.087(2) 0.0377(15) 0.0614(19) -0.0070(13) 0.0572(19) 0.0003(15) O5 0.057(2) 0.072(2) 0.057(2) 0.0086(17) 0.0375(18) 0.0165(16) O6 0.0344(14) 0.0435(15) 0.0480(16) -0.0073(12) 0.0240(13) -0.0058(11) O7 0.0676(19) 0.0527(17) 0.0351(15) 0.0009(13) 0.0305(15) -0.0040(15) O8 0.0406(15) 0.0386(14) 0.0459(16) -0.0030(12) 0.0219(13) 0.0037(12) N1 0.0311(16) 0.0373(16) 0.0330(17) -0.0051(13) 0.0189(14) -0.0077(12) N2 0.0370(17) 0.0373(16) 0.0342(17) -0.0034(13) 0.0218(15) -0.0047(13) C1 0.039(2) 0.0405(19) 0.036(2) 0.0001(16) 0.0240(17) 0.0043(16) C2 0.076(3) 0.066(3) 0.046(3) 0.001(2) 0.047(3) 0.013(2) C3 0.104(8) 0.064(7) 0.086(7) 0.007(5) 0.080(6) 0.012(6) C3A 0.100(12) 0.082(16) 0.075(11) 0.022(12) 0.074(11) 0.042(13) C4 0.164(14) 0.055(7) 0.167(14) 0.017(8) 0.140(12) 0.031(8) C4A 0.096(10) 0.168(16) 0.103(11) 0.049(10) 0.077(9) 0.069(10) C5 0.058(3) 0.055(3) 0.065(3) -0.018(2) 0.042(2) -0.001(2) C6 0.119(5) 0.094(5) 0.126(6) -0.022(4) 0.098(5) 0.002(4) C7 0.139(6) 0.127(6) 0.126(7) 0.036(5) 0.092(6) 0.039(5) C8 0.143(8) 0.235(11) 0.254(14) 0.054(11) 0.161(10) 0.014(8) C9 0.039(2) 0.036(2) 0.044(2) 0.0044(16) 0.0231(18) -0.0012(16) C10 0.055(3) 0.032(2) 0.057(3) -0.0021(18) 0.033(2) 0.0016(18) C11 0.046(2) 0.039(2) 0.045(2) -0.0128(17) 0.0266(19) -0.0039(17) C12 0.036(2) 0.045(2) 0.039(2) -0.0103(17) 0.0198(18) -0.0070(17) C13 0.0296(18) 0.0335(18) 0.036(2) -0.0018(15) 0.0181(16) -0.0028(14) C14 0.0331(19) 0.0322(19) 0.035(2) -0.0037(14) 0.0185(17) -0.0044(14) C15 0.038(2) 0.043(2) 0.051(3) -0.0025(18) 0.019(2) -0.0007(17) C16 0.044(2) 0.050(3) 0.062(3) 0.001(2) 0.022(2) 0.007(2) C17 0.064(3) 0.037(2) 0.059(3) 0.0023(19) 0.037(2) 0.008(2) C18 0.056(3) 0.036(2) 0.048(2) -0.0061(17) 0.033(2) -0.0074(18) C19 0.0277(17) 0.0345(18) 0.0326(19) 0.0017(14) 0.0168(16) -0.0004(14) C20 0.0264(17) 0.0312(17) 0.0344(19) -0.0018(15) 0.0173(15) -0.0002(14) C21 0.037(2) 0.0295(17) 0.038(2) -0.0015(15) 0.0217(17) -0.0050(14) C22 0.051(2) 0.0318(19) 0.043(2) 0.0035(16) 0.027(2) -0.0050(17) C23 0.041(2) 0.040(2) 0.0315(19) 0.0068(15) 0.0205(17) -0.0005(16) C24 0.050(2) 0.0327(18) 0.039(2) 0.0020(15) 0.032(2) -0.0003(16) C25 0.045(2) 0.0313(17) 0.036(2) -0.0028(14) 0.0271(18) -0.0057(15) C26 0.048(2) 0.045(2) 0.047(2) -0.0070(17) 0.035(2) -0.0115(17) C27 0.065(3) 0.042(2) 0.058(3) -0.015(2) 0.043(2) -0.024(2) C28 0.070(3) 0.036(2) 0.046(2) -0.0083(17) 0.041(2) -0.0089(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C5 2.124(4) . ? Sn1 C1 2.126(4) . ? Sn1 O2 2.223(3) . ? Sn1 O1 2.234(3) . ? Sn1 O3 2.257(3) . ? Sn1 O6 2.266(3) . ? S1 O5 1.437(3) . ? S1 O4 1.447(3) . ? S1 O3 1.479(3) . ? S1 C24 1.775(4) . ? S2 O8 1.435(3) . ? S2 O7 1.436(3) . ? S2 O6 1.481(3) . ? S2 C19 1.786(4) . ? O1 N1 1.339(4) . ? O2 N2 1.332(4) . ? N1 C9 1.333(5) . ? N1 C13 1.362(5) . ? N2 C18 1.332(5) . ? N2 C14 1.354(4) . ? C1 C2 1.514(6) . ? C2 C3 1.496(12) . ? C2 C3A 1.68(4) . ? C3 C4 1.44(3) . ? C3A C4A 1.63(6) . ? C5 C6 1.541(8) . ? C6 C7 1.326(10) . ? C7 C8 1.604(11) . ? C9 C10 1.367(6) . ? C10 C11 1.374(6) . ? C11 C12 1.377(5) . ? C12 C13 1.381(6) . ? C13 C14 1.481(5) . ? C14 C15 1.369(6) . ? C15 C16 1.382(6) . ? C16 C17 1.372(6) . ? C17 C18 1.376(6) . ? C19 C23 1.366(5) 5_766 ? C19 C20 1.421(5) . ? C20 C21 1.422(5) . ? C20 C20 1.426(7) 5_766 ? C21 C22 1.356(6) . ? C22 C23 1.402(5) . ? C23 C19 1.366(5) 5_766 ? C24 C28 1.361(6) 7_656 ? C24 C25 1.426(5) . ? C25 C26 1.408(5) . ? C25 C25 1.433(8) 7_656 ? C26 C27 1.358(6) . ? C27 C28 1.388(6) . ? C28 C24 1.361(6) 7_656 ? 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 C5 Sn1 C1 173.55(17) . . ? C5 Sn1 O2 94.25(16) . . ? C1 Sn1 O2 89.74(13) . . ? C5 Sn1 O1 90.69(14) . . ? C1 Sn1 O1 94.99(13) . . ? O2 Sn1 O1 80.14(9) . . ? C5 Sn1 O3 88.58(16) . . ? C1 Sn1 O3 87.70(13) . . ? O2 Sn1 O3 175.92(9) . . ? O1 Sn1 O3 96.91(10) . . ? C5 Sn1 O6 81.88(15) . . ? C1 Sn1 O6 92.88(13) . . ? O2 Sn1 O6 92.85(10) . . ? O1 Sn1 O6 169.42(10) . . ? O3 Sn1 O6 90.46(10) . . ? O5 S1 O4 114.3(2) . . ? O5 S1 O3 111.0(2) . . ? O4 S1 O3 111.80(18) . . ? O5 S1 C24 108.0(2) . . ? O4 S1 C24 106.91(19) . . ? O3 S1 C24 104.09(17) . . ? O8 S2 O7 115.22(19) . . ? O8 S2 O6 111.14(17) . . ? O7 S2 O6 112.09(18) . . ? O8 S2 C19 107.02(16) . . ? O7 S2 C19 106.98(18) . . ? O6 S2 C19 103.48(17) . . ? N1 O1 Sn1 115.2(2) . . ? N2 O2 Sn1 118.9(2) . . ? S1 O3 Sn1 136.65(16) . . ? S2 O6 Sn1 138.51(16) . . ? C9 N1 O1 119.5(3) . . ? C9 N1 C13 121.7(3) . . ? O1 N1 C13 118.8(3) . . ? C18 N2 O2 118.9(3) . . ? C18 N2 C14 121.8(3) . . ? O2 N2 C14 119.0(3) . . ? C2 C1 Sn1 117.9(3) . . ? C3 C2 C1 113.9(6) . . ? C3 C2 C3A 25.2(14) . . ? C1 C2 C3A 106.3(12) . . ? C4 C3 C2 115.4(15) . . ? C4A C3A C2 97(3) . . ? C6 C5 Sn1 120.1(3) . . ? C7 C6 C5 111.9(7) . . ? C6 C7 C8 109.0(7) . . ? N1 C9 C10 119.6(4) . . ? C9 C10 C11 120.9(4) . . ? C10 C11 C12 118.6(4) . . ? C11 C12 C13 119.9(4) . . ? N1 C13 C12 119.2(3) . . ? N1 C13 C14 118.8(3) . . ? C12 C13 C14 121.9(4) . . ? N2 C14 C15 119.3(3) . . ? N2 C14 C13 118.9(3) . . ? C15 C14 C13 121.8(3) . . ? C14 C15 C16 120.1(4) . . ? C17 C16 C15 119.0(4) . . ? C16 C17 C18 119.8(4) . . ? N2 C18 C17 120.0(4) . . ? C23 C19 C20 121.1(3) 5_766 . ? C23 C19 S2 116.8(3) 5_766 . ? C20 C19 S2 122.1(3) . . ? C19 C20 C21 123.2(3) . . ? C19 C20 C20 118.8(4) . 5_766 ? C21 C20 C20 117.9(4) . 5_766 ? C22 C21 C20 121.4(3) . . ? C21 C22 C23 120.7(3) . . ? C19 C23 C22 119.9(4) 5_766 . ? C28 C24 C25 120.9(4) 7_656 . ? C28 C24 S1 117.8(3) 7_656 . ? C25 C24 S1 121.2(3) . . ? C26 C25 C24 123.4(4) . . ? C26 C25 C25 118.8(4) . 7_656 ? C24 C25 C25 117.8(4) . 7_656 ? C27 C26 C25 121.0(4) . . ? C26 C27 C28 121.0(4) . . ? C24 C28 C27 120.5(4) 7_656 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.611 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.113 # Attachment '2_sec_revis.cif' data_22janc _database_code_depnum_ccdc_archive 'CCDC 766495' #TrackingRef '2_sec_revis.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'organotin sulfonate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H38 N2 O13 S2 Sn' _chemical_formula_weight 865.47 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 'C2/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 18.2329(13) _cell_length_b 11.0763(8) _cell_length_c 18.0241(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.3740(10) _cell_angle_gamma 90.00 _cell_volume 3591.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 3518 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.00 _exptl_crystal_description block-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_T_max 0.970 _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 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9742 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3518 _reflns_number_gt 3306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.DFIX restraints (4) and DANG (1) have been applied to 1,2- and 1,3-distances of water. ; _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^)+(0.0260P)^2^+7.6174P] 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 3518 _refine_ls_number_parameters 249 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.5000 1.028650(18) 0.7500 0.01517(8) Uani 1 2 d S . . O2 O 0.60158(9) 1.08994(15) 0.69535(9) 0.0195(3) Uani 1 1 d D . . H101 H 0.6341(13) 1.0385(17) 0.6915(15) 0.023 Uiso 1 1 d D . . H102 H 0.6086(14) 1.1520(16) 0.6722(14) 0.023 Uiso 1 1 d D . . S1 S 0.63361(3) 0.40686(5) 0.64728(3) 0.01576(12) Uani 1 1 d . . . O1 O 0.43406(8) 0.86415(13) 0.78016(8) 0.0173(3) Uani 1 1 d . . . O3 O 0.5000 1.2309(2) 0.7500 0.0263(5) Uani 1 2 d SD . . H103 H 0.4716(14) 1.277(2) 0.7675(15) 0.032 Uiso 1 1 d D . . O4 O 0.70242(9) 0.47131(15) 0.67408(9) 0.0224(4) Uani 1 1 d . . . O5 O 0.58501(9) 0.40067(14) 0.70418(9) 0.0201(3) Uani 1 1 d . . . O6 O 0.64522(9) 0.28910(15) 0.61574(8) 0.0218(3) Uani 1 1 d . . . O7 O 0.27220(9) 0.96642(14) 0.81874(9) 0.0211(3) Uani 1 1 d D . . H104 H 0.2499(14) 0.975(2) 0.7750(8) 0.025 Uiso 1 1 d D . . N1 N 0.41628(10) 0.77911(16) 0.72772(10) 0.0160(4) Uani 1 1 d . . . C1 C 0.43496(12) 1.02108(19) 0.64140(12) 0.0162(4) Uani 1 1 d . . . C2 C 0.45843(14) 0.9496(2) 0.58614(13) 0.0240(5) Uani 1 1 d . . . H2 H 0.5055 0.9149 0.5951 0.029 Uiso 1 1 calc R . . C3 C 0.41245(15) 0.9296(2) 0.51779(13) 0.0287(6) Uani 1 1 d . . . H3 H 0.4287 0.8813 0.4815 0.034 Uiso 1 1 calc R . . C4 C 0.34259(14) 0.9815(2) 0.50382(13) 0.0254(5) Uani 1 1 d . . . H4 H 0.3115 0.9676 0.4584 0.030 Uiso 1 1 calc R . . C5 C 0.31925(13) 1.0539(2) 0.55761(13) 0.0266(5) Uani 1 1 d . . . H5 H 0.2725 1.0898 0.5480 0.032 Uiso 1 1 calc R . . C6 C 0.36512(13) 1.0739(2) 0.62635(13) 0.0222(5) Uani 1 1 d . . . H6 H 0.3488 1.1228 0.6623 0.027 Uiso 1 1 calc R . . C7 C 0.34995(12) 0.7849(2) 0.68202(12) 0.0195(5) Uani 1 1 d . . . H7 H 0.3181 0.8494 0.6859 0.023 Uiso 1 1 calc R . . C8 C 0.32926(13) 0.6956(2) 0.62973(13) 0.0217(5) Uani 1 1 d . . . H8 H 0.2836 0.6996 0.5982 0.026 Uiso 1 1 calc R . . C9 C 0.37680(13) 0.5996(2) 0.62429(12) 0.0211(5) Uani 1 1 d . . . H9 H 0.3635 0.5392 0.5888 0.025 Uiso 1 1 calc R . . C10 C 0.44440(12) 0.5947(2) 0.67229(12) 0.0185(4) Uani 1 1 d . . . H10 H 0.4762 0.5296 0.6701 0.022 Uiso 1 1 calc R . . C11 C 0.46452(12) 0.68696(19) 0.72343(12) 0.0161(4) Uani 1 1 d . . . C12 C 0.58560(12) 0.4990(2) 0.57341(12) 0.0177(4) Uani 1 1 d . . . C13 C 0.61450(13) 0.6106(2) 0.56372(13) 0.0217(5) Uani 1 1 d . . . H13 H 0.6578 0.6353 0.5946 0.026 Uiso 1 1 calc R . . C14 C 0.57894(13) 0.6886(2) 0.50707(13) 0.0239(5) Uani 1 1 d . . . H14 H 0.5993 0.7641 0.5005 0.029 Uiso 