# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof Hugo Tlahuext' _publ_contact_author_email TLAHUEXT@CIQ.UAEM.MX _publ_section_title ; Self-Assembly of Diphenyltin(IV) and Tris-dithiocarbamate Ligands to Racemic Trinuclear Cavitands and Capsules ; loop_ _publ_author_name 'Hugo Tlahuext' "Patricia Garc\'ia y Garcia" 'Herbert Hopfl' 'Marcela Lopez-Cardoso' ; R.Reyes-Martinez ; # Attachment 'Comp-1.cif' data_marczehm _database_code_depnum_ccdc_archive 'CCDC 666754' _audit_update_record ; 2008-06-10 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 457.5 _chemical_formula_moiety 'C48 H51 Cl3 N4 S6 Sn3' _chemical_formula_sum 'C48 H51 Cl3 N4 S6 Sn3' _chemical_formula_weight 1338.71 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' Cl Cl 0.1484 0.1585 '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 10.0012(6) _cell_length_b 17.2313(10) _cell_length_c 18.2621(10) _cell_angle_alpha 115.0290(10) _cell_angle_beta 103.7920(10) _cell_angle_gamma 90.0190(10) _cell_volume 2751.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9937 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.13 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 1.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4731 _exptl_absorpt_correction_T_max 0.8034 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 26606 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9651 _reflns_number_gt 7263 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^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 9651 _refine_ls_number_parameters 580 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1275 _refine_ls_R_factor_gt 0.0931 _refine_ls_wR_factor_ref 0.1827 _refine_ls_wR_factor_gt 0.1697 _refine_ls_goodness_of_fit_ref 1.262 _refine_ls_restrained_S_all 1.262 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.2920(9) 0.2545(6) 0.1534(7) 0.049(3) Uani 1 1 d . . . H1A H -0.3385 0.3022 0.1842 0.058 Uiso 1 1 calc R . . H1B H -0.3599 0.2039 0.1223 0.058 Uiso 1 1 calc R . . C2 C -0.2378(10) 0.2753(6) 0.0923(6) 0.050(3) Uani 1 1 d . . . H2A H -0.3151 0.2823 0.0528 0.060 Uiso 1 1 calc R . . H2B H -0.1778 0.3295 0.1227 0.060 Uiso 1 1 calc R . . C3 C -0.0250(10) 0.2166(6) 0.0671(6) 0.045(2) Uani 1 1 d . . . C4 C -0.2288(10) 0.1760(6) 0.2385(6) 0.044(2) Uani 1 1 d . . . H4A H -0.3213 0.1848 0.2459 0.053 Uiso 1 1 calc R . . H4B H -0.1673 0.1835 0.2915 0.053 Uiso 1 1 calc R . . C5 C -0.2293(10) 0.0854(6) 0.1718(6) 0.048(3) Uani 1 1 d . . . H5A H -0.3018 0.0754 0.1218 0.058 Uiso 1 1 calc R . . H5B H -0.1413 0.0807 0.1575 0.058 Uiso 1 1 calc R . . C6 C -0.1478(10) -0.0161(6) 0.2273(6) 0.044(2) Uani 1 1 d . . . C7 C -0.1175(10) 0.3185(6) 0.2851(6) 0.052(3) Uani 1 1 d . . . H7A H -0.1686 0.3333 0.3273 0.062 Uiso 1 1 calc R . . H7B H -0.1172 0.3649 0.2684 0.062 Uiso 1 1 calc R . . C8 C 0.0327(10) 0.3058(6) 0.3212(6) 0.047(2) Uani 1 1 d . . . H8A H 0.0319 0.2538 0.3293 0.057 Uiso 1 1 calc R . . H8B H 0.0861 0.2985 0.2812 0.057 Uiso 1 1 calc R . . C9 C 0.0886(10) 0.3839(6) 0.4709(7) 0.053(3) Uani 1 1 d . . . C10 C -0.2420(11) 0.1273(7) -0.0175(7) 0.069(3) Uani 1 1 d . . . H10A H -0.2232 0.1155 -0.0702 0.104 Uiso 1 1 calc R . . H10B H -0.3392 0.1316 -0.0225 0.104 Uiso 1 1 calc R . . H10C H -0.2159 0.0815 -0.0023 0.104 Uiso 1 1 calc R . . C11 C -0.3938(11) -0.0048(7) 0.1935(7) 0.065(3) Uani 1 1 d . . . H11A H -0.4181 -0.0654 0.1583 0.098 Uiso 1 1 calc R . . H11B H -0.4542 0.0269 0.1700 0.098 Uiso 1 1 calc R . . H11C H -0.4032 0.0082 0.2484 0.098 Uiso 1 1 calc R . . C12 C 0.1774(12) 0.4471(8) 0.3963(7) 0.075(4) Uani 1 1 d . . . H12A H 0.1571 0.5021 0.4335 0.113 Uiso 1 1 calc R . . H12B H 0.1518 0.4415 0.3400 0.113 Uiso 1 1 calc R . . H12C H 0.2747 0.4429 0.4124 0.113 Uiso 1 1 calc R . . C13 C 0.3603(9) 0.2858(6) 0.0488(6) 0.040(2) Uani 1 1 d . . . C14 C 0.3863(13) 0.3758(9) 0.0902(8) 0.077(4) Uani 1 1 d . . . H14 H 0.3749 0.4054 0.1439 0.092 Uiso 1 1 calc R . . C15 C 0.4286(18) 0.4199(10) 0.0509(11) 0.114(6) Uani 1 1 d . . . H15 H 0.4512 0.4794 0.0788 0.137 Uiso 1 1 calc R . . C16 C 0.4370(16) 0.3760(13) -0.0284(11) 0.110(6) Uani 1 1 d . . . H16 H 0.4604 0.4064 -0.0561 0.132 Uiso 1 1 calc R . . C17 C 0.4127(15) 0.2908(12) -0.0682(9) 0.094(5) Uani 1 1 d . . . H17 H 0.4219 0.2620 -0.1225 0.113 Uiso 1 1 calc R . . C18 C 0.3748(11) 0.2459(8) -0.0298(7) 0.065(3) Uani 1 1 d . . . H18 H 0.3582 0.1861 -0.0582 0.078 Uiso 1 1 calc R . . C19 C 0.3702(10) 0.2414(7) 0.2313(6) 0.048(3) Uani 1 1 d . . . C20 C 0.3491(12) 0.1810(8) 0.2594(8) 0.066(3) Uani 1 1 d . . . H20 H 0.2962 0.1287 0.2223 0.079 Uiso 1 1 calc R . . C21 C 0.4046(18) 0.1968(11) 0.3407(10) 0.105(5) Uani 1 1 d . . . H21 H 0.3889 0.1556 0.3589 0.127 Uiso 1 1 calc R . . C22 C 0.4832(18) 0.2729(13) 0.3952(10) 0.106(5) Uani 1 1 d . . . H22 H 0.5210 0.2839 0.4508 0.127 Uiso 1 1 calc R . . C23 C 0.5063(15) 0.3328(10) 0.3684(9) 0.092(4) Uani 1 1 d . . . H23 H 0.5623 0.3841 0.4055 0.110 Uiso 1 1 calc R . . C24 C 0.4477(12) 0.3187(8) 0.2871(7) 0.069(3) Uani 1 1 d . . . H24 H 0.4605 0.3612 0.2699 0.083 Uiso 1 1 calc R . . C25 C 0.0957(13) -0.2203(7) 0.1708(7) 0.061(3) Uani 1 1 d . . . C26 C 0.2099(16) -0.2485(11) 