data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wright, Dominic S.' _publ_author_name D.S.Wright _publ_contact_author_email DSW1000@CAM.AC.UK data_dw0942 _database_code_depnum_ccdc_archive 'CCDC 803628' #TrackingRef '- dw0942.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H18 S6 Sn, 2(C2 H8 N)' _chemical_formula_sum 'C25 H34 N2 S6 Sn' _chemical_formula_weight 673.59 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.06670(10) _cell_length_b 28.5622(3) _cell_length_c 14.5669(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.7395(5) _cell_angle_gamma 90.00 _cell_volume 3352.42(7) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 83968 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.35 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 42629 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 23.25 _reflns_number_total 4765 _reflns_number_gt 3671 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Very poor high angle data, which is removed during refinements. Two [H2NMe2] cation presence, one fully occupied, the second one disordered over three position (ratio 45%:35%:20%). One of the [S2PhMe] groups is also disordered over two position, refined as having 50% occupancy each. A small residue peak (1.49e) is found within 1 Angstrom of Sn1, there may be a small component of the compound co-crystallising in a second orientation, and no allowance was made for it. ; _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^)+(0.1100P)^2^+7.7990P] 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 4765 _refine_ls_number_parameters 324 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1973 _refine_ls_wR_factor_gt 0.1773 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.040 _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 0.77464(8) 0.349359(17) 0.51819(4) 0.0809(3) Uani 1 1 d . . . S1 S 0.8088(4) 0.42788(7) 0.59644(17) 0.1022(8) Uani 1 1 d . A . S2 S 0.5991(3) 0.33285(8) 0.65503(17) 0.0925(6) Uani 1 1 d . A . C11 C 0.7801(10) 0.4116(3) 0.7107(5) 0.078(2) Uani 1 1 d . . . C12 C 0.8492(11) 0.4403(3) 0.7817(7) 0.093(2) Uani 1 1 d . A . H12 H 0.9129 0.4669 0.7662 0.111 Uiso 1 1 calc R . . C13 C 0.8262(13) 0.4307(4) 0.8726(7) 0.102(3) Uani 1 1 d . . . H13 H 0.8701 0.4511 0.9192 0.123 Uiso 1 1 calc R A . C14 C 0.7399(12) 0.3915(4) 0.8959(6) 0.097(3) Uani 1 1 d . A . C15 C 0.6738(10) 0.3632(3) 0.8296(6) 0.083(2) Uani 1 1 d . . . H15 H 0.6132 0.3363 0.8468 0.099 Uiso 1 1 calc R A . C16 C 0.6919(9) 0.3722(3) 0.7364(5) 0.0730(18) Uani 1 1 d . A . C17 C 0.719(2) 0.3793(7) 0.9928(10) 0.186(7) Uani 1 1 d . . . H17A H 0.7047 0.4079 1.0286 0.279 Uiso 1 1 calc R A . H17B H 0.8172 0.3624 1.0170 0.279 Uiso 1 1 calc R . . H17C H 0.6205 0.3594 0.9974 0.279 Uiso 1 1 calc R . . S3 S 1.0453(3) 0.32128(7) 0.59204(15) 0.0858(6) Uani 1 1 d . A . S4 S 0.7527(2) 0.26384(7) 0.46888(15) 0.0761(5) Uani 1 1 d . A . C21 C 1.0901(9) 0.2761(3) 0.5148(5) 0.0750(19) Uani 1 1 d . . . C22 C 1.2566(11) 0.2633(4) 0.5040(7) 0.100(3) Uani 1 1 d . A . H22 H 1.3419 0.2804 0.5362 0.120 Uiso 1 1 calc R . . C23 C 1.2997(11) 0.2270(4) 0.4485(7) 0.104(3) Uani 1 1 d . . . H23 H 1.4134 0.2192 0.4433 0.125 Uiso 1 1 calc R A . C24 C 1.1769(10) 0.2011(3) 0.3994(6) 0.089(2) Uani 1 1 d . A . C25 C 1.0148(9) 0.2144(3) 0.4084(5) 0.075(2) Uani 1 1 d . . . H25 H 0.9301 0.1979 0.3744 0.090 Uiso 1 1 calc R A . C26 C 0.9689(8) 0.2509(2) 0.4651(5) 0.0691(18) Uani 1 1 d . A . C27 C 1.2199(12) 0.1614(4) 0.3385(8) 0.117(4) Uani 1 1 d . . . H27A H 1.1198 0.1431 0.3226 0.176 Uiso 1 1 calc R A . H27B H 1.3024 0.1413 0.3705 0.176 Uiso 1 1 calc R . . H27C H 1.2657 0.1737 0.2822 