1 1 calc R . . C15 C 0.51501(13) 0.6541(2) 0.46207(12) 0.0196(5) Uani 1 1 d . . . H15 H 0.4925 0.7058 0.4245 0.024 Uiso 1 1 calc R . . C16 C 0.51782(12) 0.46006(19) 0.52827(12) 0.0148(4) Uani 1 1 d . . . C17 C 0.25658(18) 0.8491(2) 0.84275(15) 0.0356(6) Uani 1 1 d . . . H17A H 0.2882 0.8314 0.8895 0.053 Uiso 1 1 calc R . . H17B H 0.2654 0.7913 0.8055 0.053 Uiso 1 1 calc R . . H17C H 0.2055 0.8447 0.8496 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01608(12) 0.01494(12) 0.01433(11) 0.000 0.00198(8) 0.000 O2 0.0200(8) 0.0154(8) 0.0247(8) 0.0048(6) 0.0080(7) 0.0029(7) S1 0.0133(3) 0.0178(3) 0.0156(2) 0.0028(2) 0.0003(2) 0.0003(2) O1 0.0190(8) 0.0153(8) 0.0178(7) -0.0053(6) 0.0039(6) -0.0011(6) O3 0.0273(13) 0.0157(12) 0.0400(14) 0.000 0.0182(11) 0.000 O4 0.0155(8) 0.0272(9) 0.0223(8) 0.0065(7) -0.0034(6) -0.0047(7) O5 0.0197(8) 0.0201(8) 0.0210(8) 0.0021(6) 0.0047(6) -0.0008(6) O6 0.0227(8) 0.0210(8) 0.0213(8) 0.0028(7) 0.0023(6) 0.0050(7) O7 0.0200(8) 0.0214(9) 0.0205(8) 0.0003(7) -0.0011(7) -0.0012(7) N1 0.0170(9) 0.0144(9) 0.0172(8) -0.0004(7) 0.0050(7) -0.0020(7) C1 0.0173(11) 0.0165(11) 0.0149(10) 0.0021(8) 0.0028(8) -0.0011(9) C2 0.0243(12) 0.0288(13) 0.0190(11) -0.0009(10) 0.0037(9) 0.0056(10) C3 0.0378(15) 0.0289(13) 0.0187(11) -0.0046(10) 0.0020(10) 0.0022(12) C4 0.0286(13) 0.0286(13) 0.0168(11) 0.0023(9) -0.0028(10) -0.0089(11) C5 0.0176(11) 0.0378(14) 0.0238(12) 0.0092(11) 0.0017(10) 0.0017(10) C6 0.0233(12) 0.0244(12) 0.0195(11) 0.0018(9) 0.0050(9) 0.0041(10) C7 0.0135(10) 0.0197(11) 0.0256(11) 0.0024(9) 0.0044(9) 0.0005(9) C8 0.0167(11) 0.0236(12) 0.0238(11) 0.0014(9) 0.0004(9) -0.0035(9) C9 0.0217(11) 0.0220(12) 0.0193(11) -0.0036(9) 0.0027(9) -0.0048(9) C10 0.0190(11) 0.0167(11) 0.0209(11) -0.0005(9) 0.0062(9) -0.0006(9) C11 0.0156(11) 0.0135(10) 0.0199(10) 0.0027(8) 0.0055(9) 0.0006(8) C12 0.0154(10) 0.0213(11) 0.0156(10) 0.0015(9) 0.0005(8) 0.0023(9) C13 0.0186(11) 0.0225(12) 0.0224(11) 0.0013(9) -0.0016(9) -0.0027(9) C14 0.0230(12) 0.0181(12) 0.0293(12) 0.0042(10) 0.0000(10) -0.0058(10) C15 0.0208(11) 0.0161(11) 0.0209(11) 0.0029(9) 0.0004(9) 0.0003(9) C16 0.0145(10) 0.0151(11) 0.0153(10) -0.0007(8) 0.0035(8) 0.0016(8) C17 0.0565(18) 0.0234(13) 0.0254(12) 0.0024(11) 0.0021(12) -0.0002(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.119(2) . ? Sn1 C1 2.119(2) 2_656 ? Sn1 O3 2.240(2) . ? Sn1 O1 2.2964(15) 2_656 ? Sn1 O1 2.2965(15) . ? Sn1 O2 2.3356(15) 2_656 ? Sn1 O2 2.3357(15) . ? S1 O6 1.4521(17) . ? S1 O4 1.4558(16) . ? S1 O5 1.4621(16) . ? S1 C12 1.789(2) . ? O1 N1 1.336(2) . ? O7 C17 1.414(3) . ? N1 C7 1.349(3) . ? N1 C11 1.358(3) . ? C1 C6 1.387(3) . ? C1 C2 1.393(3) . ? C2 C3 1.390(3) . ? C3 C4 1.383(4) . ? C4 C5 1.378(4) . ? C5 C6 1.395(3) . ? C7 C8 1.376(3) . ? C8 C9 1.385(3) . ? C9 C10 1.387(3) . ? C10 C11 1.385(3) . ? C11 C11 1.479(4) 2_656 ? C12 C13 1.366(3) . ? C12 C16 1.431(3) . ? C13 C14 1.412(3) . ? C14 C15 1.362(3) . ? C15 C16 1.421(3) 5_666 ? C16 C15 1.421(3) 5_666 ? C16 C16 1.424(4) 5_666 ? 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 C1 Sn1 C1 175.46(12) . 2_656 ? C1 Sn1 O3 92.27(6) . . ? C1 Sn1 O3 92.27(6) 2_656 . ? C1 Sn1 O1 89.18(7) . 2_656 ? C1 Sn1 O1 87.22(7) 2_656 2_656 ? O3 Sn1 O1 142.50(4) . 2_656 ? C1 Sn1 O1 87.22(7) . . ? C1 Sn1 O1 89.18(7) 2_656 . ? O3 Sn1 O1 142.50(4) . . ? O1 Sn1 O1 74.99(7) 2_656 . ? C1 Sn1 O2 92.19(7) . 2_656 ? C1 Sn1 O2 89.13(7) 2_656 2_656 ? O3 Sn1 O2 73.10(4) . 2_656 ? O1 Sn1 O2 144.30(6) 2_656 2_656 ? O1 Sn1 O2 69.46(6) . 2_656 ? C1 Sn1 O2 89.13(7) . . ? C1 Sn1 O2 92.19(7) 2_656 . ? O3 Sn1 O2 73.10(4) . . ? O1 Sn1 O2 69.46(5) 2_656 . ? O1 Sn1 O2 144.30(5) . . ? O2 Sn1 O2 146.21(8) 2_656 . ? O6 S1 O4 113.43(10) . . ? O6 S1 O5 112.10(10) . . ? O4 S1 O5 112.22(10) . . ? O6 S1 C12 107.82(10) . . ? O4 S1 C12 104.94(10) . . ? O5 S1 C12 105.65(10) . . ? N1 O1 Sn1 117.90(11) . . ? O1 N1 C7 119.24(18) . . ? O1 N1 C11 119.04(17) . . ? C7 N1 C11 121.69(19) . . ? C6 C1 C2 118.6(2) . . ? C6 C1 Sn1 121.45(16) . . ? C2 C1 Sn1 119.49(17) . . ? C3 C2 C1 120.9(2) . . ? C4 C3 C2 120.0(2) . . ? C5 C4 C3 119.7(2) . . ? C4 C5 C6 120.5(2) . . ? C1 C6 C5 120.4(2) . . ? N1 C7 C8 120.2(2) . . ? C7 C8 C9 119.7(2) . . ? C8 C9 C10 119.3(2) . . ? C11 C10 C9 119.9(2) . . ? N1 C11 C10 119.26(19) . . ? N1 C11 C11 118.00(16) . 2_656 ? C10 C11 C11 122.68(16) . 2_656 ? C13 C12 C16 121.0(2) . . ? C13 C12 S1 117.34(17) . . ? C16 C12 S1 121.56(17) . . ? C12 C13 C14 120.3(2) . . ? C15 C14 C13 120.4(2) . . ? C14 C15 C16 120.9(2) . 5_666 ? C15 C16 C16 119.2(2) 5_666 5_666 ? C15 C16 C12 122.7(2) 5_666 . ? C16 C16 C12 118.1(2) 5_666 . ? 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 C1 Sn1 O1 N1 38.23(14) . . . . ? C1 Sn1 O1 N1 -139.01(14) 2_656 . . . ? O3 Sn1 O1 N1 128.33(11) . . . . ? O1 Sn1 O1 N1 -51.67(11) 2_656 . . . ? O2 Sn1 O1 N1 131.61(14) 2_656 . . . ? O2 Sn1 O1 N1 -46.39(17) . . . . ? Sn1 O1 N1 C7 -93.06(19) . . . . ? Sn1 O1 N1 C11 89.02(19) . . . . ? C1 Sn1 C1 C6 121.24(19) 2_656 . . . ? O3 Sn1 C1 C6 -58.75(18) . . . . ? O1 Sn1 C1 C6 158.73(19) 2_656 . . . ? O1 Sn1 C1 C6 83.72(19) . . . . ? O2 Sn1 C1 C6 14.41(19) 2_656 . . . ? O2 Sn1 C1 C6 -131.81(19) . . . . ? C1 Sn1 C1 C2 -50.90(18) 2_656 . . . ? O3 Sn1 C1 C2 129.11(18) . . . . ? O1 Sn1 C1 C2 -13.41(18) 2_656 . . . ? O1 Sn1 C1 C2 -88.42(18) . . . . ? O2 Sn1 C1 C2 -157.72(18) 2_656 . . . ? O2 Sn1 C1 C2 56.06(18) . . . . ? C6 C1 C2 C3 -1.2(4) . . . . ? Sn1 C1 C2 C3 171.19(19) . . . . ? C1 C2 C3 C4 0.4(4) . . . . ? C2 C3 C4 C5 0.7(4) . . . . ? C3 C4 C5 C6 -0.9(4) . . . . ? C2 C1 C6 C5 0.9(3) . . . . ? Sn1 C1 C6 C5 -171.27(18) . . . . ? C4 C5 C6 C1 0.1(4) . . . . ? O1 N1 C7 C8 -177.33(19) . . . . ? C11 N1 C7 C8 0.5(3) . . . . ? N1 C7 C8 C9 0.1(3) . . . . ? C7 C8 C9 C10 0.6(3) . . . . ? C8 C9 C10 C11 -1.8(3) . . . . ? O1 N1 C11 C10 176.06(18) . . . . ? C7 N1 C11 C10 -1.8(3) . . . . ? O1 N1 C11 C11 -1.2(3) . . . 2_656 ? C7 N1 C11 C11 -179.0(2) . . . 2_656 ? C9 C10 C11 N1 2.4(3) . . . . ? C9 C10 C11 C11 179.5(2) . . . 2_656 ? O6 S1 C12 C13 -129.53(19) . . . . ? O4 S1 C12 C13 -8.3(2) . . . . ? O5 S1 C12 C13 110.44(19) . . . . ? O6 S1 C12 C16 53.2(2) . . . . ? O4 S1 C12 C16 174.38(18) . . . . ? O5 S1 C12 C16 -66.9(2) . . . . ? C16 C12 C13 C14 -1.9(3) . . . . ? S1 C12 C13 C14 -179.23(18) . . . . ? C12 C13 C14 C15 0.8(4) . . . . ? C13 C14 C15 C16 0.9(4) . . . 5_666 ? C13 C12 C16 C15 -178.4(2) . . . 5_666 ? S1 C12 C16 C15 -1.2(3) . . . 5_666 ? C13 C12 C16 C16 1.4(4) . . . 5_666 ? S1 C12 C16 C16 178.6(2) . . . 5_666 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.813 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.074 data_4sepam _database_code_depnum_ccdc_archive 'CCDC 766496' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'organotin sulfonate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H40 N4 O14 S2 Sn' _chemical_formula_weight 1007.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_HALL '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.526(5) _cell_length_b 11.739(5) _cell_length_c 18.285(5) _cell_angle_alpha 92.530(5) _cell_angle_beta 103.242(5) _cell_angle_gamma 100.479(5) _cell_volume 2153.9(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4115 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.79 _exptl_crystal_description blocklike _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 0.763 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.925 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10866 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7408 _reflns_number_gt 6111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX (8) restraint used for O-H bond distances of the water molecule. The distance between two hydrogens have been made similar for all the water molecules,using SADI (6) restraint. ; _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^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7408 _refine_ls_number_parameters 592 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.59481(3) 0.16588(2) 0.762858(15) 0.03375(12) Uani 1 1 d . . . S1 S 0.80553(13) 0.68458(11) 0.54717(8) 0.0516(3) Uani 1 1 d . . . S2 S 0.47378(14) 0.57682(10) 0.81861(6) 0.0469(3) Uani 1 1 d . . . O1 O 0.6543(3) 0.0708(2) 0.87368(15) 0.0380(7) Uani 1 1 d . . . O2 O 0.5700(3) 0.2758(2) 0.86308(15) 0.0367(7) Uani 1 1 d . . . O3 O 0.5719(3) 0.1517(2) 0.63609(15) 0.0375(7) Uani 1 1 d . . . O4 O 0.6655(3) -0.0032(2) 0.73190(15) 0.0363(7) Uani 1 1 d . . . O5 O 0.5200(4) 0.3235(3) 0.71940(18) 0.0486(8) Uani 1 1 d D . . H101 H 0.508(6) 0.350(4) 0.7541(19) 0.058 Uiso 1 1 d D . . H102 H 0.528(6) 0.366(3) 0.692(2) 0.058 Uiso 1 1 d D . . O6 O 0.6856(4) 0.5991(3) 0.5321(2) 0.0736(11) Uani 1 1 d . . . O7 O 0.8284(4) 0.7508(4) 0.6215(2) 0.0756(11) Uani 1 1 d . . . O8 O 0.8191(4) 0.7586(3) 0.4891(2) 0.0749(12) Uani 1 1 d . . . O9 O 0.3860(3) 0.4668(3) 0.78450(17) 0.0512(8) Uani 1 1 d . . . O10 O 0.5819(4) 0.6075(3) 0.7819(2) 0.0670(10) Uani 1 1 d . . . O11 O 0.4030(5) 0.6700(3) 0.8256(2) 0.0716(12) Uani 1 1 d . . . O12 O 0.5376(5) 0.4231(3) 0.5931(2) 0.0721(12) Uani 1 1 d D . . H103 H 0.585(5) 0.474(4) 0.584(4) 0.086 Uiso 1 1 d D . . H104 H 0.486(5) 0.451(5) 0.607(4) 0.086 Uiso 1 1 d D . . O13 O 0.8372(5) 0.6964(5) 0.7678(3) 0.0814(13) Uani 1 1 d D . . H105 H 0.768(3) 0.666(6) 0.763(4) 0.098 Uiso 1 1 d D . . H106 H 0.845(7) 0.716(6) 0.730(2) 0.098 Uiso 1 1 d D . . O14 O 0.8270(5) 0.8936(4) 0.8558(2) 0.0829(14) Uani 1 1 d D . . H107 H 0.843(7) 0.842(4) 0.833(3) 0.099 Uiso 1 1 d D . . H108 H 0.776(6) 0.915(6) 0.825(3) 0.099 Uiso 