0.1423(11) 0.106(5) Uani 1 1 d . . . H26 H 0.2939 -0.2133 0.1676 0.127 Uiso 1 1 calc R . . C27 C 0.201(2) -0.3302(13) 0.0752(12) 0.118(6) Uani 1 1 d . . . H27 H 0.2794 -0.3483 0.0561 0.141 Uiso 1 1 calc R . . C28 C 0.087(2) -0.3798(11) 0.0400(10) 0.112(6) Uani 1 1 d . . . H28 H 0.0834 -0.4339 -0.0036 0.134 Uiso 1 1 calc R . . C29 C -0.0286(19) -0.3560(12) 0.0644(13) 0.137(8) Uani 1 1 d . . . H29 H -0.1114 -0.3924 0.0379 0.164 Uiso 1 1 calc R . . C30 C -0.0214(15) -0.2758(10) 0.1300(10) 0.114(6) Uani 1 1 d . . . H30 H -0.1016 -0.2592 0.1470 0.137 Uiso 1 1 calc R . . C31 C 0.1483(12) -0.0944(8) 0.3959(7) 0.064(3) Uani 1 1 d . . . C32 C 0.2769(18) -0.0902(12) 0.4388(11) 0.124(6) Uani 1 1 d . . . H32 H 0.3479 -0.0842 0.4160 0.149 Uiso 1 1 calc R . . C33 C 0.314(2) -0.0940(14) 0.5147(12) 0.146(8) Uani 1 1 d . . . H33 H 0.4065 -0.0911 0.5413 0.175 Uiso 1 1 calc R . . C34 C 0.215(2) -0.1020(10) 0.5501(10) 0.110(6) Uani 1 1 d . . . H34 H 0.2385 -0.1050 0.6012 0.132 Uiso 1 1 calc R . . C35 C 0.080(2) -0.1056(10) 0.5106(11) 0.112(6) Uani 1 1 d . . . H35 H 0.0099 -0.1100 0.5343 0.135 Uiso 1 1 calc R . . C36 C 0.0507(17) -0.1025(9) 0.4337(10) 0.097(5) Uani 1 1 d . . . H36 H -0.0419 -0.1063 0.4062 0.117 Uiso 1 1 calc R . . C37 C 0.2559(13) 0.2830(8) 0.6291(8) 0.070(3) Uani 1 1 d . . . C38 C 0.2634(18) 0.2210(11) 0.5508(11) 0.128(7) Uani 1 1 d . . . H38 H 0.2167 0.2263 0.5029 0.154 Uiso 1 1 calc R . . C39 C 0.336(2) 0.1542(15) 0.5433(14) 0.176(10) Uani 1 1 d . . . H39 H 0.3446 0.1135 0.4916 0.212 Uiso 1 1 calc R . . C40 C 0.401(2) 0.1492(16) 0.6197(19) 0.160(10) Uani 1 1 d . . . H40 H 0.4445 0.1008 0.6172 0.192 Uiso 1 1 calc R . . C41 C 0.4007(19) 0.2093(14) 0.6919(13) 0.120(7) Uani 1 1 d . . . H41 H 0.4520 0.2069 0.7405 0.145 Uiso 1 1 calc R . . C42 C 0.3271(15) 0.2749(10) 0.6970(10) 0.095(5) Uani 1 1 d . . . H42 H 0.3251 0.3165 0.7497 0.115 Uiso 1 1 calc R . . C43 C -0.0535(15) 0.3936(7) 0.6840(8) 0.073(4) Uani 1 1 d . . . C44 C -0.1719(19) 0.3415(10) 0.6332(9) 0.108(5) Uani 1 1 d . . . H44 H -0.1733 0.3012 0.5794 0.130 Uiso 1 1 calc R . . C45 C -0.2906(19) 0.3476(12) 0.6607(12) 0.138(7) Uani 1 1 d . . . H45 H -0.3718 0.3124 0.6249 0.166 Uiso 1 1 calc R . . C46 C -0.289(2) 0.4045(12) 0.7396(12) 0.123(6) Uani 1 1 d . . . H46 H -0.3680 0.4091 0.7587 0.147 Uiso 1 1 calc R . . C47 C -0.174(2) 0.4524(11) 0.7876(11) 0.109(6) Uani 1 1 d . . . H47 H -0.1740 0.4905 0.8421 0.131 Uiso 1 1 calc R . . C48 C -0.0526(19) 0.4511(9) 0.7641(9) 0.099(5) Uani 1 1 d . . . H48 H 0.0267 0.4877 0.8009 0.119 Uiso 1 1 calc R . . Cl1 Cl 0.3935(3) 0.08446(17) 0.04105(18) 0.0597(7) Uani 1 1 d . . . Cl2 Cl 0.3352(3) -0.0405(2) 0.2837(3) 0.0877(11) Uani 1 1 d . . . Cl3 Cl 0.2800(4) 0.4957(2) 0.7674(2) 0.1062(13) Uani 1 1 d . . . N1 N -0.1822(8) 0.2385(5) 0.2132(5) 0.0437(19) Uani 1 1 d . . . N2 N -0.1621(7) 0.2090(5) 0.0473(5) 0.044(2) Uani 1 1 d . . . N3 N -0.2516(8) 0.0194(5) 0.1991(5) 0.046(2) Uani 1 1 d . . . N4 N 0.0994(8) 0.3789(6) 0.4007(6) 0.051(2) Uani 1 1 d . . . S1 S 0.0616(3) 0.12730(17) 0.02418(18) 0.0577(8) Uani 1 1 d . . . S2 S 0.0768(2) 0.31244(16) 0.13604(16) 0.0471(6) Uani 1 1 d . . . S3 S 0.0233(3) 0.01925(19) 0.2395(2) 0.0615(8) Uani 1 1 d . . . S4 S -0.1701(3) -0.09777(18) 0.25466(19) 0.0595(8) Uani 1 1 d . . . S5 S 0.1822(3) 0.46629(18) 0.56583(18) 0.0665(8) Uani 1 1 d . . . S6 S -0.0117(3) 0.30699(19) 0.47769(18) 0.0656(8) Uani 1 1 d . . . Sn1 Sn 0.28308(6) 0.21604(4) 0.10397(4) 0.0407(2) Uani 1 1 d . . . Sn2 Sn 0.10320(7) -0.09986(5) 0.27403(5) 0.0555(2) Uani 1 1 d . . . Sn3 Sn 0.12827(9) 0.38319(5) 0.63961(5) 0.0645(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(6) 0.039(6) 0.068(7) 0.022(5) 0.014(5) 0.009(4) C2 0.035(5) 0.051(6) 0.054(7) 0.022(5) -0.003(5) 0.007(5) C3 0.056(6) 0.043(6) 0.037(6) 0.021(5) 0.008(5) -0.006(5) C4 0.053(6) 0.048(6) 0.037(6) 0.023(5) 0.012(5) 0.001(5) C5 0.053(6) 0.048(6) 0.043(6) 0.023(5) 0.007(5) 0.015(5) C6 0.042(6) 0.045(6) 0.042(6) 0.018(5) 0.010(5) 0.001(5) C7 0.062(7) 0.039(6) 0.047(6) 0.012(5) 0.015(5) 0.008(5) C8 0.047(6) 0.048(6) 0.044(6) 0.018(5) 0.012(5) 0.012(5) C9 0.051(6) 0.045(6) 0.042(6) 0.006(5) 0.000(5) 0.007(5) C10 0.050(7) 0.080(9) 0.054(7) 0.015(7) 0.000(6) -0.007(6) C11 0.057(7) 0.072(8) 0.068(8) 0.036(7) 0.009(6) 0.013(6) C12 0.078(9) 0.084(9) 0.066(8) 0.037(7) 0.014(7) -0.002(7) C13 0.031(5) 0.060(7) 0.045(6) 0.040(5) 0.002(4) -0.002(5) C14 0.097(10) 0.074(9) 0.065(9) 0.037(7) 0.018(7) -0.002(7) C15 0.155(16) 0.085(11) 0.104(13) 0.047(10) 0.025(12) -0.028(10) C16 0.118(13) 0.152(17) 0.084(12) 0.081(12) 0.013(10) -0.041(12) C17 0.097(11) 0.125(14) 0.065(10) 0.047(10) 0.018(8) -0.005(10) C18 0.061(7) 0.089(9) 0.058(8) 0.047(7) 0.013(6) -0.009(6) C19 0.044(6) 0.061(7) 0.056(7) 0.038(6) 0.021(5) 0.022(5) C20 0.078(8) 0.063(8) 0.059(8) 0.029(6) 0.017(7) -0.003(6) C21 0.152(16) 0.095(12) 0.085(12) 0.060(10) 0.020(11) 0.008(11) C22 0.130(14) 0.130(15) 0.061(10) 0.051(11) 0.014(9) 0.024(12) C23 0.095(11) 0.081(10) 0.069(10) 0.016(8) 0.000(8) -0.013(8) C24 0.079(9) 0.060(8) 0.044(7) 0.008(6) -0.001(6) -0.007(6) C25 0.065(8) 0.059(7) 0.059(7) 0.035(6) 0.002(6) 0.008(6) C26 0.094(11) 0.107(13) 