0.176 Uiso 1 1 calc R . . S5 S 0.4838(10) 0.3640(3) 0.4311(6) 0.0828(19) Uani 0.50 1 d P A 1 S6 S 0.8818(9) 0.3810(3) 0.3774(5) 0.091(2) Uani 0.50 1 d P A 1 C31 C 0.5664(16) 0.4071(5) 0.3495(9) 0.058(3) Uiso 0.50 1 d P A 1 C32 C 0.443(3) 0.4354(7) 0.3061(14) 0.102(5) Uiso 0.50 1 d P A 1 H32 H 0.3309 0.4329 0.3221 0.122 Uiso 0.50 1 calc PR A 1 C33 C 0.491(3) 0.4685(8) 0.2365(15) 0.111(6) Uiso 0.50 1 d P A 1 H33 H 0.4100 0.4886 0.2081 0.134 Uiso 0.50 1 calc PR A 1 C34 C 0.6362(14) 0.4707(4) 0.2139(7) 0.109(3) Uiso 0.50 1 d P A 1 C35 C 0.759(2) 0.4468(5) 0.2622(11) 0.074(4) Uiso 0.50 1 d P A 1 H35 H 0.8735 0.4514 0.2538 0.089 Uiso 0.50 1 calc PR A 1 C36 C 0.6930(13) 0.4124(3) 0.3302(6) 0.091(2) Uiso 0.50 1 d P A 1 C37 C 0.689(3) 0.5103(9) 0.1455(18) 0.131(7) Uiso 0.50 1 d P A 1 H37A H 0.5981 0.5160 0.0997 0.197 Uiso 0.50 1 calc PR A 1 H37B H 0.7880 0.5003 0.1144 0.197 Uiso 0.50 1 calc PR A 1 H37C H 0.7133 0.5391 0.1799 0.197 Uiso 0.50 1 calc PR A 1 S5' S 0.9677(9) 0.3770(3) 0.3888(5) 0.0917(18) Uani 0.50 1 d P A 2 S6' S 0.5506(10) 0.3712(4) 0.4090(6) 0.097(2) Uani 0.50 1 d P A 2 C31' C 0.815(2) 0.4114(6) 0.3267(11) 0.078(4) Uiso 0.50 1 d P A 2 C32' C 0.890(3) 0.4420(7) 0.2614(14) 0.106(6) Uiso 0.50 1 d P A 2 H32' H 1.0071 0.4435 0.2584 0.127 Uiso 0.50 1 calc PR A 2 C33' C 0.790(3) 0.4690(10) 0.204(2) 0.138(8) Uiso 0.50 1 d P A 2 H33' H 0.8374 0.4865 0.1561 0.166 Uiso 0.50 1 calc PR A 2 C34' C 0.6362(14) 0.4707(4) 0.2139(7) 0.109(3) Uiso 0.50 1 d P A 2 C35' C 0.566(3) 0.4400(9) 0.2736(17) 0.125(7) Uiso 0.50 1 d P A 2 H35' H 0.4494 0.4366 0.2787 0.150 Uiso 0.50 1 calc PR A 2 C36' C 0.6930(13) 0.4124(3) 0.3302(6) 0.091(2) Uiso 0.50 1 d P A 2 C37' C 0.533(4) 0.5026(11) 0.146(2) 0.158(10) Uiso 0.50 1 d P A 2 H37D H 0.5279 0.5343 0.1712 0.237 Uiso 0.50 1 calc PR A 2 H37E H 0.4207 0.4900 0.1367 0.237 Uiso 0.50 1 calc PR A 2 H37F H 0.5864 0.5036 0.0868 0.237 Uiso 0.50 1 calc PR A 2 N1 N 0.2598(11) 0.4211(3) 0.5590(7) 0.118(3) Uani 1 1 d . . . H1NA H 0.1643 0.4037 0.5509 0.141 Uiso 1 1 calc R . . H1NB H 0.3440 0.4048 0.5330 0.141 Uiso 1 1 calc R . . C1 C 0.3003(14) 0.4260(4) 0.6595(9) 0.124(3) Uani 1 1 d . . . H1A H 0.4091 0.4410 0.6690 0.185 Uiso 1 1 calc R . . H1B H 0.3029 0.3950 0.6882 0.185 Uiso 1 1 calc R . . H1C H 0.2156 0.4453 0.6872 0.185 Uiso 1 1 calc R . . C2 C 0.236(2) 0.4671(6) 0.5089(15) 0.225(11) Uani 1 1 d . . . H2A H 0.1513 0.4857 0.5386 0.338 Uiso 1 1 calc R . . H2B H 0.1996 0.4611 0.4448 0.338 Uiso 1 1 calc R . . H2C H 0.3408 0.4844 0.5108 0.338 Uiso 1 1 calc R . . N2 N 0.7512(17) 0.2670(4) 0.2375(7) 0.129(4) Uani 0.80 1 d PD . . H2NA H 0.7415 0.2642 0.2993 0.155 Uiso 0.45 1 d P B 1 H2NB H 0.7299 0.2370 0.2144 0.155 Uiso 0.45 1 d P C 1 C3 C 0.926(3) 0.2818(10) 0.216(2) 0.121(6) Uiso 0.45 1 d PD D 1 H3A H 1.0054 0.2588 0.2413 0.182 Uiso 0.45 1 calc PR D 1 H3B H 0.9496 0.3126 0.2425 0.182 Uiso 0.45 1 calc PR D 1 H3C H 0.9343 0.2833 0.1488 0.182 Uiso 0.45 1 calc PR D 1 C4 C 0.631(3) 0.2998(9) 0.1979(18) 0.116(6) Uiso 0.45 1 d PD D 1 H4A H 0.5192 0.2898 0.2121 0.175 Uiso 0.45 1 calc PR D 1 H4B H 0.6405 0.3008 0.1311 0.175 Uiso 0.45 1 calc PR D 1 H4C H 0.6529 0.3311 0.2236 0.175 Uiso 0.45 1 calc PR D 1 H2NC H 0.7819 0.2627 0.2979 0.140 Uiso 0.35 1 d P E 2 H2ND H 0.7500 0.2369 0.2126 0.140 Uiso 0.35 1 d P F 2 C3' C 0.874(4) 0.2943(12) 0.193(3) 0.121(6) Uiso 0.35 1 d PD D 2 H3'1 H 0.9830 0.2798 0.2036 0.182 Uiso 0.35 1 calc PR D 2 H3'2 H 0.8756 0.3261 0.2181 0.182 Uiso 0.35 1 calc PR D 2 H3'3 H 0.8457 0.2955 0.1268 0.182 Uiso 0.35 1 calc PR D 2 C4' C 0.577(3) 0.2887(12) 0.223(2) 0.116(6) Uiso 0.35 1 d PD D 2 H4'1 H 0.4953 0.2687 0.2516 0.175 