1 1 d D . . N1 N 0.7348(4) 0.1292(3) 0.93615(19) 0.0369(8) Uani 1 1 d . . . N2 N 0.4878(4) 0.2282(3) 0.90423(19) 0.0382(8) Uani 1 1 d . . . N3 N 0.6781(4) 0.1420(3) 0.60930(19) 0.0355(8) Uani 1 1 d . . . N4 N 0.5946(3) -0.0811(3) 0.67551(18) 0.0333(8) Uani 1 1 d . . . C1 C 0.3969(4) 0.0707(4) 0.7408(2) 0.0361(9) Uani 1 1 d . . . C2 C 0.3031(5) 0.0974(4) 0.6812(3) 0.0559(13) Uani 1 1 d . . . H2 H 0.3264 0.1573 0.6523 0.067 Uiso 1 1 calc R . . C3 C 0.1741(6) 0.0340(6) 0.6650(4) 0.0774(19) Uani 1 1 d . . . H3 H 0.1110 0.0538 0.6257 0.093 Uiso 1 1 calc R . . C4 C 0.1368(6) -0.0551(6) 0.7041(4) 0.086(2) Uani 1 1 d . . . H4 H 0.0494 -0.0963 0.6921 0.103 Uiso 1 1 calc R . . C5 C 0.2302(7) -0.0842(6) 0.7620(4) 0.085(2) Uani 1 1 d . . . H5 H 0.2062 -0.1467 0.7889 0.102 Uiso 1 1 calc R . . C6 C 0.3593(5) -0.0219(5) 0.7808(3) 0.0592(14) Uani 1 1 d . . . H6 H 0.4215 -0.0421 0.8204 0.071 Uiso 1 1 calc R . . C7 C 0.7958(4) 0.2533(4) 0.7798(2) 0.0364(10) Uani 1 1 d . . . C8 C 0.8947(5) 0.1954(4) 0.7705(3) 0.0479(12) Uani 1 1 d . . . H8 H 0.8758 0.1146 0.7632 0.057 Uiso 1 1 calc R . . C9 C 1.0231(5) 0.2557(5) 0.7717(3) 0.0588(14) Uani 1 1 d . . . H9 H 1.0882 0.2160 0.7637 0.071 Uiso 1 1 calc R . . C10 C 1.0504(6) 0.3747(6) 0.7849(3) 0.0730(18) Uani 1 1 d . . . H10 H 1.1355 0.4160 0.7866 0.088 Uiso 1 1 calc R . . C11 C 0.9570(7) 0.4315(5) 0.7951(4) 0.0775(19) Uani 1 1 d . . . H11 H 0.9781 0.5122 0.8037 0.093 Uiso 1 1 calc R . . C12 C 0.8274(6) 0.3736(4) 0.7934(3) 0.0602(14) Uani 1 1 d . . . H12 H 0.7636 0.4151 0.8011 0.072 Uiso 1 1 calc R . . C13 C 0.8653(5) 0.1284(4) 0.9501(3) 0.0456(11) Uani 1 1 d . . . H13 H 0.8995 0.0939 0.9141 0.055 Uiso 1 1 calc R . . C14 C 0.9501(5) 0.1793(5) 1.0187(3) 0.0607(14) Uani 1 1 d . . . H14 H 1.0408 0.1791 1.0286 0.073 Uiso 1 1 calc R . . C15 C 0.8974(6) 0.2306(5) 1.0722(3) 0.0638(15) Uani 1 1 d . . . H15 H 0.9517 0.2639 1.1185 0.077 Uiso 1 1 calc R . . C16 C 0.7650(6) 0.2306(4) 1.0551(3) 0.0523(13) Uani 1 1 d . . . H16 H 0.7292 0.2645 1.0906 0.063 Uiso 1 1 calc R . . C17 C 0.6824(5) 0.1824(4) 0.9874(2) 0.0380(10) Uani 1 1 d . . . C18 C 0.5405(5) 0.1815(4) 0.9679(2) 0.0396(10) Uani 1 1 d . . . C19 C 0.4558(5) 0.1425(4) 1.0145(3) 0.0507(12) Uani 1 1 d . . . H19 H 0.4898 0.1119 1.0592 0.061 Uiso 1 1 calc R . . C20 C 0.3251(6) 0.1487(5) 0.9954(3) 0.0591(14) Uani 1 1 d . . . H20 H 0.2696 0.1227 1.0267 0.071 Uiso 1 1 calc R . . C21 C 0.2764(5) 0.1935(4) 0.9297(3) 0.0569(13) Uani 1 1 d . . . H21 H 0.1863 0.1954 0.9151 0.068 Uiso 1 1 calc R . . C22 C 0.3590(5) 0.2358(4) 0.8849(3) 0.0448(11) Uani 1 1 d . . . H22 H 0.3259 0.2696 0.8413 0.054 Uiso 1 1 calc R . . C23 C 0.7594(5) 0.2396(4) 0.5989(3) 0.0496(12) Uani 1 1 d . . . H23 H 0.7465 0.3123 0.6145 0.060 Uiso 1 1 calc R . . C24 C 0.8615(6) 0.2309(5) 0.5652(3) 0.0619(15) Uani 1 1 d . . . H24 H 0.9181 0.2981 0.5585 0.074 Uiso 1 1 calc R . . C25 C 0.8810(6) 0.1268(5) 0.5416(3) 0.0641(15) Uani 1 1 d . . . H25 H 0.9481 0.1219 0.5169 0.077 Uiso 1 1 calc R . . C26 C 0.7992(5) 0.0263(5) 0.5548(3) 0.0527(12) Uani 1 1 d . . . H26 H 0.8126 -0.0464 0.5397 0.063 Uiso 1 1 calc R . . C27 C 0.6989(4) 0.0348(4) 0.5899(2) 0.0378(10) Uani 1 1 d . . . C28 C 0.6073(4) -0.0670(3) 0.6041(2) 0.0339(9) Uani 1 1 d . . . C29 C 0.5418(5) -0.1537(4) 0.5479(2) 0.0435(11) Uani 1 1 d . . . H29 H 0.5503 -0.1455 0.4989 0.052 Uiso 1 1 calc R . . C30 C 0.4640(5) -0.2520(4) 0.5637(3) 0.0526(13) Uani 1 1 d . . . H30 H 0.4186 -0.3098 0.5254 0.063 Uiso 1 1 calc R . . C31 C 0.4536(5) -0.2643(4) 0.6367(3) 0.0528(13) Uani 1 1 d . . . H31 H 0.4019 -0.3309 0.6482 0.063 Uiso 1 1 calc R . . C32 C 0.5203(5) -0.1776(4) 0.6923(3) 0.0464(12) Uani 1 1 d . . . H32 H 0.5139 -0.1856 0.7418 0.056 Uiso 1 1 calc R . . C33 C 0.9479(5) 0.5310(4) 0.4971(3) 0.0423(11) Uani 1 1 d . . . C34 C 0.9363(5) 0.6032(4) 0.5577(3) 0.0527(13) Uani 1 1 d . . . C35 C 1.0271(5) 0.6118(5) 0.6249(3) 0.0595(14) Uani 1 1 d . . . H35 H 1.0203 0.6597 0.6651 0.071 Uiso 1 1 calc R . . C36 C 1.1313(5) 0.5493(4) 0.6345(3) 0.0522(12) Uani 1 1 d . . . H36 H 1.1907 0.5552 0.6814 0.063 Uiso 1 1 calc R . . C37 C 1.1468(5) 0.4811(4) 0.5772(3) 0.0530(13) Uani 1 1 d . . . H37 H 1.2172 0.4417 0.5846 0.064 Uiso 1 1 calc R . . C38 C 0.5488(5) 0.5485(4) 0.9119(3) 0.0441(11) Uani 1 1 d . . . C39 C 0.6821(6) 0.5578(4) 0.9320(3) 0.0533(13) Uani 1 1 d . . . H39 H 0.7328 0.5822 0.8980 0.064 Uiso 1 1 calc R . . C40 C 0.7449(6) 0.5312(5) 1.0032(3) 0.0565(13) Uani 1 1 d . . . H40 H 0.8368 0.5375 1.0161 0.068 Uiso 1 1 calc R . . C41 C 0.6722(5) 0.4959(4) 1.0546(3) 0.0473(11) Uani 1 1 d . . . H41 H 0.7156 0.4780 1.1017 0.057 Uiso 1 1 calc R . . C42 C 0.5319(5) 0.4862(4) 1.0369(2) 0.0401(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 Sn1 0.03440(19) 0.03563(18) 0.03141(19) 0.00556(12) 0.00820(13) 0.00644(12) S1 0.0450(7) 0.0491(7) 0.0676(8) 0.0134(6) 0.0235(6) 0.0126(5) S2 0.0645(8) 0.0462(7) 0.0346(6) 0.0096(5) 0.0147(6) 0.0175(6) O1 0.0459(18) 0.0375(15) 0.0274(15) -0.0004(12) 0.0016(13) 0.0100(13) O2 0.0411(17) 0.0389(15) 0.0329(15) 0.0056(12) 0.0135(13) 0.0089(13) O3 0.0407(18) 0.0472(17) 0.0311(15) 0.0079(12) 0.0132(13) 0.0182(13) O4 0.0436(18) 0.0331(15) 0.0276(15) -0.0019(11) 0.0006(13) 0.0068(12) O5 0.076(2) 0.0433(19) 0.0365(19) 0.0139(14) 0.0231(18) 0.0239(17) O6 0.054(2) 0.073(3) 0.099(3) 0.018(2) 0.029(2) 0.0092(19) O7 0.070(3) 0.079(3) 0.077(3) -0.006(2) 0.016(2) 0.017(2) O8 0.082(3) 0.068(2) 0.090(3) 0.034(2) 0.038(2) 0.026(2) O9 0.055(2) 0.059(2) 0.0388(18) 0.0045(15) 0.0049(16) 0.0173(16) O10 0.077(3) 0.077(3) 0.052(2) 0.0187(18) 0.026(2) 0.011(2) O11 0.113(4) 0.066(2) 0.052(2) 0.0191(18) 0.024(2) 0.049(2) O12 0.096(4) 0.063(2) 0.057(2) 0.020(2) 0.023(2) 0.007(2) O13 0.078(3) 0.097(4) 0.071(3) -0.004(3) 0.021(3) 0.020(3) O14 0.102(4) 0.088(3) 0.060(3) -0.002(2) -0.007(2) 0.057(3) N1 0.041(2) 0.0389(19) 0.0317(19) 0.0053(15) 0.0068(16) 0.0136(16) N2 0.044(2) 0.0396(19) 0.0330(19) 0.0048(15) 0.0113(17) 0.0109(16) N3 0.037(2) 0.0385(19) 0.0326(19) 0.0086(14) 0.0115(16) 0.0057(15) N4 0.039(2) 0.0319(18) 0.0297(18) 0.0041(14) 0.0076(15) 0.0088(15) C1 0.034(2) 0.041(2) 0.033(2) 0.0003(17) 0.0091(19) 0.0053(18) C2 0.040(3) 0.056(3) 0.063(3) 0.017(2) -0.005(2) 0.007(2) C3 0.047(4) 0.084(4) 0.083(4) 0.013(3) -0.013(3) 0.001(3) C4 0.043(4) 0.093(5) 0.100(5) -0.003(4) 0.001(4) -0.017(3) C5 0.063(4) 0.082(4) 0.091(5) 0.024(4) 0.011(4) -0.028(3) C6 0.049(3) 0.066(3) 0.054(3) 0.019(2) 0.008(3) -0.006(3) C7 0.034(2) 0.041(2) 0.033(2) 0.0015(17) 0.0118(19) 0.0012(18) C8 0.037(3) 0.058(3) 0.042(3) 0.004(2) 0.001(2) 0.003(2) C9 0.040(3) 0.092(4) 0.045(3) 0.001(3) 0.007(2) 0.019(3) C10 0.047(4) 0.089(5) 0.067(4) 0.008(3) 0.005(3) -0.015(3) C11 0.064(4) 0.055(3) 0.099(5) 0.002(3) 0.011(4) -0.012(3) C12 0.057(3) 0.049(3) 0.075(4) -0.003(3) 0.024(3) 0.002(2) C13 0.043(3) 0.060(3) 0.038(3) 0.007(2) 0.009(2) 0.020(2) C14 0.043(3) 0.087(4) 0.047(3) -0.004(3) -0.002(2) 0.021(3) C15 0.060(4) 0.079(4) 0.044(3) -0.009(3) -0.006(3) 0.020(3) C16 0.068(4) 0.062(3) 0.032(3) -0.001(2) 0.009(2) 0.031(3) C17 0.050(3) 0.044(2) 0.025(2) 0.0058(17) 0.0105(19) 0.018(2) C18 0.051(3) 0.041(2) 0.029(2) 0.0052(18) 0.009(2) 0.016(2) C19 0.067(4) 0.056(3) 0.042(3) 0.017(2) 0.024(2) 0.029(2) C20 0.062(4) 0.068(3) 0.065(4) 0.026(3) 0.037(3) 0.026(3) C21 0.046(3) 0.063(3) 0.069(4) 0.010(3) 0.023(3) 0.016(2) C22 0.044(3) 0.053(3) 0.044(3) 0.011(2) 0.014(2) 0.023(2) C23 0.057(3) 0.044(3) 0.049(3) 0.017(2) 0.016(2) 0.005(2) C24 0.053(3) 0.060(3) 0.076(4) 0.029(3) 0.028(3) 0.000(3) C25 0.057(4) 0.079(4) 0.074(4) 0.035(3) 0.039(3) 0.024(3) C26 0.055(3) 0.059(3) 0.055(3) 0.019(2) 0.024(3) 0.020(2) C27 0.037(2) 0.049(3) 0.032(2) 0.0101(18) 0.0125(19) 0.0150(19) C28 0.038(2) 0.038(2) 0.028(2) 0.0056(16) 0.0081(18) 0.0128(18) C29 0.048(3) 0.053(3) 0.030(2) -0.0026(19) 0.006(2) 0.018(2) C30 0.046(3) 0.047(3) 0.053(3) -0.008(2) -0.006(2) 0.004(2) C31 0.059(3) 0.042(3) 0.051(3) 0.006(2) 0.010(3) -0.002(2) C32 0.056(3) 0.039(2) 0.044(3) 0.009(2) 0.017(2) 0.002(2) C33 0.040(3) 0.039(2) 0.051(3) 0.013(2) 0.019(2) 0.0023(18) C34 0.045(3) 0.052(3) 0.060(3) 0.010(2) 0.016(3) 0.000(2) C35 0.047(3) 0.067(3) 0.060(3) 0.009(3) 0.011(3) 0.002(3) C36 0.043(3) 0.065(3) 0.044(3) 0.006(2) 0.005(2) 0.007(2) C37 0.046(3) 0.052(3) 0.058(3) 0.013(2) 0.013(3) 0.000(2) C38 0.058(3) 0.035(2) 0.042(3) 0.0009(18) 0.018(2) 0.011(2) C39 0.061(4) 0.053(3) 0.050(3) 0.007(2) 0.022(3) 0.012(2) C40 0.052(3) 0.070(3) 0.049(3) 0.003(2) 0.011(3) 0.018(3) C41 0.049(3) 0.056(3) 0.039(3) 0.002(2) 0.008(2) 0.021(2) C42 0.049(3) 0.032(2) 0.036(2) 0.0039(17) 0.006(2) 0.0071(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.116(4) . ? Sn1 C7 2.123(4) . ? Sn1 O5 2.246(3) . ? Sn1 O3 2.270(3) . ? Sn1 O2 2.286(3) . ? Sn1 O4 2.333(3) . ? Sn1 O1 2.370(3) . ? S1 O8 1.418(4) . ? S1 O6 1.425(4) . ? S1 O7 1.483(4) . ? S1 C34 1.794(6) . ? S2 O11 1.448(4) . ? S2 O10 1.448(4) . ? S2 O9 1.464(4) . ? S2 C38 1.781(5) . ? O1 N1 1.330(4) . ? O2 N2 1.336(4) . ? O3 N3 1.340(4) . ? O4 N4 1.331(4) . ? N1 C13 1.340(6) . ? N1 C17 1.372(5) . ? N2 C22 1.341(6) . ? N2 C18 1.354(5) . ? N3 C23 1.349(6) . ? N3 C27 1.362(6) . ? N4 C32 1.344(5) . ? N4 C28 1.356(5) . ? C1 C2 1.382(6) . ? C1 C6 1.385(6) . ? C2 C3 1.383(8) . ? C3 C4 1.343(9) . ? C4 C5 1.372(9) . ? C5 C6 1.380(7) . ? C7 C8 1.379(7) . ? C7 C12 1.389(6) . ? C8 C9 1.402(7) . ? C9 C10 1.372(8) . ? C10 C11 1.327(9) . ? C11 C12 1.402(8) . ? C13 C14 1.398(7) . ? C14 C15 1.395(8) . ? C15 C16 1.356(8) . ? C16 C17 1.369(6) . ? C17 C18 1.453(6) . ? C18 C19 1.401(6) . ? C19 C20 1.355(8) . ? C20 C21 1.362(7) . ? C21 C22 1.370(7) . ? C23 C24 1.373(7) . ? C24 C25 1.344(8) . ? C25 C26 1.393(7) . ? C26 C27 1.371(6) . ? C27 C28 1.467(6) . ? C28 C29 1.377(6) . ? C29 C30 1.371(7) . ? C30 C31 1.375(7) . ? C31 C32 1.374(6) . ? C33 C34 1.406(7) . ? C33 C33 1.409(9) 2_766 ? C33 C37 1.474(7) 2_766 ? C34 C35 1.360(7) . ? C35 C36 1.410(8) . ? C36 C37 1.347(7) . ? C37 C33 1.474(7) 2_766 ? C38 C39 1.350(7) . ? C38 C42 1.427(6) 2_667 ? C39 C40 1.395(7) . ? C40 C41 1.374(7) . ? C41 C42 1.420(7) . ? C42 C38 1.427(6) 2_667 ? C42 C42 1.442(8) 2_667 ? 