0.136(15) 0.056(12) 0.061(11) 0.020(9) C27 0.152(18) 0.111(15) 0.106(14) 0.040(12) 0.075(14) 0.035(13) C28 0.161(19) 0.078(12) 0.082(12) 0.038(10) 0.000(13) 0.024(13) C29 0.094(13) 0.094(14) 0.166(19) 0.034(13) -0.024(13) 0.028(11) C30 0.075(10) 0.080(11) 0.134(14) 0.010(10) 0.004(10) 0.042(9) C31 0.057(7) 0.079(9) 0.059(8) 0.045(7) -0.007(6) -0.003(6) C32 0.102(13) 0.20(2) 0.094(13) 0.095(13) 0.005(10) -0.007(12) C33 0.094(14) 0.24(2) 0.098(15) 0.081(16) -0.007(11) 0.004(14) C34 0.155(18) 0.097(12) 0.055(10) 0.025(9) 0.000(11) 0.017(12) C35 0.169(19) 0.091(12) 0.087(13) 0.042(10) 0.044(13) 0.019(12) C36 0.112(12) 0.111(12) 0.100(12) 0.078(10) 0.020(10) 0.017(9) C37 0.082(9) 0.068(8) 0.063(8) 0.036(7) 0.013(7) 0.017(7) C38 0.147(15) 0.129(14) 0.122(15) 0.060(12) 0.047(12) 0.100(13) C39 0.20(2) 0.20(2) 0.130(18) 0.066(17) 0.072(17) 0.13(2) C40 0.152(19) 0.20(2) 0.25(3) 0.17(3) 0.11(2) 0.111(18) C41 0.125(15) 0.17(2) 0.126(16) 0.107(16) 0.064(13) 0.071(14) C42 0.105(12) 0.120(13) 0.087(11) 0.061(10) 0.040(9) 0.044(10) C43 0.105(10) 0.043(7) 0.064(8) 0.025(6) 0.009(8) 0.004(7) C44 0.140(15) 0.095(12) 0.070(10) 0.012(9) 0.040(11) -0.008(11) C45 0.132(15) 0.138(16) 0.117(15) 0.015(13) 0.058(13) -0.045(12) C46 0.142(16) 0.112(14) 0.111(15) 0.021(12) 0.080(13) -0.006(12) C47 0.142(16) 0.090(12) 0.089(12) 0.015(10) 0.061(12) 0.014(11) C48 0.149(15) 0.067(9) 0.064(10) 0.014(8) 0.027(10) 0.014(9) Cl1 0.0504(15) 0.0474(15) 0.0678(18) 0.0121(14) 0.0166(14) 0.0107(12) Cl2 0.0480(17) 0.100(3) 0.137(3) 0.079(2) 0.0108(19) 0.0016(16) Cl3 0.130(3) 0.082(3) 0.061(2) 0.0130(19) -0.020(2) -0.013(2) N1 0.039(5) 0.045(5) 0.046(5) 0.023(4) 0.002(4) 0.005(4) N2 0.031(4) 0.060(5) 0.043(5) 0.027(4) 0.003(4) -0.002(4) N3 0.049(5) 0.044(5) 0.046(5) 0.022(4) 0.009(4) 0.005(4) N4 0.040(5) 0.060(6) 0.055(6) 0.031(5) 0.006(4) 0.004(4) S1 0.0479(16) 0.0437(16) 0.0634(19) 0.0068(14) 0.0138(14) -0.0015(12) S2 0.0409(14) 0.0396(14) 0.0541(16) 0.0144(12) 0.0123(12) 0.0008(11) S3 0.0467(16) 0.0621(18) 0.086(2) 0.0456(17) 0.0104(15) 0.0024(14) S4 0.0563(17) 0.0577(18) 0.073(2) 0.0391(16) 0.0125(15) 0.0004(14) S5 0.079(2) 0.0500(17) 0.0511(18) 0.0144(14) -0.0033(15) -0.0062(15) S6 0.079(2) 0.0624(19) 0.0459(17) 0.0220(15) 0.0018(15) -0.0148(16) Sn1 0.0351(4) 0.0397(4) 0.0435(4) 0.0138(3) 0.0116(3) 0.0024(3) Sn2 0.0460(4) 0.0587(5) 0.0687(6) 0.0387(4) 0.0063(4) 0.0046(4) Sn3 0.0822(6) 0.0519(5) 0.0469(5) 0.0185(4) 0.0008(4) 0.0062(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.468(12) . ? C1 C2 1.515(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.434(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.324(11) . ? C3 S2 1.725(10) . ? C3 S1 1.743(10) . ? C4 N1 1.455(11) . ? C4 C5 1.519(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.457(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.316(12) . ? C6 S4 1.711(10) . ? C6 S3 1.747(9) . ? C7 N1 1.451(11) . ? C7 C8 1.545(13) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.460(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N4 1.277(12) . ? C9 S6 1.725(11) . ? C9 S5 1.744(10) . ? C10 N2 1.470(12) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N3 1.449(12) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N4 1.452(13) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.348(14) . ? C13 C14 1.398(15) . ? C13 Sn1 2.110(8) . ? C14 C15 1.370(17) . ? C14 H14 0.9300 . ? C15 C16 1.35(2) . ? C15 H15 0.9300 . ? C16 C17 1.32(2) . ? C16 H16 0.9300 . ? C17 C18 1.349(16) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.374(14) . ? C19 C20 1.376(14) . ? C19 Sn1 2.129(10) . ? C20 C21 1.360(17) . ? C20 H20 0.9300 . ? C21 C22 1.36(2) . ? C21 H21 0.9300 . ? C22 C23 1.357(19) . ? C22 H22 0.9300 . ? C23 C24 1.373(16) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.350(17) . ? C25 C26 1.372(16) . ? C25 Sn2 2.119(12) . ? C26 C27 1.41(2) . ? C26 H26 0.9300 . ? C27 C28 1.28(2) . ? C27 H27 0.9300 . ? C28 C29 1.34(2) . ? C28 H28 0.9300 . ? C29 C30 1.38(2) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.320(18) . ? C31 C36 1.361(17) . ? C31 Sn2 2.123(11) . ? C32 C33 1.38(2) . ? C32 H32 0.9300 . ? C33 C34 1.34(2) . ? C33 H33 0.9300 . ? C34 C35 1.35(2) . ? C34 H34 0.9300 . ? C35 C36 1.388(19) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.338(16) . ? C37 C38 1.397(18) . ? C37 Sn3 2.117(12) . ? C38 C39 1.34(2) . ? C38 H38 0.9300 . ? C39 C40 1.43(3) . ? C39 H39 0.9300 . ? C40 C41 1.29(3) . ? C40 H40 0.9300 . ? C41 C42 1.33(2) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.357(18) . ? C43 C48 1.374(16) . ? C43 Sn3 2.138(14) . ? C44 C45 1.38(2) . ? C44 H44 0.9300 . ? C45 C46 1.35(2) . ? C45 H45 0.9300 . ? C46 C47 1.29(2) . ? C46 H46 0.9300 . ? C47 C48 1.38(2) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? Cl1 Sn1 2.467(3) . ? Cl2 Sn2 2.472(3) . ? Cl3 Sn3 2.447(3) . ? S1 Sn1 2.437(3) . ? S2 Sn1 2.667(2) . ? S3 Sn2 2.471(3) . ? S4 Sn2 2.673(3) . ? S5 Sn3 2.477(3) . ? S6 Sn3 2.677(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 112.9(7) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N2 C2 C1 112.0(8) . . ? N2 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? N2 