Uiso 0.35 1 calc PR D 2 H4'2 H 0.5486 0.2914 0.1570 0.175 Uiso 0.35 1 calc PR D 2 H4'3 H 0.5758 0.3199 0.2511 0.175 Uiso 0.35 1 calc PR D 2 N3 N 1.096(7) 0.3822(15) 0.097(6) 0.23(3) Uiso 0.20 1 d PD . . H3NA H 1.0738 0.3713 0.0383 0.279 Uiso 0.20 1 calc PR . . H3NB H 1.0066 0.3763 0.1320 0.279 Uiso 0.20 1 calc PR . . C5 C 1.137(5) 0.4324(14) 0.097(3) 0.080(10) Uiso 0.20 1 d PD . . H5A H 1.0415 0.4502 0.0714 0.120 Uiso 0.20 1 calc PR . . H5B H 1.2326 0.4377 0.0591 0.120 Uiso 0.20 1 calc PR . . H5C H 1.1640 0.4428 0.1599 0.120 Uiso 0.20 1 calc PR . . C6 C 1.251(6) 0.3604(18) 0.139(4) 0.106(14) Uiso 0.20 1 d PD . . H6A H 1.2358 0.3264 0.1427 0.160 Uiso 0.20 1 calc PR . . H6B H 1.2736 0.3732 0.2004 0.160 Uiso 0.20 1 calc PR . . H6C H 1.3442 0.3673 0.1003 0.160 Uiso 0.20 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.1142(5) 0.0551(4) 0.0726(4) -0.0029(2) -0.0048(3) 0.0027(3) S1 0.165(2) 0.0522(11) 0.0901(15) -0.0029(10) 0.0151(14) -0.0023(12) S2 0.0989(15) 0.0800(13) 0.0988(15) -0.0150(12) 0.0082(12) -0.0132(11) C11 0.090(5) 0.060(4) 0.083(5) -0.013(4) 0.005(4) 0.010(4) C12 0.104(6) 0.067(5) 0.107(7) -0.018(5) 0.000(5) 0.002(4) C13 0.123(7) 0.097(7) 0.087(6) -0.026(5) -0.009(5) 0.009(6) C14 0.109(7) 0.099(7) 0.083(6) -0.012(5) 0.001(5) 0.018(6) C15 0.075(5) 0.087(5) 0.086(6) -0.006(5) 0.009(4) 0.020(4) C16 0.073(4) 0.065(4) 0.080(5) -0.006(4) -0.001(4) 0.011(4) C17 0.28(2) 0.161(15) 0.116(10) -0.023(9) 0.008(11) -0.021(13) S3 0.0953(14) 0.0689(12) 0.0915(14) -0.0117(10) -0.0131(11) -0.0110(10) S4 0.0680(11) 0.0609(11) 0.0980(14) -0.0117(9) -0.0108(9) 0.0000(8) C21 0.074(5) 0.068(4) 0.082(5) -0.004(4) -0.005(4) -0.011(4) C22 0.079(6) 0.102(7) 0.117(7) -0.015(6) -0.014(5) -0.029(5) C23 0.069(5) 0.123(8) 0.121(7) -0.033(6) 0.000(5) -0.009(5) C24 0.075(5) 0.093(6) 0.099(6) -0.015(5) -0.002(4) -0.005(4) C25 0.061(4) 0.076(5) 0.089(5) -0.007(4) -0.007(4) -0.010(3) C26 0.067(4) 0.061(4) 0.079(5) 0.001(4) -0.006(3) -0.009(3) C27 0.079(6) 0.140(9) 0.133(8) -0.056(7) 0.002(5) 0.007(5) S5 0.103(6) 0.064(3) 0.082(4) 0.007(2) 0.012(3) 0.008(3) S6 0.103(5) 0.094(4) 0.078(3) 0.017(3) 0.016(4) 0.027(4) S5' 0.110(5) 0.083(4) 0.081(3) -0.002(3) 0.003(4) 0.008(4) S6' 0.097(6) 0.102(5) 0.091(5) -0.003(4) -0.018(4) 0.027(4) N1 0.109(6) 0.078(5) 0.165(8) 0.046(5) 0.008(5) -0.006(4) C1 0.125(8) 0.107(8) 0.137(9) -0.012(7) -0.019(7) 0.014(6) C2 0.209(16) 0.159(14) 0.32(2) 0.159(16) 0.098(16) 0.059(12) N2 0.214(13) 0.086(6) 0.084(6) -0.016(5) -0.030(7) 0.016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 S6' 2.431(9) . ? Sn1 S6 2.437(8) . ? Sn1 S3 2.519(2) . ? Sn1 S1 2.525(2) . ? Sn1 S2 2.544(2) . ? Sn1 S4 2.5498(19) . ? Sn1 S5' 2.624(8) . ? Sn1 S5 2.647(9) . ? S1 C11 1.754(8) . ? S2 C16 1.773(8) . ? C11 C16 1.392(11) . ? C11 C12 1.413(11) . ? C12 C13 1.374(13) . ? C12 H12 0.9500 . ? C13 C14 1.369(14) . ? C13 H13 0.9500 . ? C14 C15 1.350(12) . ? C14 C17 1.472(17) . ? C15 C16 1.396(11) . ? C15 H15 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? S3 C21 1.761(8) . ? S4 C26 1.786(7) . ? C21 C26 1.389(10) . ? C21 C22 1.408(11) . ? C22 C23 1.370(13) . ? C22 H22 0.9500 . ? C23 C24 1.404(12) . ? C23 H23 0.9500 . ? C24 C25 1.374(10) . ? C24 C27 1.491(12) . ? C25 C26 1.391(10) . ? C25 H25 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? S5 C31 1.858(14) . ? S6 C36 1.869(11) . ? C31 C36 1.082(13) . ? C31 C32 1.41(2) . ? C32 C33 1.45(3) . ? C32 H32 0.9500 . ? C33 C34 1.23(2) . ? C33 H33 0.9500 . ? C34 C35 1.367(19) . ? C34 C37 1.58(3) . ? C35 C36 1.509(18) . ? C35 H35 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? S5' C31' 1.786(17) . ? C31' C32' 