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 C1 Sn1 C7 176.20(15) . . ? C1 Sn1 O5 90.29(16) . . ? C7 Sn1 O5 91.52(16) . . ? C1 Sn1 O3 86.83(13) . . ? C7 Sn1 O3 90.51(13) . . ? O5 Sn1 O3 72.86(11) . . ? C1 Sn1 O2 92.81(14) . . ? C7 Sn1 O2 90.93(14) . . ? O5 Sn1 O2 72.00(11) . . ? O3 Sn1 O2 144.85(10) . . ? C1 Sn1 O4 89.67(14) . . ? C7 Sn1 O4 86.96(14) . . ? O5 Sn1 O4 145.73(11) . . ? O3 Sn1 O4 72.93(10) . . ? O2 Sn1 O4 142.21(10) . . ? C1 Sn1 O1 90.74(14) . . ? C7 Sn1 O1 89.82(14) . . ? O5 Sn1 O1 143.22(11) . . ? O3 Sn1 O1 143.90(10) . . ? O2 Sn1 O1 71.23(10) . . ? O4 Sn1 O1 71.04(10) . . ? O8 S1 O6 115.5(3) . . ? O8 S1 O7 112.2(3) . . ? O6 S1 O7 111.0(3) . . ? O8 S1 C34 107.2(2) . . ? O6 S1 C34 105.0(2) . . ? O7 S1 C34 105.1(3) . . ? O11 S2 O10 113.5(2) . . ? O11 S2 O9 113.3(2) . . ? O10 S2 O9 111.5(2) . . ? O11 S2 C38 106.9(2) . . ? O10 S2 C38 105.9(2) . . ? O9 S2 C38 104.9(2) . . ? N1 O1 Sn1 120.8(2) . . ? N2 O2 Sn1 118.8(2) . . ? N3 O3 Sn1 118.8(2) . . ? N4 O4 Sn1 122.4(2) . . ? O1 N1 C13 119.0(4) . . ? O1 N1 C17 119.7(4) . . ? C13 N1 C17 121.1(4) . . ? O2 N2 C22 119.6(3) . . ? O2 N2 C18 118.2(4) . . ? C22 N2 C18 122.0(4) . . ? O3 N3 C23 118.9(4) . . ? O3 N3 C27 119.9(3) . . ? C23 N3 C27 121.1(4) . . ? O4 N4 C32 118.3(3) . . ? O4 N4 C28 120.0(3) . . ? C32 N4 C28 121.5(4) . . ? C2 C1 C6 118.5(4) . . ? C2 C1 Sn1 118.8(3) . . ? C6 C1 Sn1 122.6(3) . . ? C1 C2 C3 119.4(5) . . ? C4 C3 C2 122.3(6) . . ? C3 C4 C5 118.7(6) . . ? C4 C5 C6 120.7(6) . . ? C5 C6 C1 120.4(5) . . ? C8 C7 C12 118.4(4) . . ? C8 C7 Sn1 121.9(3) . . ? C12 C7 Sn1 119.5(4) . . ? C7 C8 C9 121.4(5) . . ? C10 C9 C8 118.5(5) . . ? C11 C10 C9 120.8(6) . . ? C10 C11 C12 122.0(6) . . ? C7 C12 C11 118.9(5) . . ? N1 C13 C14 120.1(4) . . ? C15 C14 C13 119.3(5) . . ? C16 C15 C14 118.4(5) . . ? C15 C16 C17 122.2(5) . . ? C16 C17 N1 118.8(4) . . ? C16 C17 C18 123.1(4) . . ? N1 C17 C18 118.1(4) . . ? N2 C18 C19 117.6(4) . . ? N2 C18 C17 118.9(4) . . ? C19 C18 C17 123.3(4) . . ? C20 C19 C18 121.1(4) . . ? C19 C20 C21 118.9(5) . . ? C20 C21 C22 120.6(5) . . ? N2 C22 C21 119.7(4) . . ? N3 C23 C24 119.4(5) . . ? C25 C24 C23 121.2(5) . . ? C24 C25 C26 119.0(5) . . ? C27 C26 C25 119.9(5) . . ? N3 C27 C26 119.2(4) . . ? N3 C27 C28 117.8(4) . . ? C26 C27 C28 122.9(4) . . ? N4 C28 C29 118.8(4) . . ? N4 C28 C27 119.4(4) . . ? C29 C28 C27 121.6(4) . . ? C30 C29 C28 120.6(4) . . ? C29 C30 C31 119.3(4) . . ? C32 C31 C30 119.6(4) . . ? N4 C32 C31 120.2(4) . . ? C34 C33 C33 122.4(6) . 2_766 ? C34 C33 C37 121.4(5) . 2_766 ? C33 C33 C37 116.1(5) 2_766 2_766 ? C35 C34 C33 119.0(5) . . ? C35 C34 S1 119.9(4) . . ? C33 C34 S1 121.1(4) . . ? C34 C35 C36 121.1(5) . . ? C37 C36 C35 121.5(5) . . ? C36 C37 C33 119.9(5) . 2_766 ? C39 C38 C42 121.2(4) . 2_667 ? C39 C38 S2 118.6(4) . . ? C42 C38 S2 120.1(4) 2_667 . ? C38 C39 C40 120.8(5) . . ? C41 C40 C39 120.6(5) . . ? C40 C41 C42 121.0(5) . . ? C41 C42 C38 123.7(4) . 2_667 ? C41 C42 C42 117.8(5) . 2_667 ? C38 C42 C42 118.5(5) 2_667 2_667 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.305 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.101 # Attachment 'Comp4_2octb.cif' data_2octb _database_code_depnum_ccdc_archive 'CCDC 766497' #TrackingRef 'Comp4_2octb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'organotin sulfonate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H72 O12 P4 S2 Sn' _chemical_formula_weight 1387.95 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' P P 0.1023 0.0942 '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 'C2/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 33.071(5) _cell_length_b 11.224(5) _cell_length_c 37.192(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 114.090(5) _cell_angle_gamma 90.000(5) _cell_volume 12603(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3487 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 21.93 _exptl_crystal_description blocklike _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5744 _exptl_absorpt_coefficient_mu 0.637 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.950 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 31925 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11069 _reflns_number_gt 7748 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11069 _refine_ls_number_parameters 799 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1390 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.916618(11) 0.95000(3) 0.624175(9) 0.01774(11) Uani 1 1 d . . . S1 S 0.91202(4) 0.73408(11) 0.55339(4) 0.0207(3) Uani 1 1 d . . . S2 S 0.84636(4) 0.61787(11) 0.35665(4) 0.0214(3) Uani 1 1 d . . . P1 P 0.80735(4) 0.87246(11) 0.62021(4) 0.0183(3) Uani 1 1 d . . . P2 P 0.79975(4) 1.11746(11) 0.65599(4) 0.0201(3) Uani 1 1 d . . . P3 P 1.01743(4) 1.06339(11) 0.61626(4) 0.0202(3) Uani 1 1 d . . . P4 P 1.04431(5) 1.17589(12) 0.69757(4) 0.0249(3) Uani 1 1 d . . . O1 O 0.92442(14) 1.0549(3) 0.67656(11) 0.0240(8) Uani 1 1 d . . . O2 O 0.85431(11) 0.8952(3) 0.62625(9) 0.0211(8) Uani 1 1 d . . . O3 O 0.84588(11) 1.1544(3) 0.66333(10) 0.0241(8) Uani 1 1 d . . . O4 O 0.98168(11) 1.0037(3) 0.62472(9) 0.0231(8) Uani 1 1 d . . . O5 O 1.00192(12) 1.1533(3) 0.70093(11) 0.0353(10) Uani 1 1 d . . . O6 O 0.89594(12) 0.8366(3) 0.56919(10) 0.0262(8) Uani 1 1 d . . . O7 O 0.89521(12) 0.6223(3) 0.56093(10) 0.0293(9) Uani 1 1 d . . . O8 O 0.95910(11) 0.7380(3) 0.56448(10) 0.0277(8) Uani 1 1 d . . . O9 O 0.79975(11) 0.6294(3) 0.34870(9) 0.0245(8) Uani 1 1 d . . . O10 O 0.85562(12) 0.5106(3) 0.33986(10) 0.0254(8) Uani 1 1 d . . . O11 O 0.86472(11) 0.7252(3) 0.34775(9) 0.0236(8) Uani 1 1 d . . . C1 C 0.88653(17) 1.0913(4) 0.58428(14) 0.0217(11) Uani 1 1 d . . . H1A H 0.8940 1.0817 0.5618 0.026 Uiso 1 1 calc R . . H1B H 0.8547 1.0824 0.5748 0.026 Uiso 1 1 calc R . . C2 C 0.89844(17) 1.2181(4) 0.59958(15) 0.0259(12) Uani 1 1 d . . . H2A H 0.9304 1.2259 0.6117 0.031 Uiso 1 1 calc R . . H2B H 0.8875 1.2327 0.6197 0.031 Uiso 1 1 calc R . . C3 C 0.87936(19) 1.3121(5) 0.56730(16) 0.0305(13) Uani 1 1 d . . . H3A H 0.8479 1.2974 0.5529 0.037 Uiso 1 1 calc R . . H3B H 0.8827 1.3899 0.5795 0.037 Uiso 1 1 calc R . . C4 C 0.9010(2) 1.3141(5) 0.53855(19) 0.0447(17) Uani 1 1 d . . . H4A H 0.8973 1.2379 0.5258 0.067 Uiso 1 1 calc R . . H4B H 0.9320 1.3308 0.5524 0.067 Uiso 1 1 calc R . . H4C H 0.8875 1.3747 0.5191 0.067 Uiso 1 1 calc R . . C5 C 0.9510(2) 0.8115(5) 0.66260(19) 0.0458(17) Uani 1 1 d . . . C9 C 0.79156(16) 0.9577(4) 0.65335(14) 0.0195(11) Uani 1 1 d . . . H9A H 0.8076 0.9259 0.6796 0.023 Uiso 1 1 calc R . . H9B H 0.7604 0.9430 0.6464 0.023 Uiso 1 1 calc R . . C10 C 0.80110(16) 0.7198(4) 0.63062(14) 0.0198(11) Uani 1 1 d . . . C11 C 0.77394(17) 0.6825(4) 0.64877(14) 0.0236(12) Uani 1 1 d . . . H11 H 0.7584 0.7384 0.6567 0.028 Uiso 1 1 calc R . . C12 C 0.7699(2) 0.5619(4) 0.65514(16) 0.0340(14) Uani 1 1 d . . . H12B H 0.7527 0.5376 0.6683 0.041 Uiso 1 1 calc R . . C13 C 0.7911(2) 0.4782(5) 0.64204(16) 0.0385(15) Uani 1 1 d . . . H13 H 0.7873 0.3975 0.6455 0.046 Uiso 1 1 calc R . . C14 C 0.8180(2) 0.5144(5) 0.62369(16) 0.0391(15) Uani 1 1 d . . . H14 H 0.8327 0.4577 0.6153 0.047 Uiso 1 1 calc R . . C15 C 0.82310(18) 0.6339(4) 0.61769(15) 0.0271(12) Uani 1 1 d . . . H15 H 0.8410 0.6574 0.6051 0.033 Uiso 1 1 calc R . . C16 C 0.76988(16) 0.9017(4) 0.57043(14) 0.0196(11) Uani 1 1 d . . . C17 C 0.72542(17) 0.9294(4) 0.55955(14) 0.0228(12) Uani 1 1 d . . . H17 H 0.7141 0.9338 0.5787 0.027 Uiso 1 1 calc R . . C18 C 0.69805(17) 0.9503(4) 0.52066(15) 0.0255(12) Uani 1 1 d . . . H18 H 0.6686 0.9714 0.5138 0.031 Uiso 1 1 calc R . . C19 C 0.71409(18) 0.9401(4) 0.49170(15) 0.0273(12) Uani 1 1 d . . . H19 H 0.6956 0.9541 0.4654 0.033 Uiso 1 1 calc R . . C20 C 0.75810(18) 0.9088(5) 0.50228(15) 0.0270(12) Uani 1 1 d . . . H20 H 0.7687 0.8996 0.4828 0.032 Uiso 1 1 calc R . . C21 C 0.78622(17) 0.8913(4) 0.54094(14) 0.0241(12) Uani 1 1 d . . . H21 H 0.8158 0.8728 0.5477 0.029 Uiso 1 1 calc R . . C22 C 0.78341(16) 1.1653(4) 0.69422(13) 0.0174(10) Uani 1 1 d . . . C23 C 0.80638(16) 1.2588(4) 0.71818(14) 0.0202(11) Uani 1 1 d . . . H23 H 0.8301 1.2932 0.7146 0.024 Uiso 1 1 calc R . . C24 C 0.79443(17) 1.3015(4) 0.74741(14) 0.0239(12) Uani 1 1 d . . . H24 H 0.8099 1.3648 0.7631 0.029 Uiso 1 1 calc R . . C25 C 0.75970(18) 1.2506(5) 0.75327(16) 0.0296(13) Uani 1 1 d . . . H25 H 0.7518 1.2786 0.7731 0.036 Uiso 1 1 calc R . . C26 C 0.73667(17) 1.1572(5) 0.72937(15) 0.0288(13) Uani 1 1 d . . . H26 H 0.7130 1.1234 0.7331 0.035 Uiso 1 1 calc R . . C27 C 0.74805(17) 1.1133(4) 0.70021(15) 0.0253(12) Uani 1 1 d . . . H27 H 0.7325 1.0499 0.6846 0.030 Uiso 1 1 calc R . . C28 C 0.76019(17) 1.1804(4) 0.61081(14) 0.0214(11) Uani 1 1 d . . . C29 C 0.71520(18) 1.1851(4) 0.60161(15) 0.0269(12) Uani 1 1 d . . . H29 H 0.7044 1.1522 0.6189 0.032 Uiso 1 1 calc R . . C30 C 0.68588(19) 1.2380(5) 0.56705(15) 0.0326(13) Uani 1 1 d . . . H30 H 0.6557 1.2409 0.5612 0.039 Uiso 1 1 calc R . . C31 C 0.7024(2) 1.2869(5) 0.54115(17) 0.0387(15) Uani 1 1 d . . . H31 H 0.6833 1.3236 0.5180 0.046 Uiso 1 1 calc R . . C32 C 0.7468(2) 1.2804(5) 0.54995(16) 0.0328(14) Uani 1 1 d . . . H32 H 0.7575 1.3126 0.5325 0.039 Uiso 1 1 calc R . . C33 C 0.77570(18) 1.2275(4) 0.58399(15) 0.0251(12) Uani 1 1 d . . . H33 H 0.8057 1.2230 0.5892 0.030 Uiso 1 1 calc R . . C34 C 1.03839(16) 1.1938(4) 0.64710(14) 0.0220(11) Uani 1 1 d . . . H34A H 1.0185 1.2600 0.6353 0.026 Uiso 1 1 calc R . . H34B H 1.0670 1.2143 0.6475 0.026 Uiso 1 1 calc R . . C35 C 0.99796(16) 1.1087(4) 0.56569(14) 0.0190(11) Uani 1 1 d . . . C36 C 0.96658(16) 1.0367(4) 0.53776(14) 0.0223(11) Uani 1 1 d . . . H36 H 0.9556 0.9705 0.5459 0.027 Uiso 1 1 calc R . . C37 C 0.95140(17) 1.0624(4) 0.49785(14) 0.0230(12) Uani 1 1 d . . . H37 H 0.9300 1.0143 0.4794 0.028 Uiso 1 1 calc R . . C38 C 0.96830(17) 1.1601(5) 0.48566(16) 0.0263(12) Uani 1 1 d . . . H38 H 0.9582 1.1780 0.4590 0.032 Uiso 1 1 calc R . . C39 C 1.00030(18) 1.2309(5) 0.51334(16) 0.0300(13) Uani 1 1 d . . . H39 H 1.0118 1.2957 0.5051 0.036 Uiso 1 1 calc R . . C40 C 1.01528(16) 1.2062(4) 0.55320(16) 0.0251(12) Uani 1 1 d . . . H40 H 1.0367 1.2542 0.5716 0.030 Uiso 1 1 calc R . . C41 C 1.06220(16) 0.9615(4) 0.62485(13) 0.0198(11) Uani 1 1 d . . . C42 C 1.05887(17) 0.8461(4) 0.63694(15) 0.0258(12) Uani 1 1 d . . . H42 H 1.0338 0.8228 0.6406 0.031 Uiso 1 1 calc R . . C43 C 1.09339(18) 0.7649(5) 0.64365(15) 0.0279(12) Uani 1 1 d . . . H43 H 1.0915 0.6879 0.6520 0.034 Uiso 1 1 calc R . . C44 C 1.13012(18) 0.7996(5) 0.63780(15) 0.0300(13) Uani 1 1 d . . . H44 H 1.1532 0.7459 0.6425 0.036 Uiso 1 1 calc R . . C45 C 1.13312(18) 0.9139(5) 0.62494(16) 0.0311(13) Uani 1 1 d . . . H45 H 1.1579 0.9361 0.6207 0.037 Uiso 1 1 calc R . . C46 C 1.09926(17) 0.9952(5) 0.61835(15) 0.0256(12) Uani 1 1 d . . . H46 H 1.1012 1.0717 0.6096 0.031 Uiso 1 1 calc R . . C47 C 1.08317(18) 1.0556(4) 0.71743(14) 0.0267(12) Uani 1 1 d . . . C48 C 1.0716(2) 0.9599(5) 0.73530(17) 0.0422(16) Uani 1 1 d . . . H48 H 1.0450 0.9604 0.7383 0.051 Uiso 1 1 calc R . . C49 C 1.1004(3) 0.8639(6) 0.74857(19) 0.059(2) Uani 1 1 d . . . H49 H 1.0928 0.7994 0.7603 0.071 Uiso 1 1 calc R . . C50 C 1.1399(3) 0.8630(6) 0.74459(18) 0.0514(19) Uani 1 1 d . . . H50 H 1.1585 0.7973 0.7532 0.062 Uiso 1 1 calc R . . C51 C 1.15213(19) 0.9582(5) 0.72807(15) 0.0342(14) Uani 1 1 d . . . H51 H 1.1793 0.9580 0.7261 0.041 Uiso 1 1 calc R . . C52 C 1.12385(18) 1.0545(5) 0.71434(14) 0.0276(12) Uani 1 1 d . . . H52 H 1.1320 1.1188 0.7030 0.033 Uiso 1 1 calc R . . C53 C 1.07026(16) 1.3086(4) 0.72403(14) 0.0209(11) Uani 1 1 d . . . C54 C 1.06883(18) 1.3246(5) 0.76074(15) 0.0289(13) Uani 1 1 d . . . H54 H 1.0540 1.2697 0.7697 0.035 Uiso 1 1 calc R . . C55 C 1.0891(2) 1.4203(5) 0.78340(16) 0.0349(14) Uani 1 1 d . . . H55 H 1.0885 1.4296 0.8080 0.042 Uiso 1 1 calc R . . C56 C 1.11044(19) 1.5039(5) 0.77008(16) 0.0342(14) Uani 1 1 d . . . H56 H 1.1242 1.5691 0.7858 0.041 Uiso 1 1 calc R . . C57 C 1.11145(17) 1.4909(5) 0.73361(16) 0.0274(12) Uani 1 1 d . . . H57 H 1.1255 1.5478 0.7245 0.033 Uiso 1 1 calc R . . C58 C 1.09160(17) 1.3929(5) 0.71052(15) 0.0275(12) Uani 1 1 d . . . H58 H 1.0925 1.3835 0.6860 0.033 Uiso 1 1 calc R . . C59 C 0.88640(16) 0.7586(4) 0.50164(14) 0.0204(11) Uani 1 1 d . . . C60 C 0.86067(16) 0.8562(4) 0.48703(15) 0.0224(11) Uani 1 1 d . . . H60 H 0.8571 0.9113 0.5042 0.027 Uiso 1 1 calc R . . C61 C 0.83932(17) 0.8746(4) 0.44615(14) 0.0227(11) Uani 1 1 d . . . H61 H 0.8223 0.9427 0.4365 0.027 Uiso 1 1 calc R . . C62 C 0.84330(16) 0.7944(4) 0.42059(14) 0.0203(11) Uani 1 1 d . . . H62 H 0.8284 0.8074 0.3937 0.024 Uiso 1 1 calc R . . C63 C 0.86990(16) 0.6902(4) 0.43423(14) 0.0197(11) Uani 1 1 d . . . C64 C 0.89266(16) 0.6725(4) 0.47585(14) 0.0188(11) Uani 1 1 d . . . C65 C 0.91906(16) 0.5687(4) 0.48981(15) 0.0238(12) Uani 1 1 d . . . H65 H 0.9343 0.5566 0.5168 0.029 Uiso 1 1 calc R . . C66 C 0.92217(18) 0.4869(4) 0.46402(15) 0.0268(12) Uani 1 1 d . . . H66 H 0.9397 0.4196 0.4736 0.032 Uiso 1 1 calc R . . C67 C 0.89939(18) 0.5030(5) 0.42333(15) 0.0270(12) Uani 1 1 d . . . H67 H 0.9017 0.4458 0.4061 0.032 Uiso 1 1 calc R . . C68 C 0.87391(16) 0.6017(4) 0.40867(14) 0.0194(11) Uani 1 1 d . . . H101 H 0.947(2) 1.097(5) 0.6877(18) 0.05(2) Uiso 1 1 d . . . H102 H 0.9022(19) 1.095(4) 0.6745(15) 0.024(16) Uiso 1 1 d . . . C8 C 0.9777(4) 0.4869(13) 0.6649(4) 0.159(5) Uani 1 1 d . . . C7 C 0.9794(4) 0.6019(10) 0.6856(4) 0.030(3) Uiso 0.50 1 d P A 1 C7A C 1.0017(8) 0.6023(18) 0.7021(6) 0.022(5) Uiso 0.25 1 d P A 2 C7B C 0.9837(9) 0.687(2) 0.7180(8) 0.052(7) Uiso 0.25 1 d P B 3 C6 C 0.9534(4) 0.6943(9) 0.6507(3) 0.028(2) Uiso 0.50 1 d P A 1 C6A C 0.9825(6) 0.8130(16) 0.6933(6) 0.018(4) Uiso 0.25 1 d P A 2 C6B C 0.9382(9) 0.749(2) 0.6824(8) 0.051(7) Uiso 0.25 1 d P B 3 O12 O 0.5132(5) 0.9934(13) 0.1004(4) 0.144(7) Uiso 0.567(14) 1 d P C 1 O12A O 0.4760(4) 1.0417(10) 0.1054(3) 0.065(5) Uiso 0.433(14) 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01855(19) 0.01857(19) 0.01907(19) -0.00023(14) 0.01072(15) -0.00088(14) S1 0.0243(7) 0.0203(7) 0.0193(7) -0.0013(5) 0.0106(6) -0.0010(5) S2 0.0218(7) 0.0250(7) 0.0208(7) -0.0027(5) 0.0121(6) -0.0041(5) P1 0.0195(7) 0.0182(7) 0.0205(7) -0.0007(5) 0.0114(6) -0.0025(5) P2 0.0227(7) 0.0187(7) 0.0237(7) -0.0030(6) 0.0145(6) -0.0024(5) P3 0.0169(7) 0.0247(7) 0.0215(7) -0.0044(6) 0.0103(6) -0.0025(5) P4 0.0230(8) 0.0298(8) 0.0259(8) -0.0071(6) 0.0141(6) -0.0072(6) O1 0.020(2) 0.030(2) 0.024(2) -0.0048(17) 0.0117(18) -0.0048(19) O2 0.0195(19) 0.0262(19) 0.0220(19) -0.0051(15) 0.0129(16) -0.0037(14) O3 0.026(2) 0.0237(19) 0.029(2) -0.0036(15) 0.0176(17) -0.0046(15) O4 0.023(2) 0.0264(19) 0.026(2) -0.0031(15) 0.0161(17) -0.0017(15) O5 0.029(2) 0.050(2) 0.034(2) -0.0153(19) 0.0205(19) -0.0156(18) O6 0.033(2) 0.024(2) 0.0228(19) -0.0027(15) 0.0134(17) 0.0064(16) O7 0.041(2) 0.023(2) 0.027(2) -0.0012(16) 0.0172(19) -0.0062(16) O8 0.021(2) 0.034(2) 0.028(2) -0.0019(16) 0.0093(17) -0.0008(16) O9 0.022(2) 0.031(2) 0.0243(19) -0.0030(16) 0.0133(17) -0.0040(15) O10 0.032(2) 0.0244(19) 0.0241(19) -0.0065(15) 0.0158(17) -0.0042(15) O11 0.027(2) 0.026(2) 0.0216(19) -0.0011(15) 0.0143(17) -0.0044(15) C1 0.021(3) 0.023(3) 0.020(3) 0.003(2) 0.008(2) 0.004(2) C2 0.026(3) 0.022(3) 0.034(3) 0.004(2) 0.016(3) 0.003(2) C3 0.037(3) 0.023(3) 0.039(3) 0.003(2) 0.023(3) 0.001(2) C4 0.045(4) 0.043(4) 0.063(4) 0.032(3) 0.039(4) 0.021(3) C5 0.040(4) 0.039(4) 0.051(4) 0.026(3) 0.012(3) 0.016(3) C9 0.022(3) 0.019(3) 0.020(3) -0.002(2) 0.011(2) 0.002(2) C10 0.018(3) 0.021(3) 0.021(3) 0.000(2) 0.009(2) 0.001(2) C11 0.022(3) 0.022(3) 0.023(3) 0.004(2) 0.006(2) 0.002(2) C12 0.052(4) 0.019(3) 0.029(3) 0.007(2) 0.014(3) -0.005(3) C13 0.066(5) 0.024(3) 0.026(3) 0.002(2) 0.019(3) -0.005(3) C14 0.062(4) 0.024(3) 0.028(3) 0.002(3) 0.016(3) 0.018(3) C15 0.034(3) 0.026(3) 0.022(3) -0.006(2) 0.011(3) 0.001(2) C16 0.024(3) 0.013(2) 0.023(3) -0.002(2) 0.010(2) -0.003(2) C17 0.027(3) 0.022(3) 0.023(3) 0.000(2) 0.013(2) -0.001(2) C18 0.020(3) 0.022(3) 0.032(3) 0.000(2) 0.008(2) 0.000(2) C19 0.027(3) 0.027(3) 0.022(3) 0.003(2) 0.004(2) -0.004(2) C20 0.031(3) 0.035(3) 0.019(3) 0.000(2) 0.014(3) -0.005(2) C21 0.026(3) 0.023(3) 0.025(3) 0.001(2) 0.013(3) -0.002(2) C22 0.021(3) 0.019(3) 0.016(3) -0.005(2) 0.011(2) -0.001(2) C23 0.019(3) 0.023(3) 0.021(3) -0.001(2) 0.011(2) -0.001(2) C24 0.026(3) 0.026(3) 0.019(3) -0.008(2) 0.010(2) -0.003(2) C25 0.035(3) 0.033(3) 0.027(3) -0.007(2) 0.018(3) -0.001(2) C26 0.022(3) 0.037(3) 0.035(3) -0.005(3) 0.018(3) -0.007(2) C27 0.027(3) 0.027(3) 0.027(3) -0.006(2) 0.017(3) -0.003(2) C28 0.025(3) 0.017(3) 0.026(3) -0.003(2) 0.015(2) 0.001(2) C29 0.030(3) 0.022(3) 0.030(3) 0.003(2) 0.013(3) 0.004(2) C30 0.028(3) 0.043(4) 0.029(3) -0.005(3) 0.013(3) 0.008(3) C31 0.058(5) 0.031(3) 0.026(3) 0.000(3) 0.016(3) 0.009(3) C32 0.049(4) 0.031(3) 0.026(3) -0.002(3) 0.023(3) -0.005(3) C33 0.034(3) 0.019(3) 0.028(3) -0.003(2) 0.019(3) -0.004(2) C34 0.017(3) 0.022(3) 0.029(3) -0.004(2) 0.011(2) -0.001(2) C35 0.019(3) 0.018(3) 0.023(3) -0.002(2) 0.011(2) 0.003(2) C36 0.025(3) 0.020(3) 0.028(3) -0.001(2) 0.017(2) -0.001(2) C37 0.023(3) 0.028(3) 0.020(3) -0.006(2) 0.011(2) 0.001(2) C38 0.020(3) 0.031(3) 0.028(3) 0.004(2) 0.010(3) 0.008(2) C39 0.034(3) 0.025(3) 0.039(3) 0.012(3) 0.023(3) 0.003(2) C40 0.017(3) 0.019(3) 0.038(3) 0.001(2) 0.011(3) 0.001(2) C41 0.016(3) 0.028(3) 0.013(2) 0.001(2) 0.005(2) 0.000(2) C42 0.026(3) 0.027(3) 0.027(3) 0.000(2) 0.014(3) 0.003(2) C43 0.037(3) 0.023(3) 0.028(3) 0.001(2) 0.016(3) 0.004(2) C44 0.032(3) 0.034(3) 0.021(3) -0.005(2) 0.009(3) 0.013(2) C45 0.025(3) 0.038(3) 0.038(3) -0.003(3) 0.021(3) 0.002(2) C46 0.026(3) 0.027(3) 0.027(3) -0.002(2) 0.014(3) 0.000(2) C47 0.035(3) 0.026(3) 0.021(3) -0.006(2) 0.013(3) -0.008(2) C48 0.067(5) 0.036(4) 0.040(4) 0.001(3) 0.038(4) -0.005(3) C49 0.111(7) 0.031(4) 0.046(4) 0.010(3) 0.044(5) 0.001(4) C50 0.085(6) 0.032(4) 0.036(4) 0.006(3) 0.023(4) 0.012(3) C51 0.031(3) 0.038(4) 0.023(3) -0.009(3) 0.001(3) 0.000(3) C52 0.029(3) 0.028(3) 0.020(3) -0.002(2) 0.004(2) -0.004(2) C53 0.018(3) 0.026(3) 0.021(3) -0.003(2) 0.010(2) -0.002(2) C54 0.031(3) 0.027(3) 0.030(3) 0.004(2) 0.015(3) 0.003(2) C55 0.048(4) 0.038(4) 0.023(3) -0.006(3) 0.019(3) 0.004(3) C56 0.044(4) 0.025(3) 0.031(3) -0.005(3) 0.013(3) -0.001(3) C57 0.023(3) 0.023(3) 0.040(3) -0.003(2) 0.015(3) -0.003(2) C58 0.024(3) 0.035(3) 0.024(3) -0.001(2) 0.011(3) -0.001(2) C59 0.022(3) 0.020(3) 0.023(3) 0.004(2) 