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N2 C3 S2 123.0(7) . . ? N2 C3 S1 120.3(7) . . ? S2 C3 S1 116.7(6) . . ? N1 C4 C5 109.4(7) . . ? N1 C4 H4A 109.8 . . ? C5 C4 H4A 109.8 . . ? N1 C4 H4B 109.8 . . ? C5 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? N3 C5 C4 112.5(8) . . ? N3 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? N3 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N3 C6 S4 123.0(7) . . ? N3 C6 S3 120.8(7) . . ? S4 C6 S3 116.1(6) . . ? N1 C7 C8 108.2(7) . . ? N1 C7 H7A 110.0 . . ? C8 C7 H7A 110.1 . . ? N1 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? N4 C8 C7 111.9(7) . . ? N4 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N4 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N4 C9 S6 122.2(8) . . ? N4 C9 S5 121.7(9) . . ? S6 C9 S5 116.0(7) . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 118.1(10) . . ? C18 C13 Sn1 121.1(8) . . ? C14 C13 Sn1 120.6(8) . . ? C15 C14 C13 119.4(13) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C16 C15 C14 119.2(15) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 121.8(14) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 119.9(14) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C13 C18 C17 121.5(13) . . ? C13 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C24 C19 C20 118.8(11) . . ? C24 C19 Sn1 120.5(8) . . ? C20 C19 Sn1 120.7(9) . . ? C21 C20 C19 121.0(12) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 119.9(14) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 119.9(14) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.7(14) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C19 119.6(12) . . ? C23 C24 H24 120.2 . . ? C19 C24 H24 120.2 . . ? C30 C25 C26 115.3(13) . . ? C30 C25 Sn2 122.1(10) . . ? C26 C25 Sn2 122.6(11) . . ? C25 C26 C27 120.7(15) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C28 C27 C26 120.4(18) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 121.9(19) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C28 C29 C30 118.2(17) . . ? C28 C29 H29 120.9 . . ? C30 C29 H29 120.9 . . ? C25 C30 C29 123.6(15) . . ? C25 C30 H30 118.2 . . ? C29 C30 H30 118.2 . . ? C32 C31 C36 113.9(13) . . ? C32 C31 Sn2 121.5(11) . . ? C36 C31 Sn2 124.4(10) . . ? C31 C32 C33 124.8(16) . . ? C31 C32 H32 117.6 . . ? C33 C32 H32 117.6 . . ? C34 C33 C32 119.6(17) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 119.2(18) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C34 C35 C36 118.2(17) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? C31 C36 C35 124.3(15) . . ? C31 C36 H36 117.9 . . ? C35 C36 H36 117.9 . . ? C42 C37 C38 117.8(13) . . ? C42 C37 Sn3 121.1(10) . . ? C38 C37 Sn3 121.0(10) . . ? C39 C38 C37 121.4(17) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C38 C39 C40 115.8(19) . . ? C38 C39 H39 122.1 . . ? C40 C39 H39 122.1 . . ? C41 C40 C39 122.3(19) . . ? C41 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? C40 C41 C42 120.0(19) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C37 122.4(15) . . ? C41 C42 H42 118.8 . . ? C37 C42 H42 118.8 . . ? C44 C43 C48 118.7(14) . . ? C44 C43 Sn3 119.9(10) . . ? C48 C43 Sn3 121.4(12) . . ? C43 C44 C45 120.7(14) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C46 C45 C44 120.1(17) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C47 C46 C45 118.4(17) . . ? C47 C46 H46 120.8 . . ? C45 C46 H46 120.8 . . ? C46 C47 C48 124.8(16) . . ? C46 C47 H47 117.6 . . ? C48 C47 H47 117.6 . . ? C43 C48 C47 117.3(15) . . ? C43 C48 H48 121.4 . . ? C47 C48 H48 121.4 . . ? C7 N1 C4 111.5(8) . . ? C7 N1 C1 111.2(7) . . ? C4 N1 C1 113.2(7) . . ? C3 N2 C2 122.3(8) . . ? C3 N2 C10 120.0(8) . . ? C2 N2 C10 117.4(8) . . ? C6 N3 C11 122.0(8) . . ? C6 N3 C5 121.5(8) . . ? C11 N3 C5 116.5(8) . . ? C9 N4 C12 121.2(9) . . ? C9 N4 C8 122.3(9) . . ? C12 N4 C8 116.5(9) . . ? C3 S1 Sn1 89.9(3) . . ? C3 S2 Sn1 83.0(3) . . ? C6 S3 Sn2 89.8(3) . . ? C6 S4 Sn2 84.1(3) . . ? C9 S5 Sn3 89.5(4) . . ? C9 S6 Sn3 83.5(4) . . ? C13 Sn1 C19 121.7(4) . . ? C13 Sn1 S1 116.0(3) . . ? C19 Sn1 S1 121.1(3) . . ? C13 Sn1 Cl1 96.9(3) . . ? C19 Sn1 Cl1 96.9(3) . . ? S1 Sn1 Cl1 86.85(9) . . ? C13 Sn1 S2 93.9(3) . . ? C19 Sn1 S2 94.3(2) . . ? S1 Sn1 S2 70.49(8) . . ? Cl1 Sn1 S2 157.33(9) . . ? C25 Sn2 C31 118.6(4) . . ? C25 Sn2 S3 116.0(3) . . ? C31 Sn2 S3 124.7(3) . . ? C25 Sn2 Cl2 96.7(4) . . ? C31 Sn2 Cl2 97.5(3) . . ? S3 Sn2 Cl2 84.06(10) . . ? C25 Sn2 S4 97.3(3) . . ? C31 Sn2 S4 95.6(3) . . ? S3 Sn2 S4 69.42(9) . . ? Cl2 Sn2 S4 153.35(10) . . ? C37 Sn3 C43 123.7(5) . . ? C37 Sn3 Cl3 97.0(4) . . ? C43 Sn3 Cl3 97.0(4) . . ? C37 Sn3 S5 111.9(3) . . ? C43 Sn3 S5 123.1(3) . . ? Cl3 Sn3 S5 86.92(12) . . ? C37 Sn3 S6 93.9(4) . . ? C43 Sn3 S6 94.3(4) . . ? Cl3 Sn3 S6 156.32(12) . . ? S5 Sn3 S6 69.49(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 56.0(11) . . . . ? N1 C4 C5 N3 170.1(8) . . . . ? N1 C7 C8 N4 -171.8(8) . . . . ? C18 C13 C14 C15 -1.7(18) . . . . ? Sn1 C13 C14 C15 -176.2(11) . . . . ? C13 C14 C15 C16 4(2) . . . . ? C14 C15 C16 C17 -4(3) . . . . ? C15 C16 C17 C18 2(3) . . . . ? C14 C13 C18 C17 -0.2(17) . . . . ? Sn1 C13 C18 C17 174.3(10) . . . . ? C16 C17 C18 C13 