1.45(3) . ? C32' C33' 1.37(3) . ? C32' H32' 0.9500 . ? C33' H33' 0.9500 . ? C35' H35' 0.9500 . ? C37' H37D 0.9800 . ? C37' H37E 0.9800 . ? C37' H37F 0.9800 . ? N1 C1 1.490(14) . ? N1 C2 1.512(14) . ? N1 H1NA 0.9200 . ? N1 H1NB 0.9200 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? N2 C3' 1.436(18) . ? N2 C4 1.447(17) . ? N2 C3 1.517(17) . ? N2 C4' 1.543(18) . ? N2 H2NA 0.911(11) . ? N2 H2NB 0.935(10) . ? N2 H2NC 0.911(10) . ? N2 H2ND 0.934(10) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C3' H3'1 0.9800 . ? C3' H3'2 0.9800 . ? C3' H3'3 0.9800 . ? C4' H4'1 0.9800 . ? C4' H4'2 0.9800 . ? C4' H4'3 0.9800 . ? N3 C5 1.47(2) . ? N3 C6 1.50(2) . ? N3 H3NA 0.9200 . ? N3 H3NB 0.9200 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S6' Sn1 S6 68.7(3) . . ? S6' Sn1 S3 164.4(2) . . ? S6 Sn1 S3 98.19(17) . . ? S6' Sn1 S1 97.4(2) . . ? S6 Sn1 S1 90.8(2) . . ? S3 Sn1 S1 90.93(8) . . ? S6' Sn1 S2 97.8(2) . . ? S6 Sn1 S2 163.98(16) . . ? S3 Sn1 S2 96.31(8) . . ? S1 Sn1 S2 82.17(8) . . ? S6' Sn1 S4 91.3(2) . . ? S6 Sn1 S4 98.1(2) . . ? S3 Sn1 S4 82.09(6) . . ? S1 Sn1 S4 169.33(8) . . ? S2 Sn1 S4 90.54(7) . . ? S6' Sn1 S5' 84.3(3) . . ? S6 Sn1 S5' 15.66(15) . . ? S3 Sn1 S5' 82.57(17) . . ? S1 Sn1 S5' 90.08(18) . . ? S2 Sn1 S5' 172.17(18) . . ? S4 Sn1 S5' 96.97(18) . . ? S6' Sn1 S5 14.4(2) . . ? S6 Sn1 S5 83.1(2) . . ? S3 Sn1 S5 170.24(19) . . ? S1 Sn1 S5 98.7(2) . . ? S2 Sn1 S5 83.75(16) . . ? S4 Sn1 S5 88.15(19) . . ? S5' Sn1 S5 98.7(2) . . ? C11 S1 Sn1 100.2(3) . . ? C16 S2 Sn1 100.0(3) . . ? C16 C11 C12 117.4(8) . . ? C16 C11 S1 124.2(6) . . ? C12 C11 S1 118.4(7) . . ? C13 C12 C11 121.5(9) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 119.8(9) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 120.0(9) . . ? C15 C14 C17 119.0(11) . . ? C13 C14 C17 121.0(11) . . ? C14 C15 C16 122.0(9) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C11 C16 C15 119.3(7) . . ? C11 C16 S2 122.5(6) . . ? C15 C16 S2 118.2(6) . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C21 S3 Sn1 99.3(3) . . ? C26 S4 Sn1 98.7(2) . . ? C26 C21 C22 117.3(7) . . ? C26 C21 S3 123.5(6) . . ? C22 C21 S3 119.2(6) . . ? C23 C22 C21 122.2(8) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 C23 C24 120.4(8) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 117.2(8) . . ? C25 C24 C27 121.1(7) . . ? C23 C24 C27 121.7(8) . . ? C24 C25 C26 123.1(7) . . ? C24 C25 H25 118.5 . . ? C26 C25 H25 118.5 . . ? C21 C26 C25 119.8(7) . . ? C21 C26 S4 122.7(6) . . ? C25 C26 S4 117.5(5) . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C31 S5 Sn1 94.3(5) . . ? C36 S6 Sn1 99.9(4) . . ? C36 C31 C32 117.3(15) . . ? C36 C31 S5 129.1(11) . . ? C32 C31 S5 113.6(12) . . ? C31 C32 C33 118.8(18) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? C34 C33 C32 120(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.6(16) . . ? C33 C34 C37 119.5(17) . . ? C35 C34 C37 118.2(14) . . ? C34 C35 C36 113.3(12) . . ? C34 C35 H35 123.4 . . ? C36 C35 H35 123.4 . . ? C31 C36 C35 128.7(12) . . ? C31 C36 S6 126.9(10) . . ? C35 C36 S6 104.4(9) . . ? C31' S5' Sn1 96.4(6) . . ? C32' C31' S5' 111.6(14) . . ? C33' C32' C31' 119(2) . . ? C33' C32' H32' 120.3 . . ? C31' C32' H32' 120.3 . . ? C32' C33' H33' 119.9 . . ? H37D C37' H37E 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? C1 N1 C2 114.2(13) . . ? C1 N1 H1NA 108.7 . . ? C2 N1 H1NA 108.7 . . ? C1 N1 H1NB 108.7 . . ? C2 N1 H1NB 108.7 . . ? H1NA N1 H1NB 107.6 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3' N2 C4 86.0(19) . . ? C4 N2 C3 110.2(17) . . ? C3' N2 C4' 111(2) . . ? C3 N2 C4' 135.1(19) . . ? C3' N2 H2NA 126.0(19) . . ? C4 N2 H2NA 111.4(15) . . ? C3 N2 H2NA 110.9(15) . . ? C4' N2 H2NA 92.9(16) . . ? C3' N2 H2NB 117.0(19) . . ? C4 N2 H2NB 110.0(15) . . ? C3 N2 H2NB 109.6(15) . . ? C4' N2 H2NB 99.7(17) . . ? H2NA N2 H2NB 104.6(11) . . ? C3' N2 H2NC 110(2) . . ? C4 N2 H2NC 128.3(15) . . ? C3 N2 H2NC 91.7(14) . . ? C4' N2 H2NC 113.0(17) . . ? H2NB N2 H2NC 105.1(11) . . ? C3' N2 H2ND 108.6(19) . . ? C4 N2 H2ND 116.5(15) . . ? C3 N2 H2ND 99.6(15) . . ? C4' N2 H2ND 108.9(17) . . ? H2NA N2 H2ND 107.6(11) . . ? H2NC N2 H2ND 104.3(10) . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C3' H3'1 109.5 . . ? N2 C3' H3'2 109.5 . . ? H3'1 C3' H3'2 109.5 . . ? N2 C3' H3'3 109.5 . . ? H3'1 C3' H3'3 109.5 . . ? H3'2 C3' H3'3 109.5 . . ? N2 C4' H4'1 109.5 . . ? N2 C4' H4'2 109.5 . . ? H4'1 C4' H4'2 109.5 . . ? N2 C4' H4'3 109.5 . . ? H4'1 C4' H4'3 109.5 . . ? H4'2 C4' H4'3 109.5 . . ? C5 N3 C6 103(4) . . ? C5 N3 H3NA 111.2 . . ? C6 N3 H3NA 111.2 . . ? C5 N3 H3NB 111.2 . . ? C6 N3 H3NB 111.2 . . ? H3NA N3 H3NB 109.1 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.491 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.138 # Attachment '- dw0951.cif' data_dw0951 _database_code_depnum_ccdc_archive 'CCDC 803629' #TrackingRef '- dw0951.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 S6 Sn, 2(C2 H8 N), C2 H3 N' _chemical_formula_sum 'C24 H31 N3 S6 Sn' _chemical_formula_weight 672.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.7617(1) _cell_length_b 13.0775(2) _cell_length_c 28.9361(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.770(1) _cell_angle_gamma 90.00 _cell_volume 2910.15(8) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 19001 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 20.60 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 9164 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 20.59 _reflns_number_total 2909 _reflns_number_gt 2802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+10.2228P] 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 2909 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.441 _refine_ls_restrained_S_all 1.441 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.21845(5) 0.51515(3) 0.346720(14) 0.02315(18) Uani 1 1 d . . . S1 S 0.4783(2) 0.58882(13) 0.31539(6) 0.0313(4) Uani 1 1 d . . . S2 S 0.15435(19) 0.44725(12) 0.26377(5) 0.0252(4) Uani 1 1 d . . . S3 S 0.3992(2) 0.36759(13) 0.38097(6) 0.0380(5) Uani 1 1 d . . . S4 S -0.0354(2) 0.41127(13) 0.36732(6) 0.0344(4) Uani 1 1 d . . . S5 S 0.2843(2) 0.60494(13) 0.42401(6) 0.0322(4) Uani 1 1 d . . . S6 S 0.0194(2) 0.66806(13) 0.32656(6) 0.0327(4) Uani 1 1 d . . . N1 N 0.7317(9) 0.5850(6) 0.4195(2) 0.066(2) Uani 1 1 d . . . H1A H 0.6244 0.5627 0.4058 0.079 Uiso 1 1 calc R . . H1B H 0.8131 0.5599 0.4021 0.079 Uiso 1 1 calc R . . N2 N -0.0757(7) 0.2292(4) 0.2828(2) 0.0424(15) Uani 1 1 d . . . H2A H -0.0927 0.2199 0.2510 0.051 Uiso 1 1 calc R . . H2B H -0.0599 0.2980 0.2884 0.051 Uiso 1 1 calc R . . N3 N 0.6855(13) 1.0182(9) 0.4423(4) 0.127(4) Uani 1 1 d . . . C11 C 0.5065(8) 0.4962(4) 0.2728(2) 0.0216(15) Uani 1 1 d . . . C12 C 0.6712(8) 0.4854(5) 0.2592(2) 0.0268(16) Uani 1 1 d . . . H12 H 0.7648 0.5256 0.2739 0.032 Uiso 1 1 calc R . . C13 C 0.7005(8) 0.4173(5) 0.2248(2) 0.0323(17) Uani 1 1 d . . . H13 H 0.8127 0.4124 0.2154 0.039 Uiso 1 1 calc R . . C14 C 0.5667(8) 0.3560(5) 0.2041(2) 0.0355(18) Uani 1 1 d . . . H14 H 0.5873 0.3087 0.1805 0.043 Uiso 1 1 calc R . . C15 C 0.4045(8) 0.3633(5) 0.2175(2) 0.0271(16) Uani 1 1 d . . . H15 H 0.3142 0.3193 0.2039 0.032 Uiso 1 1 calc R . . C16 C 0.3703(7) 0.4348(5) 0.2509(2) 0.0247(15) Uani 1 1 d . . . C21 C 0.2549(10) 