0.013(2) -0.001(2) C60 0.022(3) 0.025(3) 0.026(3) -0.004(2) 0.016(2) -0.002(2) C61 0.027(3) 0.020(3) 0.024(3) 0.004(2) 0.014(3) 0.003(2) C62 0.024(3) 0.020(3) 0.021(3) 0.003(2) 0.014(2) -0.004(2) C63 0.020(3) 0.020(3) 0.026(3) -0.002(2) 0.016(2) -0.007(2) C64 0.024(3) 0.018(3) 0.021(3) -0.001(2) 0.015(2) -0.005(2) C65 0.019(3) 0.027(3) 0.024(3) 0.004(2) 0.008(2) -0.002(2) C66 0.033(3) 0.020(3) 0.030(3) 0.000(2) 0.015(3) 0.006(2) C67 0.036(3) 0.026(3) 0.024(3) -0.003(2) 0.017(3) 0.000(2) C68 0.017(3) 0.023(3) 0.022(3) -0.004(2) 0.011(2) -0.005(2) C8 0.123(11) 0.194(14) 0.160(12) 0.048(11) 0.058(10) 0.026(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C5 2.104(6) . ? Sn1 C1 2.121(5) . ? Sn1 O2 2.182(3) . ? Sn1 O1 2.200(4) . ? Sn1 O4 2.227(3) . ? Sn1 O6 2.265(3) . ? S1 O8 1.439(4) . ? S1 O7 1.445(3) . ? S1 O6 1.485(3) . ? S1 C59 1.780(5) . ? S2 O10 1.446(3) . ? S2 O11 1.447(3) . ? S2 O9 1.452(3) . ? S2 C68 1.780(5) . ? P1 O2 1.498(3) . ? P1 C10 1.787(5) . ? P1 C16 1.788(5) . ? P1 C9 1.798(5) . ? P2 O3 1.494(3) . ? P2 C22 1.797(4) . ? P2 C28 1.800(5) . ? P2 C9 1.810(5) . ? P3 O4 1.499(3) . ? P3 C41 1.794(5) . ? P3 C35 1.795(5) . ? P3 C34 1.814(5) . ? P4 O5 1.479(4) . ? P4 C53 1.798(5) . ? P4 C47 1.801(6) . ? P4 C34 1.817(5) . ? C1 C2 1.524(7) . ? C2 C3 1.528(7) . ? C3 C4 1.510(7) . ? C5 C6A 1.19(2) . ? C5 C6B 1.21(3) . ? C5 C6 1.400(11) . ? C10 C11 1.390(7) . ? C10 C15 1.406(7) . ? C11 C12 1.390(7) . ? C12 C13 1.374(8) . ? C13 C14 1.385(8) . ? C14 C15 1.382(7) . ? C16 C17 1.391(7) . ? C16 C21 1.411(6) . ? C17 C18 1.378(7) . ? C18 C19 1.386(7) . ? C19 C20 1.389(7) . ? C20 C21 1.371(7) . ? C22 C23 1.385(6) . ? C22 C27 1.403(7) . ? C23 C24 1.385(6) . ? C24 C25 1.378(7) . ? C25 C26 1.384(7) . ? C26 C27 1.376(7) . ? C28 C29 1.385(7) . ? C28 C33 1.398(7) . ? C29 C30 1.388(7) . ? C30 C31 1.399(8) . ? C31 C32 1.369(8) . ? C32 C33 1.372(7) . ? C35 C36 1.389(7) . ? C35 C40 1.400(6) . ? C36 C37 1.389(7) . ? C37 C38 1.388(7) . ? C38 C39 1.386(7) . ? C39 C40 1.386(7) . ? C41 C42 1.390(7) . ? C41 C46 1.395(7) . ? C42 C43 1.401(7) . ? C43 C44 1.375(7) . ? C44 C45 1.387(7) . ? C45 C46 1.386(7) . ? C47 C52 1.396(7) . ? C47 C48 1.397(7) . ? C48 C49 1.388(9) . ? C49 C50 1.375(10) . ? C50 C51 1.374(8) . ? C51 C52 1.383(7) . ? C53 C58 1.391(7) . ? C53 C54 1.397(7) . ? C54 C55 1.361(7) . ? C55 C56 1.383(8) . ? C56 C57 1.378(7) . ? C57 C58 1.384(7) . ? C59 C60 1.357(7) . ? C59 C64 1.435(6) . ? C60 C61 1.406(7) . ? C61 C62 1.354(6) . ? C62 C63 1.426(7) . ? C63 C68 1.419(6) . ? C63 C64 1.432(7) . ? C64 C65 1.421(7) . ? C65 C66 1.361(7) . ? C66 C67 1.400(7) . ? C67 C68 1.364(7) . ? C8 C7 1.491(17) . ? C8 C7A 1.82(3) . ? C7 C6 1.609(15) . ? C7B C6B 1.70(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Sn1 C1 175.3(2) . . ? C5 Sn1 O2 91.4(2) . . ? C1 Sn1 O2 93.18(16) . . ? C5 Sn1 O1 87.6(2) . . ? C1 Sn1 O1 94.09(17) . . ? O2 Sn1 O1 83.74(13) . . ? C5 Sn1 O4 86.6(2) . . ? C1 Sn1 O4 88.83(17) . . ? O2 Sn1 O4 177.58(12) . . ? O1 Sn1 O4 94.78(14) . . ? C5 Sn1 O6 94.5(2) . . ? C1 Sn1 O6 84.61(16) . . ? O2 Sn1 O6 86.09(12) . . ? O1 Sn1 O6 169.66(14) . . ? O4 Sn1 O6 95.45(12) . . ? O8 S1 O7 115.3(2) . . ? O8 S1 O6 112.5(2) . . ? O7 S1 O6 111.5(2) . . ? O8 S1 C59 106.7(2) . . ? O7 S1 C59 107.0(2) . . ? O6 S1 C59 102.6(2) . . ? O10 S2 O11 114.3(2) . . ? O10 S2 O9 112.4(2) . . ? O11 S2 O9 112.9(2) . . ? O10 S2 C68 106.2(2) . . ? O11 S2 C68 104.9(2) . . ? O9 S2 C68 105.1(2) . . ? O2 P1 C10 109.6(2) . . ? O2 P1 C16 111.2(2) . . ? C10 P1 C16 107.9(2) . . ? O2 P1 C9 112.4(2) . . ? C10 P1 C9 105.7(2) . . ? C16 P1 C9 109.9(2) . . ? O3 P2 C22 112.8(2) . . ? O3 P2 C28 111.1(2) . . ? C22 P2 C28 106.4(2) . . ? O3 P2 C9 113.8(2) . . ? C22 P2 C9 104.6(2) . . ? C28 P2 C9 107.6(2) . . ? O4 P3 C41 110.0(2) . . ? O4 P3 C35 111.7(2) . . ? C41 P3 C35 106.5(2) . . ? O4 P3 C34 111.0(2) . . ? C41 P3 C34 109.1(2) . . ? C35 P3 C34 108.3(2) . . ? O5 P4 C53 110.7(2) . . ? O5 P4 C47 112.3(2) . . ? C53 P4 C47 107.2(2) . . ? O5 P4 C34 113.6(2) . . ? C53 P4 C34 107.4(2) . . ? C47 P4 C34 105.3(2) . . ? P1 O2 Sn1 168.3(2) . . ? P3 O4 Sn1 163.9(2) . . ? S1 O6 Sn1 140.1(2) . . ? C2 C1 Sn1 117.4(3) . . ? C1 C2 C3 113.0(4) . . ? C4 C3 C2 113.8(4) . . ? C6A C5 C6B 79.1(16) . . ? C6A C5 C6 100.2(11) . . ? C6B C5 C6 74.2(13) . . ? C6A C5 Sn1 131.3(10) . . ? C6B C5 Sn1 127.9(14) . . ? C6 C5 Sn1 124.3(6) . . ? P1 C9 P2 119.0(3) . . ? C11 C10 C15 119.1(5) . . ? C11 C10 P1 123.3(4) . . ? C15 C10 P1 117.5(4) . . ? C10 C11 C12 120.2(5) . . ? C13 C12 C11 120.4(5) . . ? C12 C13 C14 119.9(5) . . ? C15 C14 C13 120.7(5) . . ? C14 C15 C10 119.7(5) . . ? C17 C16 C21 119.1(5) . . ? C17 C16 P1 123.1(4) . . ? C21 C16 P1 117.8(4) . . ? C18 C17 C16 120.5(5) . . ? C17 C18 C19 120.4(5) . . ? C18 C19 C20 119.3(5) . . ? C21 C20 C19 121.1(5) . . ? C20 C21 C16 119.5(5) . . ? C23 C22 C27 119.1(4) . . ? C23 C22 P2 118.2(4) . . ? C27 C22 P2 122.7(4) . . ? C24 C23 C22 120.7(5) . . ? C25 C24 C23 120.3(5) . . ? C24 C25 C26 119.2(5) . . ? C27 C26 C25 121.4(5) . . ? C26 C27 C22 119.3(5) . . ? C29 C28 C33 118.6(5) . . ? C29 C28 P2 122.9(4) . . ? C33 C28 P2 118.4(4) . . ? C28 C29 C30 121.3(5) . . ? C29 C30 C31 118.9(5) . . ? C32 C31 C30 119.8(5) . . ? C31 C32 C33 121.3(5) . . ? C32 C33 C28 120.1(5) . . ? P3 C34 P4 114.6(3) . . ? C36 C35 C40 119.3(5) . . ? C36 C35 P3 117.2(4) . . ? C40 C35 P3 123.3(4) . . ? C35 C36 C37 120.8(5) . . ? C38 C37 C36 119.6(5) . . ? C39 C38 C37 119.8(5) . . ? C40 C39 C38 120.7(5) . . ? C39 C40 C35 119.7(5) . . ? C42 C41 C46 120.0(5) . . ? C42 C41 P3 118.9(4) . . ? C46 C41 P3 121.1(4) . . ? C41 C42 C43 119.8(5) . . ? C44 C43 C42 119.8(5) . . ? C43 C44 C45 120.6(5) . . ? C46 C45 C44 120.2(5) . . ? C45 C46 C41 119.6(5) . . ? C52 C47 C48 119.5(5) . . ? C52 C47 P4 121.5(4) . . ? C48 C47 P4 118.9(4) . . ? C49 C48 C47 119.0(6) . . ? C50 C49 C48 120.8(6) . . ? C51 C50 C49 120.6(6) . . ? C50 C51 C52 119.7(6) . . ? C51 C52 C47 120.4(5) . . ? C58 C53 C54 119.3(5) . . ? C58 C53 P4 124.4(4) . . ? C54 C53 P4 116.3(4) . . ? C55 C54 C53 120.2(5) . . ? C54 C55 C56 120.5(5) . . ? C57 C56 C55 120.1(5) . . ? C56 C57 C58 119.9(5) . . ? C57 C58 C53 119.9(5) . . ? C60 C59 C64 120.9(5) . . ? C60 C59 S1 120.1(4) . . ? C64 C59 S1 118.9(4) . . ? C59 C60 C61 120.5(5) . . ? C62 C61 C60 120.8(5) . . ? C61 C62 C63 121.2(5) . . ? C68 C63 C62 123.3(5) . . ? C68 C63 C64 118.4(4) . . ? C62 C63 C64 118.3(4) . . ? C65 C64 C63 118.8(4) . . ? C65 C64 C59 122.9(4) . . ? C63 C64 C59 118.3(4) . . ? C66 C65 C64 120.5(5) . . ? C65 C66 C67 120.9(5) . . ? C68 C67 C66 120.6(5) . . ? C67 C68 C63 120.9(5) . . ? C67 C68 S2 118.4(4) . . ? C63 C68 S2 120.7(4) . . ? C7 C8 C7A 23.3(8) . . ? C8 C7 C6 104.4(10) . . ? C5 C6 C7 115.5(8) . . ? C5 C6B C7B 107(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.835 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.141 data_16octb _database_code_depnum_ccdc_archive 'CCDC 766498' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'organotin sulfonate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 O10 P4 S2 Sn' _chemical_formula_weight 1391.89 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' P P 0.1023 0.0942 '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)/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 15.154(5) _cell_length_b 11.657(5) _cell_length_c 19.051(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 112.254(5) _cell_angle_gamma 90.000(5) _cell_volume 3114.7(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3839 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.54 _exptl_crystal_description block-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.959 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15603 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5471 _reflns_number_gt 4532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5471 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1087 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.45411(6) 0.12560(7) 0.14634(5) 0.0167(2) Uani 1 1 d . . . O3 O 0.50337(16) 0.0351(2) 0.19948(13) 0.0191(5) Uani 1 1 d . . . O4 O 0.35140(16) 0.1127(2) 0.11598(13) 0.0226(6) Uani 1 1 d . . . O5 O 0.48516(18) 0.2400(2) 0.17699(14) 0.0253(6) Uani 1 1 d . . . C32 C 0.4922(2) 0.1115(3) 0.06871(18) 0.0159(7) Uani 1 1 d . . . C33 C 0.5368(2) 0.2027(3) 0.05086(19) 0.0200(8) Uani 1 1 d . . . H33 H 0.5416 0.2724 0.0757 0.024 Uiso 1 1 calc R . . C34 C 0.4244(2) -0.1904(3) 0.00526(19) 0.0206(8) Uani 1 1 d . . . H34 H 0.3938 -0.2524 0.0168 0.025 Uiso 1 1 calc R . . C35 C 0.4309(2) -0.0899(3) 0.04275(18) 0.0177(7) Uani 1 1 d . . . H35 H 0.4027 -0.0831 0.0782 0.021 Uiso 1 1 calc R . . C36 C 0.4802(2) 0.0051(3) 0.02847(19) 0.0149(7) Uani 1 1 d . . . Sn1 Sn 1.0000 1.0000 0.0000 0.01436(13) Uani 1 2 d S . . P1 P 1.06662(6) 0.97983(7) 0.19175(5) 0.0146(2) Uani 1 1 d . . . P2 P 0.88556(6) 0.85187(7) 0.09429(5) 0.0151(2) Uani 1 1 d . . . O1 O 1.05879(16) 1.0472(2) 0.12150(12) 0.0175(5) Uani 1 1 d . . . O2 O 0.88968(15) 0.90389(19) 0.02236(12) 0.0170(5) Uani 1 1 d . . . C1 C 0.9107(2) 1.1470(3) -0.02716(18) 0.0167(7) Uani 1 1 d . . . C2 C 0.9487(3) 1.2565(3) -0.01077(19) 0.0228(8) Uani 1 1 d . . . H2 H 1.0133 1.2656 0.0181 0.027 Uiso 1 1 calc R . . C3 C 0.8921(3) 1.3525(3) -0.0367(2) 0.0268(9) Uani 1 1 d . . . H3 H 0.9183 1.4255 -0.0245 0.032 Uiso 1 1 calc R . . C4 C 0.7959(3) 1.3394(3) -0.0808(2) 0.0265(9) Uani 1 1 d . . . H4 H 0.7580 1.4037 -0.0999 0.032 Uiso 1 1 calc R . . C5 C 0.7568(2) 1.2312(3) -0.09638(19) 0.0242(8) Uani 1 1 d . . . H5 H 0.6921 1.2226 -0.1250 0.029 Uiso 