0(2) . . . . ? C24 C19 C20 C21 -0.5(18) . . . . ? Sn1 C19 C20 C21 179.9(10) . . . . ? C19 C20 C21 C22 -1(2) . . . . ? C20 C21 C22 C23 0(3) . . . . ? C21 C22 C23 C24 2(3) . . . . ? C22 C23 C24 C19 -3(2) . . . . ? C20 C19 C24 C23 2.3(17) . . . . ? Sn1 C19 C24 C23 -178.2(9) . . . . ? C30 C25 C26 C27 0(2) . . . . ? Sn2 C25 C26 C27 177.9(12) . . . . ? C25 C26 C27 C28 -1(3) . . . . ? C26 C27 C28 C29 1(3) . . . . ? C27 C28 C29 C30 -1(3) . . . . ? C26 C25 C30 C29 0(2) . . . . ? Sn2 C25 C30 C29 -177.7(14) . . . . ? C28 C29 C30 C25 0(3) . . . . ? C36 C31 C32 C33 0(3) . . . . ? Sn2 C31 C32 C33 -174.0(16) . . . . ? C31 C32 C33 C34 0(3) . . . . ? C32 C33 C34 C35 0(3) . . . . ? C33 C34 C35 C36 1(3) . . . . ? C32 C31 C36 C35 1(2) . . . . ? Sn2 C31 C36 C35 174.8(11) . . . . ? C34 C35 C36 C31 -1(2) . . . . ? C42 C37 C38 C39 2(3) . . . . ? Sn3 C37 C38 C39 -175.4(17) . . . . ? C37 C38 C39 C40 2(3) . . . . ? C38 C39 C40 C41 -7(4) . . . . ? C39 C40 C41 C42 7(4) . . . . ? C40 C41 C42 C37 -3(3) . . . . ? C38 C37 C42 C41 -2(2) . . . . ? Sn3 C37 C42 C41 175.4(13) . . . . ? C48 C43 C44 C45 2(2) . . . . ? Sn3 C43 C44 C45 -179.7(14) . . . . ? C43 C44 C45 C46 -2(3) . . . . ? C44 C45 C46 C47 0(3) . . . . ? C45 C46 C47 C48 1(3) . . . . ? C44 C43 C48 C47 0(2) . . . . ? Sn3 C43 C48 C47 -179.1(11) . . . . ? C46 C47 C48 C43 -1(3) . . . . ? C8 C7 N1 C4 79.9(10) . . . . ? C8 C7 N1 C1 -152.7(8) . . . . ? C5 C4 N1 C7 -152.6(8) . . . . ? C5 C4 N1 C1 81.1(10) . . . . ? C2 C1 N1 C7 85.7(10) . . . . ? C2 C1 N1 C4 -147.8(8) . . . . ? S2 C3 N2 C2 -11.6(13) . . . . ? S1 C3 N2 C2 167.7(7) . . . . ? S2 C3 N2 C10 174.5(8) . . . . ? S1 C3 N2 C10 -6.2(12) . . . . ? C1 C2 N2 C3 -101.3(10) . . . . ? C1 C2 N2 C10 72.7(11) . . . . ? S4 C6 N3 C11 3.7(13) . . . . ? S3 C6 N3 C11 -175.9(7) . . . . ? S4 C6 N3 C5 -176.4(7) . . . . ? S3 C6 N3 C5 4.0(13) . . . . ? C4 C5 N3 C6 -99.1(10) . . . . ? C4 C5 N3 C11 80.8(11) . . . . ? S6 C9 N4 C12 176.0(8) . . . . ? S5 C9 N4 C12 -7.4(14) . . . . ? S6 C9 N4 C8 -2.8(14) . . . . ? S5 C9 N4 C8 173.7(7) . . . . ? C7 C8 N4 C9 87.1(12) . . . . ? C7 C8 N4 C12 -91.8(11) . . . . ? N2 C3 S1 Sn1 -178.9(7) . . . . ? S2 C3 S1 Sn1 0.4(5) . . . . ? N2 C3 S2 Sn1 178.9(8) . . . . ? S1 C3 S2 Sn1 -0.4(5) . . . . ? N3 C6 S3 Sn2 -173.4(8) . . . . ? S4 C6 S3 Sn2 6.9(5) . . . . ? N3 C6 S4 Sn2 173.9(8) . . . . ? S3 C6 S4 Sn2 -6.4(5) . . . . ? N4 C9 S5 Sn3 -164.9(9) . . . . ? S6 C9 S5 Sn3 11.9(5) . . . . ? N4 C9 S6 Sn3 165.7(9) . . . . ? S5 C9 S6 Sn3 -11.0(5) . . . . ? C18 C13 Sn1 C19 138.8(8) . . . . ? C14 C13 Sn1 C19 -46.8(10) . . . . ? C18 C13 Sn1 S1 -53.5(9) . . . . ? C14 C13 Sn1 S1 120.8(8) . . . . ? C18 C13 Sn1 Cl1 36.3(8) . . . . ? C14 C13 Sn1 Cl1 -149.3(8) . . . . ? C18 C13 Sn1 S2 -123.7(8) . . . . ? C14 C13 Sn1 S2 50.7(9) . . . . ? C24 C19 Sn1 C13 20.1(10) . . . . ? C20 C19 Sn1 C13 -160.4(8) . . . . ? C24 C19 Sn1 S1 -147.0(7) . . . . ? C20 C19 Sn1 S1 32.6(9) . . . . ? C24 C19 Sn1 Cl1 122.5(8) . . . . ? C20 C19 Sn1 Cl1 -57.9(8) . . . . ? C24 C19 Sn1 S2 -77.2(8) . . . . ? C20 C19 Sn1 S2 102.4(8) . . . . ? C3 S1 Sn1 C13 -84.9(4) . . . . ? C3 S1 Sn1 C19 82.8(4) . . . . ? C3 S1 Sn1 Cl1 179.0(3) . . . . ? C3 S1 Sn1 S2 -0.3(3) . . . . ? C3 S2 Sn1 C13 116.5(4) . . . . ? C3 S2 Sn1 C19 -121.3(4) . . . . ? C3 S2 Sn1 S1 0.3(3) . . . . ? C3 S2 Sn1 Cl1 -1.6(4) . . . . ? C30 C25 Sn2 C31 87.7(12) . . . . ? C26 C25 Sn2 C31 -90.2(11) . . . . ? C30 C25 Sn2 S3 -83.4(12) . . . . ? C26 C25 Sn2 S3 98.8(11) . . . . ? C30 C25 Sn2 Cl2 -170.0(11) . . . . ? C26 C25 Sn2 Cl2 12.1(11) . . . . ? C30 C25 Sn2 S4 -12.8(12) . . . . ? C26 C25 Sn2 S4 169.4(10) . . . . ? C32 C31 Sn2 C25 81.4(14) . . . . ? C36 C31 Sn2 C25 -92.5(12) . . . . ? C32 C31 Sn2 S3 -108.4(13) . . . . ? C36 C31 Sn2 S3 77.7(12) . . . . ? C32 C31 Sn2 Cl2 -20.5(13) . . . . ? C36 C31 Sn2 Cl2 165.7(11) . . . . ? C32 C31 Sn2 S4 -177.2(13) . . . . ? C36 C31 Sn2 S4 9.0(12) . . . . ? C6 S3 Sn2 C25 83.9(5) . . . . ? C6 S3 Sn2 C31 -86.5(5) . . . . ? C6 S3 Sn2 Cl2 178.5(3) . . . . ? C6 S3 Sn2 S4 -4.2(3) . . . . ? C6 S4 Sn2 C25 -110.7(4) . . . . ? C6 S4 Sn2 C31 129.4(5) . . . . ? C6 S4 Sn2 S3 4.4(3) . . . . ? C6 S4 Sn2 Cl2 10.4(5) . . . . ? C42 C37 Sn3 C43 -65.1(13) . . . . ? C38 C37 Sn3 C43 111.9(13) . . . . ? C42 C37 Sn3 Cl3 38.2(12) . . . . ? C38 C37 Sn3 Cl3 -144.8(12) . . . . ? C42 C37 Sn3 S5 127.7(11) . . . . ? C38 C37 Sn3 S5 -55.3(13) . . . . ? C42 C37 Sn3 S6 -162.8(11) . . . . ? C38 C37 Sn3 S6 14.2(13) . . . . ? C44 C43 Sn3 C37 -76.4(13) . . . . ? C48 C43 Sn3 C37 102.2(11) . . . . ? C44 C43 Sn3 Cl3 -179.7(11) . . . . ? C48 C43 Sn3 Cl3 -1.1(11) . . . . ? C44 C43 Sn3 S5 89.4(11) . . . . ? C48 C43 Sn3 S5 -92.0(11) . . . . ? C44 C43 Sn3 S6 21.1(11) . . . . ? C48 C43 Sn3 S6 -160.3(10) . . . . ? C9 S5 Sn3 C37 78.5(5) . . . . ? C9 S5 Sn3 C43 -88.7(5) . . . . ? C9 S5 Sn3 Cl3 174.9(4) . . . . ? C9 S5 Sn3 S6 -7.3(3) . . . . ? C9 S6 Sn3 C37 -104.5(5) . . . . ? C9 S6 Sn3 C43 131.3(5) . . . . ? C9 S6 Sn3 Cl3 12.9(5) . . . . ? C9 S6 Sn3 S5 7.