0.3086(5) 0.4144(2) 0.0380(18) Uani 1 1 d . . . C22 C 0.3266(13) 0.2372(6) 0.4486(3) 0.057(2) Uani 1 1 d . . . H22 H 0.4491 0.2280 0.4539 0.068 Uiso 1 1 calc R . . C23 C 0.2263(19) 0.1823(6) 0.4735(3) 0.077(3) Uani 1 1 d . . . H23 H 0.2785 0.1342 0.4957 0.092 Uiso 1 1 calc R . . C24 C 0.0484(19) 0.1946(7) 0.4673(3) 0.079(3) Uani 1 1 d . . . H24 H -0.0218 0.1540 0.4846 0.095 Uiso 1 1 calc R . . C25 C -0.0287(13) 0.2674(6) 0.4354(3) 0.057(2) Uani 1 1 d . . . H25 H -0.1507 0.2782 0.4321 0.068 Uiso 1 1 calc R . . C26 C 0.0739(10) 0.3242(5) 0.4085(2) 0.0396(19) Uani 1 1 d . . . C31 C 0.2124(8) 0.7311(5) 0.4102(2) 0.0280(16) Uani 1 1 d . . . C32 C 0.2665(9) 0.8080(5) 0.4428(2) 0.0362(18) Uani 1 1 d . . . H32 H 0.3453 0.7909 0.4697 0.043 Uiso 1 1 calc R . . C33 C 0.2093(10) 0.9070(6) 0.4371(3) 0.048(2) Uani 1 1 d . . . H33 H 0.2485 0.9577 0.4595 0.058 Uiso 1 1 calc R . . C34 C 0.0931(10) 0.9319(5) 0.3979(3) 0.0412(19) Uani 1 1 d . . . H34 H 0.0487 0.9994 0.3939 0.049 Uiso 1 1 calc R . . C35 C 0.0423(8) 0.8583(5) 0.3646(2) 0.0307(17) Uani 1 1 d . . . H35 H -0.0337 0.8767 0.3373 0.037 Uiso 1 1 calc R . . C36 C 0.0999(8) 0.7578(5) 0.3702(2) 0.0243(15) Uani 1 1 d . . . C41 C 0.7662(13) 0.5415(8) 0.4663(3) 0.086(3) Uani 1 1 d . . . H41A H 0.7584 0.4668 0.4644 0.129 Uiso 1 1 calc R . . H41B H 0.6801 0.5673 0.4853 0.129 Uiso 1 1 calc R . . H41C H 0.8830 0.5613 0.4807 0.129 Uiso 1 1 calc R . . C42 C 0.7347(10) 0.6976(7) 0.4171(3) 0.062(3) Uani 1 1 d . . . H42A H 0.7269 0.7192 0.3845 0.094 Uiso 1 1 calc R . . H42B H 0.8433 0.7231 0.4345 0.094 Uiso 1 1 calc R . . H42C H 0.6357 0.7254 0.4308 0.094 Uiso 1 1 calc R . . C43 C -0.2346(10) 0.1964(6) 0.3017(3) 0.052(2) Uani 1 1 d . . . H43A H -0.3326 0.2392 0.2885 0.077 Uiso 1 1 calc R . . H43B H -0.2169 0.2034 0.3357 0.077 Uiso 1 1 calc R . . H43C H -0.2596 0.1248 0.2933 0.077 Uiso 1 1 calc R . . C44 C 0.0843(10) 0.1752(6) 0.3022(3) 0.0460(19) Uani 1 1 d . . . H44A H 0.1819 0.2003 0.2871 0.069 Uiso 1 1 calc R . . H44B H 0.0696 0.1016 0.2964 0.069 Uiso 1 1 calc R . . H44C H 0.1079 0.1876 0.3358 0.069 Uiso 1 1 calc R . . C45 C 0.5972(12) 1.0404(8) 0.4092(4) 0.070(3) Uani 1 1 d . . . C46 C 0.4838(11) 1.0748(7) 0.3690(3) 0.066(2) Uani 1 1 d . . . H46A H 0.3641 1.0547 0.3718 0.079 Uiso 1 1 calc R . . H46B H 0.5193 1.0439 0.3409 0.079 Uiso 1 1 calc R . . H46C H 0.4906 1.1495 0.3668 0.079 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 0.0236(3) 0.0224(3) 0.0235(3) -0.0008(2) 0.00295(19) -0.00034(19) S1 0.0329(10) 0.0318(10) 0.0301(10) -0.0093(8) 0.0074(8) -0.0124(8) S2 0.0198(9) 0.0295(10) 0.0264(10) -0.0050(7) 0.0034(7) -0.0038(7) S3 0.0392(11) 0.0316(10) 0.0413(11) 0.0037(9) -0.0009(9) 0.0069(8) S4 0.0333(10) 0.0370(11) 0.0352(11) -0.0050(8) 0.0131(8) -0.0091(8) S5 0.0394(10) 0.0348(10) 0.0212(9) -0.0024(8) -0.0002(8) 0.0045(8) S6 0.0338(10) 0.0281(10) 0.0328(10) -0.0078(8) -0.0072(8) 0.0055(8) N1 0.050(4) 0.101(6) 0.042(5) -0.028(4) -0.012(3) 0.036(4) N2 0.051(4) 0.035(4) 0.042(4) -0.002(3) 0.006(3) -0.003(3) N3 0.093(7) 0.169(11) 0.107(9) 0.032(8) -0.029(7) 0.011(7) C11 0.026(4) 0.017(3) 0.021(3) 0.004(3) 0.001(3) -0.005(3) C12 0.019(4) 0.032(4) 0.028(4) 0.002(3) -0.002(3) -0.006(3) C13 0.022(4) 0.040(4) 0.035(4) -0.004(4) 0.007(3) 0.005(3) C14 0.035(4) 0.030(4) 0.042(4) -0.014(3) 0.006(4) 0.003(3) C15 0.021(4) 0.026(4) 0.034(4) -0.011(3) 0.001(3) -0.001(3) C16 0.018(4) 0.025(4) 0.031(4) 0.008(3) 0.003(3) 0.003(3) C21 0.067(6) 0.024(4) 0.021(4) -0.007(3) 0.001(4) 0.003(4) C22 0.111(7) 0.031(5) 0.026(5) -0.005(4) 0.003(5) 0.010(5) C23 0.179(12) 0.023(5) 0.031(5) 0.005(4) 0.027(7) 0.009(7) C24 0.166(12) 0.045(6) 