1 1 calc R . . C6 C 0.8137(2) 1.1347(3) -0.06945(19) 0.0201(8) Uani 1 1 d . . . H6 H 0.7868 1.0619 -0.0798 0.024 Uiso 1 1 calc R . . C7 C 1.0187(2) 1.0629(3) 0.24807(18) 0.0182(7) Uani 1 1 d . . . C8 C 0.9861(3) 1.0130(3) 0.3002(2) 0.0187(8) Uani 1 1 d . . . H8 H 0.9895 0.9341 0.3078 0.022 Uiso 1 1 calc R . . C9 C 0.9485(3) 1.0834(3) 0.3409(2) 0.0252(8) Uani 1 1 d . . . H9 H 0.9251 1.0508 0.3750 0.030 Uiso 1 1 calc R . . C10 C 0.9452(2) 1.2012(3) 0.3314(2) 0.0252(8) Uani 1 1 d . . . H10 H 0.9189 1.2469 0.3585 0.030 Uiso 1 1 calc R . . C11 C 0.9807(2) 1.2510(3) 0.2819(2) 0.0271(9) Uani 1 1 d . . . H11 H 0.9806 1.3304 0.2768 0.033 Uiso 1 1 calc R . . C12 C 1.0170(2) 1.1816(3) 0.2395(2) 0.0212(8) Uani 1 1 d . . . H12 H 1.0400 1.2147 0.2054 0.025 Uiso 1 1 calc R . . C13 C 1.1880(2) 0.9448(3) 0.24876(17) 0.0156(7) Uani 1 1 d . . . C14 C 1.2603(3) 1.0082(3) 0.2381(2) 0.0195(8) Uani 1 1 d . . . H14 H 1.2453 1.0647 0.2009 0.023 Uiso 1 1 calc R . . C15 C 1.3548(3) 0.9857(3) 0.2837(2) 0.0231(8) Uani 1 1 d . . . H15 H 1.4034 1.0275 0.2773 0.028 Uiso 1 1 calc R . . C16 C 1.3763(2) 0.9014(3) 0.33849(19) 0.0220(8) Uani 1 1 d . . . H16 H 1.4397 0.8869 0.3688 0.026 Uiso 1 1 calc R . . C17 C 1.3047(2) 0.8378(3) 0.3490(2) 0.0217(8) Uani 1 1 d . . . H17 H 1.3199 0.7807 0.3858 0.026 Uiso 1 1 calc R . . C18 C 1.2104(2) 0.8604(3) 0.30422(19) 0.0195(7) Uani 1 1 d . . . H18 H 1.1620 0.8189 0.3113 0.023 Uiso 1 1 calc R . . C19 C 0.8136(2) 0.9357(3) 0.13010(19) 0.0183(7) Uani 1 1 d . . . C20 C 0.8074(2) 1.0542(3) 0.11944(19) 0.0204(8) Uani 1 1 d . . . H20 H 0.8353 1.0887 0.0889 0.024 Uiso 1 1 calc R . . C21 C 0.7599(2) 1.1206(3) 0.1543(2) 0.0262(9) Uani 1 1 d . . . H21 H 0.7571 1.1998 0.1480 0.031 Uiso 1 1 calc R . . C22 C 0.7170(3) 1.0689(4) 0.1982(2) 0.0300(9) Uani 1 1 d . . . H22 H 0.6852 1.1136 0.2216 0.036 Uiso 1 1 calc R . . C23 C 0.7208(3) 0.9520(4) 0.2077(2) 0.0326(10) Uani 1 1 d . . . H23 H 0.6901 0.9181 0.2364 0.039 Uiso 1 1 calc R . . C24 C 0.7696(3) 0.8842(3) 0.1751(2) 0.0262(9) Uani 1 1 d . . . H24 H 0.7733 0.8053 0.1829 0.031 Uiso 1 1 calc R . . C25 C 0.8372(2) 0.7101(3) 0.07893(18) 0.0174(7) Uani 1 1 d . . . C26 C 0.8769(2) 0.6186(3) 0.12831(19) 0.0201(8) Uani 1 1 d . . . H26 H 0.9334 0.6290 0.1701 0.024 Uiso 1 1 calc R . . C27 C 0.8325(3) 0.5132(3) 0.1153(2) 0.0253(9) Uani 1 1 d . . . H27 H 0.8595 0.4520 0.1476 0.030 Uiso 1 1 calc R . . C28 C 0.7466(3) 0.4988(3) 0.0531(2) 0.0279(9) Uani 1 1 d . . . H28 H 0.7160 0.4280 0.0447 0.033 Uiso 1 1 calc R . . C29 C 0.7071(3) 0.5886(3) 0.0042(2) 0.0296(9) Uani 1 1 d . . . H29 H 0.6504 0.5778 -0.0373 0.036 Uiso 1 1 calc R . . C30 C 0.7513(2) 0.6944(3) 0.01657(19) 0.0221(8) Uani 1 1 d . . . H30 H 0.7242 0.7550 -0.0163 0.027 Uiso 1 1 calc R . . C31 C 1.0033(2) 0.8447(3) 0.16854(18) 0.0147(7) Uani 1 1 d . . . H31A H 0.9974 0.8146 0.2140 0.018 Uiso 1 1 calc R . . H31B H 1.0414 0.7908 0.1532 0.018 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 S1 0.0204(5) 0.0154(5) 0.0159(4) -0.0015(3) 0.0090(3) 0.0012(3) O3 0.0222(13) 0.0215(13) 0.0144(12) 0.0006(10) 0.0079(10) 0.0018(10) O4 0.0181(13) 0.0308(15) 0.0204(13) 0.0018(11) 0.0091(10) 0.0043(11) O5 0.0369(15) 0.0181(14) 0.0273(14) -0.0063(11) 0.0192(12) -0.0024(11) C32 0.0183(17) 0.0180(18) 0.0121(16) -0.0002(13) 0.0066(14) 0.0020(14) C33 0.0250(19) 0.0169(19) 0.0179(18) 0.0007(14) 0.0079(15) 0.0020(15) C34 0.0268(19) 0.0169(19) 0.0177(18) 0.0031(14) 0.0080(15) -0.0015(15) C35 0.0182(18) 0.0204(19) 0.0147(17) -0.0014(14) 0.0066(14) -0.0025(14) C36 0.0128(17) 0.0173(19) 0.0116(17) -0.0006(13) 0.0013(14) 0.0032(13) Sn1 0.0143(2) 0.0154(2) 0.0132(2) 0.00274(12) 0.00505(14) 0.00018(12) P1 0.0144(5) 0.0164(5) 0.0125(5) 0.0011(3) 0.0044(4) -0.0015(3) P2 0.0151(4) 0.0157(5) 0.0141(4) 0.0019(3) 0.0051(4) -0.0008(3) O1 0.0204(12) 0.0175(13) 0.0132(12) 0.0023(10) 0.0049(10) -0.0014(10) O2 0.0150(12) 0.0189(13) 0.0149(12) 0.0025(10) 0.0032(9) -0.0017(10) C1 0.0175(18) 0.0217(19) 0.0128(17) 0.0052(14) 0.0080(14) 0.0045(14) C2 0.0222(19) 0.027(2) 0.0174(18) -0.0016(15) 0.0059(15) 0.0022(16) C3 0.031(2) 0.019(2) 0.029(2) 0.0009(16) 0.0093(17) 0.0005(16) C4 0.028(2) 0.028(2) 0.028(2) 0.0087(16) 0.0155(17) 0.0107(17) C5 0.0176(18) 0.033(2) 0.0199(19) 0.0041(16) 0.0049(15) 0.0047(16) C6 0.0206(18) 0.0195(19) 0.0193(18) 0.0024(15) 0.0067(15) 0.0001(15) C7 0.0158(17) 0.0169(19) 0.0175(18) -0.0016(14) 0.0015(14) 0.0033(14) C8 0.0198(19) 0.0179(19) 0.0162(18) 0.0018(13) 0.0043(15) 0.0031(14) C9 0.026(2) 0.032(2) 0.0196(19) -0.0012(16) 0.0106(16) 0.0017(16) C10 0.0212(19) 0.025(2) 0.024(2) -0.0085(16) 0.0032(15) 0.0050(16) C11 0.025(2) 0.013(2) 0.037(2) -0.0051(16) 0.0042(17) 0.0019(15) C12 0.0189(18) 0.019(2) 0.0234(19) 0.0005(15) 0.0056(15) -0.0029(14) C13 0.0156(18) 0.0191(19) 0.0107(16) -0.0023(13) 0.0036(13) -0.0012(14) C14 0.0188(19) 0.024(2) 0.0147(18) 0.0027(14) 0.0058(15) -0.0043(14) C15 0.0161(19) 0.030(2) 0.023(2) -0.0049(16) 0.0078(16) -0.0069(15) C16 0.0158(18) 0.026(2) 0.0220(19) -0.0016(15) 0.0046(15) 0.0046(15) C17 0.024(2) 0.0177(19) 0.0208(19) 0.0044(14) 0.0056(15) 0.0036(15) C18 0.0207(18) 0.0181(19) 0.0193(18) 0.0003(14) 0.0071(15) -0.0021(15) C19 0.0142(17) 0.022(2) 0.0175(18) -0.0012(15) 0.0045(14) -0.0001(14) C20 0.0167(18) 0.020(2) 0.0215(19) 0.0039(15) 0.0040(14) 0.0021(15) C21 0.0211(19) 0.021(2) 0.033(2) -0.0035(16) 0.0058(17) 0.0027(16) C22 0.0160(19) 0.039(3) 0.033(2) -0.0131(18) 0.0071(17) 0.0010(17) C23 0.029(2) 0.039(3) 0.039(2) -0.011(2) 0.0231(19) -0.0140(19) C24 0.028(2) 0.023(2) 0.033(2) -0.0034(16) 0.0187(17) -0.0054(16) C25 0.0215(18) 0.0176(19) 0.0157(17) -0.0013(14) 0.0101(14) -0.0004(14) C26 0.0203(18) 0.021(2) 0.0164(18) 0.0013(14) 0.0034(14) -0.0005(15) C27 0.034(2) 0.021(2) 0.022(2) 0.0047(15) 0.0123(17) 0.0021(16) C28 0.036(2) 0.021(2) 0.029(2) -0.0102(16) 0.0159(19) -0.0129(16) C29 0.027(2) 0.032(2) 0.024(2) -0.0070(17) 0.0039(16) -0.0078(17) C30 0.0214(19) 0.021(2) 0.0205(19) 0.0017(15) 0.0047(15) -0.0020(15) C31 0.0168(17) 0.0142(17) 0.0131(16) 0.0041(13) 0.0056(13) 0.0013(13) _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 S1 O4 1.448(2) . ? S1 O3 1.457(2) . ? S1 O5 1.460(3) . ? S1 C32 1.787(3) . ? C32 C33 1.371(5) . ? C32 C36 1.433(4) . ? C33 C34 1.408(5) 3_655 ? C34 C35 1.357(5) . ? C34 C33 1.408(5) 3_655 ? C35 C36 1.418(5) . ? C36 C36 1.430(7) 3_655 ? Sn1 C1 2.122(3) . ? Sn1 C1 2.122(3) 3_775 ? Sn1 O2 2.184(2) . ? Sn1 O2 2.184(2) 3_775 ? Sn1 O1 2.212(2) 3_775 ? Sn1 O1 2.212(2) . ? P1 O1 1.517(2) . ? P1 C7 1.791(3) . ? P1 C13 1.794(3) . ? P1 C31 1.809(3) . ? P2 O2 1.521(2) . ? P2 C19 1.781(3) . ? P2 C25 1.786(4) . ? P2 C31 1.811(3) . ? C1 C2 1.387(5) . ? C1 C6 1.391(5) . ? C2 C3 1.382(5) . ? C3 C4 1.387(5) . ? C4 C5 1.377(5) . ? C5 C6 1.392(5) . ? C7 C12 1.392(5) . ? C7 C8 1.393(5) . ? C8 C9 1.390(5) . ? C9 C10 1.383(5) . ? C10 C11 1.379(5) . ? C11 C12 1.394(5) . ? C13 C18 1.389(5) . ? C13 C14 1.398(5) . ? C14 C15 1.390(5) . ? C15 C16 1.380(5) . ? C16 C17 1.391(5) . ? C17 C18 1.384(5) . ? C19 C20 1.394(5) . ? C19 C24 1.404(5) . ? C20 C21 1.385(5) . ? C21 C22 1.379(5) . ? C22 C23 1.373(6) . ? C23 C24 1.380(5) . ? C25 C26 1.399(5) . ? C25 C30 1.403(5) . ? C26 C27 1.378(5) . ? C27 C28 1.399(6) . ? C28 C29 1.379(5) . ? C29 C30 1.380(5) . ? 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 O4 S1 O3 113.12(14) . . ? O4 S1 O5 112.92(15) . . ? O3 S1 O5 112.37(15) . . ? O4 S1 C32 107.14(15) . . ? O3 S1 C32 105.51(14) . . ? O5 S1 C32 105.01(15) . . ? C33 C32 C36 120.9(3) . . ? C33 C32 S1 118.6(3) . . ? C36 C32 S1 120.5(2) . . ? C32 C33 C34 119.8(3) . 3_655 ? C35 C34 C33 121.3(3) . 3_655 ? C34 C35 C36 120.8(3) . . ? C35 C36 C36 118.9(4) . 3_655 ? C35 C36 C32 122.8(3) . . ? C36 C36 C32 118.3(4) 3_655 . ? C1 Sn1 C1 180.0 . 3_775 ? C1 Sn1 O2 89.85(11) . . ? C1 Sn1 O2 90.15(11) 3_775 . ? C1 Sn1 O2 90.16(11) . 3_775 ? C1 Sn1 O2 89.85(11) 3_775 3_775 ? O2 Sn1 O2 179.999(2) . 3_775 ? C1 Sn1 O1 88.77(11) . 3_775 ? C1 Sn1 O1 91.23(11) 3_775 3_775 ? O2 Sn1 O1 92.41(8) . 3_775 ? O2 Sn1 O1 87.59(8) 3_775 3_775 ? C1 Sn1 O1 91.23(11) . . ? C1 Sn1 O1 88.77(11) 3_775 . ? O2 Sn1 O1 87.60(8) . . ? O2 Sn1 O1 92.40(8) 3_775 . ? O1 Sn1 O1 180.0 3_775 . ? O1 P1 C7 109.56(15) . . ? O1 P1 C13 111.81(14) . . ? C7 P1 C13 108.43(15) . . ? O1 P1 C31 112.18(14) . . ? C7 P1 C31 108.64(16) . . ? C13 P1 C31 106.07(16) . . ? O2 P2 C19 111.49(15) . . ? O2 P2 C25 112.05(14) . . ? C19 P2 C25 107.29(16) . . ? O2 P2 C31 110.93(14) . . ? C19 P2 C31 106.94(15) . . ? C25 P2 C31 107.90(15) . . ? P1 O1 Sn1 131.35(14) . . ? P2 O2 Sn1 132.51(13) . . ? C2 C1 C6 118.9(3) . . ? C2 C1 Sn1 121.1(2) . . ? C6 C1 Sn1 119.6(3) . . ? C3 C2 C1 121.1(3) . . ? C2 C3 C4 119.6(4) . . ? C5 C4 C3 119.9(3) . . ? C4 C5 C6 120.3(3) . . ? C1 C6 C5 120.1(3) . . ? C12 C7 C8 120.1(3) . . ? C12 C7 P1 117.5(3) . . ? C8 C7 P1 122.4(3) . . ? C9 C8 C7 118.8(3) . . ? C10 C9 C8 121.0(3) . . ? C11 C10 C9 120.2(3) . . ? C10 C11 C12 119.5(3) . . ? C7 C12 C11 120.2(3) . . ? C18 C13 C14 120.4(3) . . ? C18 C13 P1 121.4(3) . . ? C14 C13 P1 118.1(3) . . ? C15 C14 C13 119.2(3) . . ? C16 C15 C14 120.0(3) . . ? C15 C16 C17 121.0(3) . . ? C18 C17 C16 119.3(3) . . ? C17 C18 C13 120.1(3) . . ? C20 C19 C24 119.4(3) . . ? C20 C19 P2 120.3(2) . . ? C24 C19 P2 120.1(3) . . ? C21 C20 C19 120.1(3) . . ? C22 C21 C20 119.8(4) . . ? C23 C22 C21 120.5(3) . . ? C22 C23 C24 120.8(4) . . ? C23 C24 C19 119.3(4) . . ? C26 C25 C30 119.6(3) . . ? C26 C25 P2 123.4(3) . . ? C30 C25 P2 116.8(3) . . ? C27 C26 C25 120.2(3) . . ? C26 C27 C28 119.6(3) . . ? C29 C28 C27 