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.290 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.126 # Attachment 'Comp-5.cif' data_comp5m _database_code_depnum_ccdc_archive 'CCDC 691697' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H96 N8 S12 Sn3,2(C H Cl3),3(C6 H6)' _chemical_formula_sum 'C116 H116 Cl6 N8 S12 Sn3' _chemical_formula_weight 2575.66 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' Cl Cl 0.1484 0.1585 '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 Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 22.2740(12) _cell_length_b 22.2740(12) _cell_length_c 13.8830(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5965.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5900 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.42 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 1.017 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7637 _exptl_absorpt_correction_T_max 0.8147 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43833 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7027 _reflns_number_gt 5787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+15.1145P] 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 7027 _refine_ls_number_parameters 470 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.793203(17) 0.140399(17) 0.26765(2) 0.02174(12) Uani 1 1 d . . . S1 S 0.68201(6) 0.07725(6) 0.36870(9) 0.0254(3) Uani 1 1 d . . . S2 S 0.77147(6) 0.22918(6) 0.37310(9) 0.0232(3) Uani 1 1 d . . . S3 S 0.72987(6) 0.18033(6) 0.13684(9) 0.0268(3) Uani 1 1 d . . . S4 S 0.88055(6) 0.24639(7) 0.16845(9) 0.0259(3) Uani 1 1 d . . . N1 N 0.65940(19) 0.16112(19) 0.4815(3) 0.0195(8) Uani 1 1 d . . . N2 N 0.6667 0.3333 0.4815(5) 0.0205(15) Uani 1 3 d S . . N3 N 0.8194(2) 0.3099(2) 0.0845(3) 0.0274(9) Uani 1 1 d . . . N4 N 0.6667 0.3333 0.1065(6) 0.0353(18) Uani 1 3 d S . . C1 C 0.7000(2) 0.1572(2) 0.4144(3) 0.0216(10) Uani 1 1 d . . . C2 C 0.6721(2) 0.2286(2) 0.5167(3) 0.0217(10) Uani 1 1 d . . . H2A H 0.7226 0.2598 0.5251 0.018(12) Uiso 1 1 calc R . . H2B H 0.6498 0.2223 0.5805 0.020(12) Uiso 1 1 calc R . . C3 C 0.6442(2) 0.2624(2) 0.4483(3) 0.0209(10) Uani 1 1 d . . . H3A H 0.6618 0.2638 0.3824 0.016(12) Uiso 1 1 calc R . . H3B H 0.5929 0.2350 0.4466 0.021(12) Uiso 1 1 calc R . . C4 C 0.8108(2) 0.2518(3) 0.1242(3) 0.0243(11) Uani 1 1 d . . . C5 C 0.7603(3) 0.3161(3) 0.0529(3) 0.0275(11) Uani 1 1 d . . . H5A H 0.7225 0.2701 0.0320 0.036(15) Uiso 1 1 calc R . . H5B H 0.7741 0.3479 -0.0029 0.021(12) Uiso 1 1 calc R . . C6 C 0.7342(3) 0.3433(3) 0.1330(4) 0.0336(12) Uani 1 1 d . . . H6A H 0.7304 0.3183 0.1936 0.037(15) Uiso 1 1 calc R . . H6B H 0.7672 0.3932 0.1435 0.021(12) Uiso 1 1 calc R . . C7 C 0.5991(2) 0.1000(2) 0.5239(3) 0.0226(10) Uani 1 1 d . . . H7A H 0.6018 0.1044 0.5949 0.025(13) Uiso 1 1 calc R . . H7B H 0.6012 0.0580 0.5066 0.016(11) Uiso 1 1 calc R . . C8 C 0.5305(2) 0.0911(2) 0.4906(3) 0.0214(10) Uani 1 1 d . . . C9 C 0.5113(2) 0.0772(2) 0.3944(3) 0.0242(11) Uani 1 1 d . . . H9 H 0.5428 0.0765 0.3490 0.019(12) Uiso 1 1 calc R . . C10 C 0.4471(3) 0.0644(3) 0.3641(4) 0.0328(12) Uani 1 1 d . . . H10 H 0.4345 0.0544 0.2982 0.032(15) Uiso 1 1 calc R . . C11 C 0.4009(3) 0.0661(3) 0.4289(4) 0.0341(13) Uani 1 1 d . . . H11 H 0.3564 0.0566 0.4081 0.034(15) Uiso 1 1 calc R . . C12 C 0.4200(3) 0.0816(3) 0.5231(4) 0.0326(13) Uani 1 1 d . . . H12 H 0.3886 0.0834 0.5677 0.040(16) Uiso 1 1 calc R . . C13 C 0.4845(3) 0.0946(2) 0.5546(4) 0.0285(12) Uani 1 1 d . . . H13 H 0.4972 0.1059 0.6202 0.035(15) Uiso 1 1 calc R . . C14 C 0.8871(3) 0.3761(3) 0.0842(4) 0.0324(12) Uani 1 1 d . . . H14A H 0.9219 0.3691 0.1192 0.041(16) Uiso 1 1 calc R . . H14B H 0.8819 0.4120 0.1190 0.045(17) Uiso 1 1 calc R . . C15 C 0.9130(2) 0.4013(2) -0.0153(4) 0.0257(11) Uani 1 1 d . . . C16 C 0.9392(3) 0.3685(3) -0.0715(5) 0.0491(17) Uani 1 1 d . . . H16 H 0.9399 0.3291 -0.0471 0.053(19) Uiso 1 1 calc R . . C17 C 0.9636(4) 0.3920(4) -0.1608(6) 0.077(3) Uani 1 1 d . . . H17 H 0.9815 0.3688 -0.1984 0.10(3) Uiso 1 1 calc R . . C18 C 0.9632(4) 0.4479(5) -0.1978(5) 0.074(3) Uani 1 1 d . . . H18 H 0.9816 0.4642 -0.2602 0.07(2) Uiso 1 1 calc R . . C19 C 0.9364(3) 0.4809(4) -0.1456(5) 0.054(2) Uani 1 1 d . . . H19 H 0.9348 0.5192 -0.1726 0.048(17) Uiso 1 1 calc R . . C20 C 0.9116(3) 0.4586(3) -0.0528(4) 0.0348(13) Uani 1 1 d . . . H20 H 0.8939 0.4821 -0.0156 0.047(17) Uiso 1 1 calc R . . C21 C 0.7742(3) 0.0527(2) 0.1803(4) 0.0260(11) Uani 1 1 d . . . C22 C 0.7791(3) 0.0549(3) 0.0809(4) 0.0312(12) Uani 1 1 d . . . H22 H 0.7899 0.0965 0.0479 0.031(14) Uiso 1 1 calc R . . C23 C 0.7684(3) -0.0023(3) 0.0290(4) 0.0441(15) Uani 1 1 d . . . H23 H 0.7726 0.0002 -0.0392 0.06(2) Uiso 1 1 calc R . . C24 C 0.7518(4) -0.0626(3) 0.0756(5) 0.0527(17) Uani 1 1 d . . . H24 H 0.7453 -0.1018 0.0397 0.06(2) Uiso 1 1 calc R . . C25 C 0.7444(4) -0.0670(3) 0.1743(5) 0.0557(18) Uani 1 1 d . . . H25 H 0.7315 -0.1093 0.2068 0.044(17) Uiso 1 1 calc R . . C26 C 0.7563(4) -0.0082(3) 0.2258(4) 0.0470(16) Uani 1 1 d . . . H26 H 0.7518 -0.0107 0.2939 0.06(2) Uiso 1 1 calc R . . C27 C 0.8704(2) 0.1474(2) 0.3681(3) 0.0255(11) Uani 1 1 d . . . C28 C 0.9277(3) 0.1466(4) 0.3319(4) 0.0545(19) Uani 1 1 d . . . H28 H 0.9323 0.1428 0.2646 0.057(19) Uiso 1 1 calc R . . C29 C 0.9785(4) 0.1515(5) 0.3947(6) 0.086(3) Uani 1 1 d . . . H29 H 1.0181 0.1512 0.3699 