0.035(6) -0.011(5) 0.047(7) -0.044(7) C25 0.106(7) 0.038(5) 0.032(5) -0.010(4) 0.031(5) -0.026(5) C26 0.072(6) 0.026(4) 0.024(4) -0.011(3) 0.016(4) -0.016(4) C31 0.031(4) 0.029(4) 0.026(4) -0.006(3) 0.012(3) -0.005(3) C32 0.045(4) 0.034(5) 0.028(4) -0.004(4) 0.003(3) -0.003(4) C33 0.066(5) 0.042(5) 0.037(5) -0.012(4) 0.011(4) -0.014(4) C34 0.059(5) 0.021(4) 0.047(5) -0.004(4) 0.016(4) -0.006(4) C35 0.030(4) 0.029(4) 0.034(4) 0.006(4) 0.009(3) 0.000(3) C36 0.022(3) 0.030(4) 0.022(4) -0.003(3) 0.007(3) -0.004(3) C41 0.098(8) 0.112(9) 0.043(6) -0.005(6) -0.009(5) 0.048(7) C42 0.051(5) 0.091(8) 0.047(5) -0.017(5) 0.012(4) -0.031(5) C43 0.054(5) 0.052(5) 0.052(5) -0.016(4) 0.016(4) -0.013(4) C44 0.057(5) 0.037(4) 0.042(5) -0.003(4) -0.001(4) 0.002(4) C45 0.055(6) 0.082(7) 0.071(7) -0.003(6) 0.003(6) 0.001(5) C46 0.064(6) 0.077(6) 0.056(6) -0.002(5) 0.006(5) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 S3 2.5094(18) . ? Sn1 S1 2.5123(16) . ? Sn1 S5 2.5165(17) . ? Sn1 S4 2.5299(17) . ? Sn1 S2 2.5444(16) . ? Sn1 S6 2.5460(17) . ? S1 C11 1.764(6) . ? S2 C16 1.774(6) . ? S3 C21 1.755(8) . ? S4 C26 1.779(8) . ? S5 C31 1.770(7) . ? S6 C36 1.774(6) . ? N1 C41 1.461(11) . ? N1 C42 1.474(11) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C44 1.472(9) . ? N2 C43 1.478(9) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 C45 1.138(12) . ? C11 C12 1.394(8) . ? C11 C16 1.408(9) . ? C12 C13 1.376(9) . ? C12 H12 0.9500 . ? C13 C14 1.383(9) . ? C13 H13 0.9500 . ? C14 C15 1.370(9) . ? C14 H14 0.9500 . ? C15 C16 1.395(9) . ? C15 H15 0.9500 . ? C21 C26 1.407(10) . ? C21 C22 1.418(10) . ? C22 C23 1.339(13) . ? C22 H22 0.9500 . ? C23 C24 1.378(14) . ? C23 H23 0.9500 . ? C24 C25 1.402(14) . ? C24 H24 0.9500 . ? C25 C26 1.400(10) . ? C25 H25 0.9500 . ? C31 C36 1.398(9) . ? C31 C32 1.403(9) . ? C32 C33 1.372(10) . ? C32 H32 0.9500 . ? C33 C34 1.389(10) . ? C33 H33 0.9500 . ? C34 C35 1.380(9) . ? C34 H34 0.9500 . ? C35 C36 1.390(9) . ? C35 H35 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.434(13) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Sn1 S1 90.25(6) . . ? S3 Sn1 S5 88.41(6) . . ? S1 Sn1 S5 93.74(6) . . ? S3 Sn1 S4 84.58(6) . . ? S1 Sn1 S4 168.43(6) . . ? S5 Sn1 S4 96.45(6) . . ? S3 Sn1 S2 97.57(6) . . ? S1 Sn1 S2 81.81(5) . . ? S5 Sn1 S2 172.53(6) . . ? S4 Sn1 S2 88.60(5) . . ? S3 Sn1 S6 169.70(6) . . ? S1 Sn1 S6 96.20(6) . . ? S5 Sn1 S6 83.18(5) . . ? S4 Sn1 S6 90.45(6) . . ? S2 Sn1 S6 91.30(5) . . ? C11 S1 Sn1 99.8(2) . . ? C16 S2 Sn1 99.3(2) . . ? C21 S3 Sn1 101.0(2) . . ? C26 S4 Sn1 100.7(2) . . ? C31 S5 Sn1 102.4(2) . . ? C36 S6 Sn1 102.3(2) . . ? C41 N1 C42 115.4(7) . . ? C41 N1 H1A 108.4 . . ? C42 N1 H1A 108.4 . . ? C41 N1 H1B 108.4 . . ? C42 N1 H1B 108.4 . . ? H1A N1 H1B 107.5 . . ? C44 N2 C43 115.0(6) . . ? C44 N2 H2A 108.5 . . ? C43 N2 H2A 108.5 . . ? C44 N2 H2B 108.5 . . ? C43 N2 H2B 108.5 . . ? H2A N2 H2B 107.5 . . ? C12 C11 C16 118.5(6) . . ? C12 C11 S1 118.2(5) . . ? C16 C11 S1 123.3(4) . . ? C13 C12 C11 121.1(6) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 120.0(6) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.1(6) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.7(6) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C11 119.5(5) . . ? C15 C16 S2 118.7(5) . . ? C11 C16 S2 121.8(5) . . ? C26 C21 C22 118.1(7) . . ? C26 C21 S3 124.8(5) . . ? C22 C21 S3 117.0(6) . . ? C23 C22 C21 121.8(9) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C22 C23 C24 120.9(9) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C25 119.7(8) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 