120.5(3) . . ? C28 C29 C30 120.3(3) . . ? C29 C30 C25 119.7(3) . . ? P1 C31 P2 115.17(17) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.612 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.134 data_27marb _database_code_depnum_ccdc_archive 'CCDC 766499' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'organotin sulfonate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H58 N2 O10 S2 Sn2' _chemical_formula_weight 1076.42 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 '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 25.783(5) _cell_length_b 8.597(5) _cell_length_c 24.133(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 116.270(5) _cell_angle_gamma 90.000(5) _cell_volume 4797(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2803 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 21.78 _exptl_crystal_description 'block like' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 1.183 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14974 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 28.27 _reflns_number_total 5837 _reflns_number_gt 3508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX (2) applied to restrict the O-H bond distance of water molecule to around 0.8. The 'similar' ADP restraint SIMU (30) and the rigid bond restraint DELU (7) have been applied to the carbon atoms of the n-butyl chains. SADI was used for one of the 1,2- distance (C3-C4 & C3-C4A) of one of the n-butyl chain ; _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^)+(0.1068P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5837 _refine_ls_number_parameters 289 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1956 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.837340(16) 0.53993(5) 0.022954(17) 0.05549(19) Uani 1 1 d . . . C1 C 0.8428(3) 0.6109(10) 0.1089(3) 0.0802(19) Uani 1 1 d U . . H1A H 0.8123 0.6866 0.1002 0.096 Uiso 1 1 calc R . . H1B H 0.8331 0.5209 0.1267 0.096 Uiso 1 1 calc R . . C2 C 0.8934(4) 0.6748(12) 0.1556(4) 0.104(3) Uani 1 1 d U B . H2A H 0.9059 0.7596 0.1379 0.125 Uiso 1 1 calc R . . H2B H 0.9234 0.5959 0.1688 0.125 Uiso 1 1 calc R . . C3 C 0.8888(5) 0.7364(18) 0.2131(5) 0.153(5) Uani 1 1 d DU . . H3A H 0.8660 0.8309 0.2003 0.184 Uiso 1 1 calc R A 1 H3B H 0.8655 0.6614 0.2222 0.184 Uiso 1 1 calc R A 1 C4 C 0.9320(15) 0.768(4) 0.2651(11) 0.144(12) Uani 0.40 1 d PDU B 1 C4A C 0.9063(15) 0.653(4) 0.2599(12) 0.213(13) Uani 0.60 1 d PDU B 2 C5 C 0.8203(3) 0.3858(8) -0.0522(2) 0.0628(15) Uani 1 1 d . . . H5A H 0.8568 0.3454 -0.0484 0.075 Uiso 1 1 calc R . . H5B H 0.7980 0.2985 -0.0489 0.075 Uiso 1 1 calc R . . C6 C 0.7877(4) 0.4584(9) -0.1161(3) 0.082(2) Uani 1 1 d . . . H6A H 0.7502 0.4930 -0.1206 0.098 Uiso 1 1 calc R . . H6B H 0.8087 0.5499 -0.1183 0.098 Uiso 1 1 calc R . . C7 C 0.7787(3) 0.3568(11) -0.1683(3) 0.096(3) Uani 1 1 d . . . H7A H 0.7549 0.2694 -0.1682 0.115 Uiso 1 1 calc R . . H7B H 0.8158 0.3159 -0.1624 0.115 Uiso 1 1 calc R . . C8 C 0.7504(5) 0.4355(14) -0.2304(4) 0.128(4) Uani 1 1 d . . . H8A H 0.7099 0.4497 -0.2420 0.193 Uiso 1 1 calc R . . H8B H 0.7549 0.3721 -0.2607 0.193 Uiso 1 1 calc R . . H8C H 0.7681 0.5350 -0.2281 0.193 Uiso 1 1 calc R . . S2 S 0.89288(7) 0.1996(2) 0.10074(6) 0.0618(4) Uani 1 1 d . . . O1 O 0.81367(17) 0.7517(5) -0.02708(18) 0.0612(10) Uani 1 1 d . . . O2 O 0.90883(17) 0.3446(5) 0.08072(17) 0.0672(11) Uani 1 1 d . . . O3 O 0.83067(19) 0.1990(6) 0.0817(2) 0.0791(13) Uani 1 1 d . . . O4 O 0.9131(2) 0.0644(6) 0.0829(2) 0.0818(14) Uani 1 1 d . . . O5 O 0.7391(2) 0.5270(7) -0.0071(3) 0.0829(15) Uani 1 1 d D . . N1 N 0.9215(2) 0.6417(6) 0.0280(2) 0.0596(12) Uani 1 1 d . . . C9 C 0.8537(3) 0.8107(7) -0.0440(3) 0.0599(15) Uani 1 1 d . . . C10 C 0.8403(4) 0.9239(9) -0.0889(3) 0.078(2) Uani 1 1 d . . . H10 H 0.8028 0.9625 -0.1083 0.094 Uiso 1 1 calc R . . C11 C 0.8811(4) 0.9805(9) -0.1057(4) 0.0757(19) Uani 1 1 d . . . H11 H 0.8706 1.0551 -0.1367 0.091 Uiso 1 1 calc R . . C12 C 0.9344(5) 0.9311(9) -0.0788(4) 0.089(3) Uani 1 1 d . . . H12 H 0.9609 0.9723 -0.0913 0.107 Uiso 1 1 calc R . . C13 C 0.9541(4) 0.8161(8) -0.0307(3) 0.074(2) Uani 1 1 d . . . C14 C 0.9095(3) 0.7557(7) -0.0160(3) 0.0567(14) Uani 1 1 d . . . C15 C 0.9781(3) 0.5944(9) 0.0606(3) 0.0672(16) Uani 1 1 d . . . H15 H 0.9874 0.5198 0.0914 0.081 Uiso 1 1 calc R . . C16 C 1.0202(3) 0.6552(9) 0.0482(4) 0.078(2) Uani 1 1 d . . . H16 H 1.0582 0.6235 0.0719 0.094 Uiso 1 1 calc R . . C17 C 1.0091(3) 0.7604(9) 0.0027(4) 0.0743(19) Uani 1 1 d . . . H17 H 1.0389 0.7950 -0.0061 0.089 Uiso 1 1 calc R . . C18 C 0.9253(3) 0.2088(7) 0.1831(2) 0.0584(14) Uani 1 1 d . . . C19 C 0.8914(3) 0.2131(9) 0.2124(3) 0.0723(19) Uani 1 1 d . . . H19 H 0.8514 0.2116 0.1892 0.087 Uiso 1 1 calc R . . C20 C 0.9146(3) 0.2197(10) 0.2756(3) 0.078(2) Uani 1 1 d . . . H20 H 0.8905 0.2259 0.2950 0.093 Uiso 1 1 calc R . . C21 C 0.9757(3) 0.2172(8) 0.3115(3) 0.0658(16) Uani 1 1 d . . . H21 H 0.9915 0.2177 0.3544 0.079 Uiso 1 1 calc R . . C22 C 1.0113(2) 0.2139(7) 0.2825(2) 0.0526(13) Uani 1 1 d . . . H101 H 0.728(2) 0.459(5) -0.031(2) 0.043(16) Uiso 1 1 d D . . H102 H 0.741(5) 0.601(9) 0.014(5) 0.17(5) 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 Sn1 0.0448(3) 0.0694(3) 0.0512(3) -0.00753(18) 0.02028(19) -0.00405(18) C1 0.087(5) 0.095(5) 0.065(4) -0.011(4) 0.039(3) -0.001(4) C2 0.082(5) 0.132(7) 0.077(4) -0.033(5) 0.017(4) 0.005(5) C3 0.143(9) 0.208(13) 0.081(5) -0.044(7) 0.025(6) 0.024(9) C4 0.22(3) 0.12(2) 0.072(10) -0.039(14) 0.044(12) -0.03(2) C4A 0.23(3) 0.30(4) 0.121(14) 0.017(17) 0.081(19) 0.06(3) C5 0.062(4) 0.073(4) 0.048(3) -0.014(3) 0.019(3) 0.003(3) C6 0.080(5) 0.100(6) 0.052(4) 0.001(4) 0.016(3) 0.019(4) C7 0.082(5) 0.114(7) 0.067(4) -0.017(4) 0.011(4) 0.007(5) C8 0.121(8) 0.195(12) 0.054(5) 0.008(5) 0.025(5) 0.038(7) S2 0.0488(8) 0.0785(11) 0.0492(8) -0.0029(7) 0.0135(6) -0.0081(7) O1 0.051(2) 0.066(3) 0.070(2) 0.000(2) 0.0302(19) 0.0041(19) O2 0.056(2) 0.084(3) 0.054(2) 0.008(2) 0.0172(19) -0.004(2) O3 0.058(3) 0.102(4) 0.065(2) -0.007(2) 0.015(2) -0.013(2) O4 0.082(4) 0.083(3) 0.068(3) -0.012(2) 0.022(3) 0.002(2) O5 0.050(3) 0.090(4) 0.109(4) -0.041(4) 0.036(3) -0.015(3) N1 0.048(3) 0.070(3) 0.060(3) -0.017(3) 0.024(2) -0.008(2) C9 0.059(4) 0.059(4) 0.060(3) -0.015(3) 0.025(3) -0.004(3) C10 0.085(5) 0.074(5) 0.070(4) -0.002(4) 0.029(4) 0.006(4) C11 0.082(5) 0.074(4) 0.078(5) 0.001(4) 0.042(4) -0.003(4) C12 0.146(9) 0.067(5) 0.096(6) -0.025(4) 0.093(6) -0.027(5) C13 0.104(6) 0.056(4) 0.084(4) -0.033(4) 0.064(4) -0.023(4) C14 0.060(4) 0.056(3) 0.061(3) -0.016(3) 0.033(3) -0.012(3) C15 0.041(3) 0.082(4) 0.077(4) -0.013(3) 0.024(3) -0.011(3) C16 0.047(4) 0.080(5) 0.107(5) -0.028(5) 0.033(4) -0.012(3) C17 0.051(4) 0.077(5) 0.102(5) -0.026(4) 0.039(4) -0.014(3) C18 0.053(3) 0.069(4) 0.050(3) 0.007(3) 0.020(3) -0.002(3) C19 0.043(3) 0.112(6) 0.056(3) 0.011(4) 0.016(3) -0.008(3) C20 0.039(3) 0.133(7) 0.068(4) 0.014(4) 0.030(3) -0.006(4) C21 0.053(4) 0.096(5) 0.049(3) 0.010(3) 0.022(3) 0.004(3) C22 0.037(3) 0.068(3) 0.047(3) 0.002(3) 0.013(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.106(6) . ? Sn1 O1 2.120(4) . ? Sn1 C5 2.128(6) . ? Sn1 N1 2.291(5) . ? Sn1 O5 2.307(5) . ? Sn1 O2 2.426(4) . ? C1 C2 1.403(10) . ? C2 C3 1.539(12) . ? C3 C4A 1.24(2) . ? C3 C4 1.28(2) . ? C5 C6 1.526(9) . ? C6 C7 1.464(10) . ? C7 C8 1.507(11) . ? S2 O4 1.416(5) . ? S2 O3 1.460(5) . ? S2 O2 1.461(5) . ? S2 C18 1.785(6) . ? O1 C9 1.366(7) . ? N1 C14 1.376(8) . ? N1 C15 1.377(8) . ? C9 C14 1.374(8) . ? C9 C10 1.382(9) . ? C10 C11 1.373(11) . ? C11 C12 1.303(12) . ? C12 C13 1.436(11) . ? C13 C17 1.371(10) . ? C13 C14 1.441(9) . ? C15 C16 1.352(9) . ? C16 C17 1.354(10) . ? C18 C19 1.346(8) . ? C18 C22 1.469(7) 2_755 ? C19 C20 1.373(9) . ? C20 C21 1.422(8) . ? C21 C22 1.380(8) . ? C22 C22 1.411(10) 2_755 ? C22 C18 1.469(7) 2_755 ? 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 C1 Sn1 O1 100.9(3) . . ? C1 Sn1 C5 156.6(3) . . ? O1 Sn1 C5 98.7(2) . . ? C1 Sn1 N1 100.8(2) . . ? O1 Sn1 N1 74.31(17) . . ? C5 Sn1 N1 96.7(2) . . ? C1 Sn1 O5 84.8(3) . . ? O1 Sn1 O5 82.1(2) . . ? C5 Sn1 O5 85.3(2) . . ? N1 Sn1 O5 156.4(2) . . ? C1 Sn1 O2 86.1(2) . . ? O1 Sn1 O2 151.14(15) . . ? C5 Sn1 O2 82.9(2) . . ? N1 Sn1 O2 76.88(17) . . ? O5 Sn1 O2 126.60(19) . . ? C2 C1 Sn1 122.5(6) . . ? C1 C2 C3 116.4(8) . . ? C4A C3 C4 54.9(19) . . ? C4A C3 C2 119(2) . . ? C4 C3 C2 125(2) . . ? C6 C5 Sn1 114.8(5) . . ? C7 C6 C5 115.6(6) . . ? C6 C7 C8 114.2(8) . . ? O4 S2 O3 113.7(3) . . ? O4 S2 O2 113.9(3) . . ? O3 S2 O2 109.3(3) . . ? O4 S2 C18 108.7(3) . . ? O3 S2 C18 105.0(3) . . ? O2 S2 C18 105.6(3) . . ? C9 O1 Sn1 115.1(4) . . ? S2 O2 Sn1 121.8(2) . . ? C14 N1 C15 118.0(5) . . ? C14 N1 Sn1 110.3(4) . . ? C15 N1 Sn1 131.0(5) . . ? O1 C9 C14 119.4(6) . . ? O1 C9 C10 122.4(6) . . ? C14 C9 C10 118.2(7) . . ? C11 C10 C9 121.5(7) . . ? C12 C11 C10 120.9(8) . . ? C11 C12 C13 123.0(8) . . ? C17 C13 C12 128.2(7) . . ? C17 C13 C14 117.4(7) . . ? C12 C13 C14 114.4(7) . . ? C9 C14 N1 117.0(5) . . ? C9 C14 C13 121.9(6) . . ? N1 C14 C13 121.1(6) . . ? C16 C15 N1 120.8(7) . . ? C15 C16 C17 122.4(7) . . ? C16 C17 C13 120.1(7) . . ? C19 C18 C22 121.4(5) . 2_755 ? C19 C18 S2 119.5(5) . . ? C22 C18 S2 119.1(4) 2_755 . ? C18 C19 C20 121.3(6) . . ? C19 C20 C21 119.8(6) . . ? C22 C21 C20 119.9(5) . . ? C21 C22 C22 121.4(6) . 2_755 ? C21 C22 C18 122.5(5) . 2_755 ? C22 C22 C18 116.0(6) 2_755 2_755 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.061 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.146