0.14(4) Uiso 1 1 calc R . . C30 C 0.9718(3) 0.1569(4) 0.4938(5) 0.0546(18) Uani 1 1 d . . . H30 H 1.0074 0.1616 0.5363 0.07(2) Uiso 1 1 calc R . . C31 C 0.9148(3) 0.1555(3) 0.5288(4) 0.0388(14) Uani 1 1 d . . . H31 H 0.9091 0.1573 0.5963 0.027(14) Uiso 1 1 calc R . . C32 C 0.8647(3) 0.1513(3) 0.4663(4) 0.0355(13) Uani 1 1 d . . . H32 H 0.8251 0.1512 0.4918 0.025(13) Uiso 1 1 calc R . . C33 C 0.7761(3) 0.1838(3) 0.6763(4) 0.0406(14) Uani 1 1 d . . . H33 H 0.7904 0.2072 0.6163 0.049 Uiso 1 1 calc R . . C34 C 0.7435(3) 0.1124(3) 0.6793(4) 0.0461(15) Uani 1 1 d . . . H34 H 0.7349 0.0870 0.6210 0.055 Uiso 1 1 calc R . . C35 C 0.7238(4) 0.0784(4) 0.7637(5) 0.061(2) Uani 1 1 d . . . H35 H 0.7032 0.0293 0.7655 0.074 Uiso 1 1 calc R . . C36 C 0.7340(4) 0.1162(6) 0.8499(6) 0.081(3) Uani 1 1 d . . . H36 H 0.7179 0.0925 0.9095 0.097 Uiso 1 1 calc R . . C37 C 0.7668(5) 0.1865(5) 0.8471(6) 0.081(3) Uani 1 1 d . . . H37 H 0.7756 0.2124 0.9049 0.097 Uiso 1 1 calc R . . C38 C 0.7877(4) 0.2205(4) 0.7576(6) 0.068(2) Uani 1 1 d . . . H38 H 0.8102 0.2696 0.7549 0.082 Uiso 1 1 calc R . . C51 C 0.6667 0.3333 0.7435(8) 0.051(3) Uani 1 3 d S . . H51 H 0.6667 0.3333 0.6715 0.062 Uiso 1 3 calc SR . . Cl1 Cl 0.75295(9) 0.37798(10) 0.78353(12) 0.0585(5) Uani 1 1 d . . . C52 C 1.0000 0.0000 0.0870(14) 0.252(5) Uani 0.50 3 d SPD . . H52 H 1.0000 0.0000 0.0150 0.303 Uiso 0.50 3 calc SPRD A 1 Cl2A Cl 0.9418(9) 0.0244(11) 0.1313(14) 0.252(5) Uani 0.25 1 d PD B 1 Cl2B Cl 0.9207(4) -0.0660(8) 0.1312(14) 0.252(5) Uani 0.25 1 d PD B 2 C53 C 1.0000 0.0000 0.225(2) 0.252(5) Uani 0.50 3 d SPD . 3 H53 H 1.0000 0.0000 0.2970 0.303 Uiso 0.50 3 calc SPR . 3 Cl3 Cl 0.9224(5) -0.0124(6) 0.1751(13) 0.252(5) Uani 0.50 1 d PD C 3 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 0.0227(2) 0.0220(2) 0.01931(19) -0.00069(13) 0.00284(13) 0.01035(15) S1 0.0257(6) 0.0192(6) 0.0263(7) -0.0029(5) 0.0059(5) 0.0076(5) S2 0.0201(6) 0.0189(6) 0.0259(6) -0.0007(5) 0.0050(5) 0.0063(5) S3 0.0216(6) 0.0272(7) 0.0265(7) 0.0018(5) 0.0004(5) 0.0085(5) S4 0.0222(6) 0.0315(7) 0.0227(6) 0.0022(5) 0.0024(5) 0.0124(6) N1 0.019(2) 0.020(2) 0.018(2) 0.0019(16) 0.0022(16) 0.0089(17) N2 0.018(2) 0.018(2) 0.025(4) 0.000 0.000 0.0091(11) N3 0.023(2) 0.029(2) 0.024(2) 0.0042(18) 0.0001(17) 0.0077(19) N4 0.033(3) 0.033(3) 0.040(5) 0.000 0.000 0.0164(14) C1 0.025(3) 0.022(2) 0.019(2) 0.0008(19) -0.0010(19) 0.012(2) C2 0.025(3) 0.024(3) 0.017(2) -0.0016(19) 0.0036(19) 0.012(2) C3 0.022(3) 0.022(3) 0.018(2) -0.0014(19) -0.0002(19) 0.011(2) C4 0.026(3) 0.031(3) 0.015(2) 0.000(2) 0.0028(19) 0.013(2) C5 0.026(3) 0.034(3) 0.019(3) 0.007(2) 0.001(2) 0.012(2) C6 0.036(3) 0.030(3) 0.035(3) -0.004(2) -0.005(2) 0.016(3) C7 0.023(3) 0.021(2) 0.020(2) 0.0070(19) 0.006(2) 0.008(2) C8 0.024(3) 0.013(2) 0.023(3) 0.0059(19) 0.007(2) 0.006(2) C9 0.025(3) 0.020(2) 0.027(3) 0.003(2) 0.005(2) 0.010(2) C10 0.034(3) 0.023(3) 0.040(3) -0.001(2) -0.008(2) 0.013(2) C11 0.026(3) 0.022(3) 0.051(4) 0.004(2) 0.000(3) 0.010(2) C12 0.025(3) 0.020(3) 0.055(4) 0.010(2) 0.016(3) 0.013(2) C13 0.031(3) 0.022(3) 0.028(3) 0.007(2) 0.010(2) 0.010(2) C14 0.030(3) 0.028(3) 0.030(3) 0.003(2) -0.005(2) 0.007(2) C15 0.019(3) 0.023(3) 0.028(3) 0.000(2) 0.000(2) 0.006(2) C16 0.043(4) 0.032(3) 0.069(5) 0.001(3) 0.021(3) 0.016(3) C17 0.064(5) 0.060(5) 0.070(5) -0.015(4) 0.043(4) 0.003(4) C18 0.054(5) 0.077(6) 0.028(4) -0.006(4) 0.015(3) -0.014(4) C19 0.033(3) 0.054(4) 0.051(4) 0.036(3) -0.010(3) 0.003(3) C20 0.025(3) 0.034(3) 0.045(3) 0.012(3) 0.004(2) 0.014(3) C21 0.027(3) 0.024(3) 0.025(3) -0.004(2) -0.001(2) 0.011(2) C22 0.028(3) 0.033(3) 0.029(3) -0.003(2) 0.005(2) 0.013(2) C23 0.044(4) 0.048(4) 0.031(3) -0.012(3) 0.000(3) 0.016(3) C24 0.066(5) 0.040(4) 0.047(4) -0.018(3) -0.003(3) 0.023(3) C25 0.087(5) 0.031(3) 0.049(4) 0.001(3) 0.001(4) 0.028(4) C26 0.074(5) 0.036(3) 0.034(3) -0.003(3) -0.003(3) 0.030(3) C27 0.022(3) 0.025(3) 0.025(3) 0.000(2) -0.001(2) 0.009(2) C28 0.035(3) 0.101(6) 0.026(3) 0.005(3) 0.002(3) 0.032(4) C29 0.034(4) 0.169(9) 0.056(5) 0.024(5) 0.008(3) 0.052(5) C30 0.030(3) 0.070(5) 0.045(4) 0.011(3) -0.012(3) 0.011(3) C31 0.052(4) 0.028(3) 0.025(3) -0.001(2) -0.010(3) 0.012(3) C32 0.049(4) 0.032(3) 0.031(3) -0.001(2) 0.002(3) 0.025(3) C33 0.042(3) 0.059(4) 0.029(3) 0.011(3) 0.001(3) 0.031(3) C34 0.045(4) 0.049(4) 0.033(3) -0.005(3) -0.005(3) 0.015(3) C35 0.051(4) 0.041(4) 0.068(5) 0.014(3) -0.016(4) 0.004(3) C36 0.051(5) 0.141(9) 0.041(4) 0.035(5) 0.011(4) 0.041(5) C37 0.073(6) 0.107(8) 0.066(6) -0.032(5) 0.004(5) 0.048(6) C38 0.086(6) 0.051(4) 0.076(6) -0.018(4) -0.002(4) 0.040(4) C51 0.055(4) 0.055(4) 0.045(7) 0.000 0.000 0.027(2) Cl1 0.0543(10) 0.0717(12) 0.0438(10) 0.0038(8) -0.0056(8) 0.0273(9) C52 0.153(5) 0.153(5) 0.451(17) 0.000 0.000 0.077(2) Cl2A 0.153(5) 0.153(5) 0.451(17) 0.000 0.000 0.077(2) Cl2B 0.153(5) 0.153(5) 0.451(17) 0.000 0.000 0.077(2) C53 0.153(5) 0.153(5) 0.451(17) 0.000 0.000 0.077(2) Cl3 0.153(5) 0.153(5) 0.451(17) 0.000 0.000 0.077(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 C21 2.155(5) . ? Sn1 C27 2.158(5) . ? Sn1 S1 2.5685(12) . ? Sn1 S4 2.5812(13) . ? Sn1 S2 2.6917(12) . ? Sn1 S3 