120.2(9) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C21 119.3(7) . . ? C25 C26 S4 117.2(7) . . ? C21 C26 S4 123.5(5) . . ? C36 C31 C32 118.3(6) . . ? C36 C31 S5 124.3(5) . . ? C32 C31 S5 117.4(5) . . ? C33 C32 C31 122.2(7) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C32 C33 C34 118.9(7) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C35 C34 C33 119.9(7) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 121.4(6) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C35 C36 C31 119.2(6) . . ? C35 C36 S6 117.8(5) . . ? C31 C36 S6 123.0(5) . . ? N1 C41 H41A 109.5 . . ? N1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N1 C42 H42A 109.5 . . ? N1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N2 C43 H43A 109.5 . . ? N2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N2 C44 H44A 109.5 . . ? N2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N3 C45 C46 176.2(12) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S3 Sn1 S1 C11 68.0(2) . . . . ? S5 Sn1 S1 C11 156.5(2) . . . . ? S4 Sn1 S1 C11 4.8(4) . . . . ? S2 Sn1 S1 C11 -29.6(2) . . . . ? S6 Sn1 S1 C11 -120.0(2) . . . . ? S3 Sn1 S2 C16 -59.1(2) . . . . ? S1 Sn1 S2 C16 30.1(2) . . . . ? S5 Sn1 S2 C16 83.9(5) . . . . ? S4 Sn1 S2 C16 -143.4(2) . . . . ? S6 Sn1 S2 C16 126.1(2) . . . . ? S1 Sn1 S3 C21 171.3(2) . . . . ? S5 Sn1 S3 C21 77.5(2) . . . . ? S4 Sn1 S3 C21 -19.1(2) . . . . ? S2 Sn1 S3 C21 -107.0(2) . . . . ? S6 Sn1 S3 C21 42.3(4) . . . . ? S3 Sn1 S4 C26 18.1(2) . . . . ? S1 Sn1 S4 C26 81.8(4) . . . . ? S5 Sn1 S4 C26 -69.7(2) . . . . ? S2 Sn1 S4 C26 115.8(2) . . . . ? S6 Sn1 S4 C26 -152.9(2) . . . . ? S3 Sn1 S5 C31 167.8(2) . . . . ? S1 Sn1 S5 C31 77.6(2) . . . . ? S4 Sn1 S5 C31 -107.9(2) . . . . ? S2 Sn1 S5 C31 24.4(5) . . . . ? S6 Sn1 S5 C31 -18.2(2) . . . . ? S3 Sn1 S6 C36 53.0(4) . . . . ? S1 Sn1 S6 C36 -75.5(2) . . . . ? S5 Sn1 S6 C36 17.5(2) . . . . ? S4 Sn1 S6 C36 114.0(2) . . . . ? S2 Sn1 S6 C36 -157.4(2) . . . . ? Sn1 S1 C11 C12 -156.0(4) . . . . ? Sn1 S1 C11 C16 25.9(5) . . . . ? C16 C11 C12 C13 0.8(9) . . . . ? S1 C11 C12 C13 -177.5(5) . . . . ? C11 C12 C13 C14 -1.9(10) . . . . ? C12 C13 C14 C15 0.4(10) . . . . ? C13 C14 C15 C16 2.3(10) . . . . ? C14 C15 C16 C11 -3.4(9) . . . . ? C14 C15 C16 S2 175.5(5) . . . . ? C12 C11 C16 C15 1.8(9) . . . . ? S1 C11 C16 C15 -180.0(5) . . . . ? C12 C11 C16 S2 -177.0(5) . . . . ? S1 C11 C16 S2 1.2(8) . . . . ? Sn1 S2 C16 C15 154.1(5) . . . . ? Sn1 S2 C16 C11 -27.1(5) . . . . ? Sn1 S3 C21 C26 18.6(6) . . . . ? Sn1 S3 C21 C22 -164.1(5) . . . . ? C26 C21 C22 C23 2.7(10) . . . . ? S3 C21 C22 C23 -174.9(6) . . . . ? C21 C22 C23 C24 -1.1(12) . . . . ? C22 C23 C24 C25 -1.7(13) . . . . ? C23 C24 C25 C26 2.8(12) . . . . ? C24 C25 C26 C21 -1.1(10) . . . . ? C24 C25 C26 S4 177.7(6) . . . . ? C22 C21 C26 C25 -1.5(9) . . . . ? S3 C21 C26 C25 175.8(5) . . . . ? C22 C21 C26 S4 179.8(5) . . . . ? S3 C21 C26 S4 -2.9(9) . . . . ? Sn1 S4 C26 C25 166.7(5) . . . . ? Sn1 S4 C26 C21 -14.6(6) . . . . ? Sn1 S5 C31 C36 17.5(5) . . . . ? Sn1 S5 C31 C32 -165.3(4) . . . . ? C36 C31 C32 C33 1.6(10) . . . . ? S5 C31 C32 C33 -175.7(5) . . . . ? C31 C32 C33 C34 0.4(11) . . . . ? C32 C33 C34 C35 -2.5(10) . . . . ? C33 C34 C35 C36 2.4(10) . . . . ? C34 C35 C36 C31 -0.3(9) . . . . ? C34 C35 C36 S6 177.3(5) . . . . ? C32 C31 C36 C35 -1.7(9) . . . . ? S5 C31 C36 C35 175.4(5) . . . . ? C32 C31 C36 S6 -179.2(5) . . . . ? S5 C31 C36 S6 -2.1(8) . . . . ? Sn1 S6 C36 C35 168.0(4) . . . . ? Sn1 S6 C36 C31 -14.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 20.59 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.322 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.065