2.7081(13) . ? S1 C1 1.738(5) . ? S2 C1 1.697(5) . ? S3 C4 1.717(5) . ? S4 C4 1.730(5) . ? N1 C1 1.332(6) . ? N1 C2 1.467(6) . ? N1 C7 1.474(6) . ? N2 C3 1.472(5) . ? N2 C3 1.472(5) 2_655 ? N2 C3 1.472(5) 3_665 ? N3 C4 1.331(6) . ? N3 C5 1.457(6) . ? N3 C14 1.492(6) . ? N4 C6 1.454(6) . ? N4 C6 1.454(6) 3_665 ? N4 C6 1.454(6) 2_655 ? C2 C3 1.525(6) . ? C5 C6 1.514(7) . ? C7 C8 1.512(7) . ? C8 C13 1.386(7) . ? C8 C9 1.390(7) . ? C9 C10 1.377(7) . ? C10 C11 1.380(8) . ? C11 C12 1.365(8) . ? C12 C13 1.387(7) . ? C14 C15 1.495(7) . ? C15 C16 1.380(8) . ? C15 C20 1.394(7) . ? C16 C17 1.351(10) . ? C17 C18 1.349(12) . ? C18 C19 1.364(11) . ? C19 C20 1.392(8) . ? C21 C26 1.362(8) . ? C21 C22 1.383(7) . ? C22 C23 1.377(8) . ? C23 C24 1.364(9) . ? C24 C25 1.379(9) . ? C25 C26 1.395(8) . ? C27 C32 1.377(7) . ? C27 C28 1.378(8) . ? C28 C29 1.389(9) . ? C29 C30 1.395(10) . ? C30 C31 1.345(9) . ? C31 C32 1.380(8) . ? C33 C38 1.339(9) . ? C33 C34 1.381(9) . ? C34 C35 1.345(9) . ? C35 C36 1.415(12) . ? C36 C37 1.357(12) . ? C37 C38 1.407(12) . ? C51 Cl1 1.755(4) . ? C51 Cl1 1.755(4) 3_665 ? C51 Cl1 1.755(4) 2_655 ? C52 Cl2A 1.7498(10) 3_765 ? C52 Cl2A 1.7498(10) 2_645 ? C52 Cl2A 1.7498(10) . ? C52 Cl2B 1.7500(10) 2_645 ? C52 Cl2B 1.7500(10) 3_765 ? C52 Cl2B 1.7500(10) . ? C53 Cl3 1.7502(10) . ? C53 Cl3 1.7502(10) 3_765 ? C53 Cl3 1.7502(10) 2_645 ? 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 C21 Sn1 C27 102.54(19) . . ? C21 Sn1 S1 96.46(13) . . ? C27 Sn1 S1 101.67(13) . . ? C21 Sn1 S4 104.21(14) . . ? C27 Sn1 S4 93.98(13) . . ? S1 Sn1 S4 150.67(4) . . ? C21 Sn1 S2 161.20(13) . . ? C27 Sn1 S2 91.44(13) . . ? S1 Sn1 S2 68.09(4) . . ? S4 Sn1 S2 87.04(4) . . ? C21 Sn1 S3 91.27(14) . . ? C27 Sn1 S3 159.48(13) . . ? S1 Sn1 S3 91.61(4) . . ? S4 Sn1 S3 67.67(4) . . ? S2 Sn1 S3 78.98(4) . . ? C1 S1 Sn1 88.43(16) . . ? C1 S2 Sn1 85.28(16) . . ? C4 S3 Sn1 83.98(17) . . ? C4 S4 Sn1 87.76(16) . . ? C1 N1 C2 120.7(4) . . ? C1 N1 C7 123.7(4) . . ? C2 N1 C7 115.6(4) . . ? C3 N2 C3 110.6(3) . 2_655 ? C3 N2 C3 110.6(3) . 3_665 ? C3 N2 C3 110.6(3) 2_655 3_665 ? C4 N3 C5 121.3(4) . . ? C4 N3 C14 123.0(4) . . ? C5 N3 C14 115.0(4) . . ? C6 N4 C6 113.8(3) . 3_665 ? C6 N4 C6 113.8(3) . 2_655 ? C6 N4 C6 113.8(3) 3_665 2_655 ? N1 C1 S2 121.4(4) . . ? N1 C1 S1 120.4(3) . . ? S2 C1 S1 118.2(3) . . ? N1 C2 C3 112.4(4) . . ? N2 C3 C2 109.3(4) . . ? N3 C4 S3 121.2(4) . . ? N3 C4 S4 121.2(4) . . ? S3 C4 S4 117.5(3) . . ? N3 C5 C6 111.3(4) . . ? N4 C6 C5 109.2(5) . . ? N1 C7 C8 113.2(4) . . ? C13 C8 C9 118.3(5) . . ? C13 C8 C7 121.6(4) . . ? C9 C8 C7 120.1(4) . . ? C10 C9 C8 120.8(5) . . ? C9 C10 C11 120.4(5) . . ? C12 C11 C10 119.3(5) . . ? C11 C12 C13 120.9(5) . . ? C8 C13 C12 120.3(5) . . ? N3 C14 C15 112.5(4) . . ? C16 C15 C20 118.8(5) . . ? C16 C15 C14 120.6(5) . . ? C20 C15 C14 120.5(5) . . ? C17 C16 C15 120.6(7) . . ? C18 C17 C16 121.2(7) . . ? C17 C18 C19 120.1(6) . . ? C18 C19 C20 120.1(6) . . ? C19 C20 C15 119.1(6) . . ? C26 C21 C22 118.5(5) . . ? C26 C21 Sn1 118.0(4) . . ? C22 C21 Sn1 123.6(4) . . ? C23 C22 C21 121.0(5) . . ? C24 C23 C22 120.0(6) . . ? C23 C24 C25 120.3(6) . . ? C24 C25 C26 118.9(6) . . ? C21 C26 C25 121.4(6) . . ? C32 C27 C28 118.5(5) . . ? C32 C27 Sn1 123.3(4) . . ? C28 C27 Sn1 118.2(4) . . ? C27 C28 C29 119.6(6) . . ? C28 C29 C30 120.5(7) . . ? C31 C30 C29 119.6(6) . . ? C30 C31 C32 119.8(5) . . ? C27 C32 C31 122.0(5) . . ? C38 C33 C34 120.5(6) . . ? C35 C34 C33 120.7(6) . . ? C34 C35 C36 119.4(7) . . ? C37 C36 C35 119.8(7) . . ? C36 C37 C38 119.2(7) . . ? C33 C38 C37 120.3(7) . . ? Cl1 C51 Cl1 110.5(4) . 3_665 ? Cl1 C51 Cl1 110.5(4) . 2_655 ? Cl1 C51 Cl1 110.5(4) 3_665 2_655 ? Cl2A C52 Cl2A 108.37(12) 3_765 2_645 ? Cl2A C52 Cl2A 108.37(12) 3_765 . ? Cl2A C52 Cl2A 108.37(12) 2_645 . ? Cl2B C52 Cl2B 108.41(12) 2_645 3_765 ? Cl2B C52 Cl2B 108.41(12) 2_645 . ? Cl2B C52 Cl2B 108.41(12) 3_765 . ? Cl3 C53 Cl3 105.4(9) . 3_765 ? Cl3 C53 Cl3 105.4(9) . 2_645 ? Cl3 C53 Cl3 105.4(9) 3_765 2_645 ? 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 C21 Sn1 S1 C1 -169.9(2) . . . . ? C27 Sn1 S1 C1 85.8(2) . . . . ? S4 Sn1 S1 C1 -35.01(18) . . . . ? S2 Sn1 S1 C1 -1.02(16) . . . . ? S3 Sn1 S1 C1 -78.46(16) . . . . ? C21 Sn1 S2 C1 37.4(5) . . . . ? C27 Sn1 S2 C1 -101.0(2) . . . . ? S1 Sn1 S2 C1 1.04(16) . . . . ? S4 Sn1 S2 C1 165.13(16) . . . . ? S3 Sn1 S2 C1 97.31(16) . . . . ? C21 Sn1 S3 C4 -115.3(2) . . . . ? C27 Sn1 S3 C4 17.5(4) . . . . ? S1 Sn1 S3 C4 148.21(16) . . . . ? S4 Sn1 S3 C4 -10.42(16) . . . . ? S2 Sn1 S3 C4 80.90(16) . . . . ? C21 Sn1 S4 C4 95.7(2) . . . . ? C27 Sn1 S4 C4 -160.2(2) . . . . ? S1 Sn1 S4 C4 -37.71(19) . . . . ? S2 Sn1 S4 C4 -69.00(16) . . . . ? S3 Sn1 S4 C4 10.30(16) . . . . ? C2 N1 C1 S2 4.8(6) . . . . ? C7 N1 C1 S2 -176.3(3) . . . . ? C2 N1 C1 S1 -176.7(3) . . . . ? C7 N1 C1 S1 2.1(6) . . . . ? Sn1 S2 C1 N1 176.8(4) . . . . ? Sn1 S2 C1 S1 -1.6(3) . . . . ? Sn1 S1 C1 N1 -176.8(4) . . . . ? Sn1 S1 C1 S2 1.7(3) . . . . ? C1 N1 C2 C3 79.8(5) . . . . ? C7 N1 C2 C3 -99.1(4) . . . . ? C3 N2 C3 C2 82.7(6) 2_655 . . . ? C3 N2 C3 C2 -154.3(4) 3_665 . . . ? N1 C2 C3 N2 -172.6(4) . . . . ? C5 N3 C4 S3 2.0(6) . . . . ? C14 N3 C4 S3 171.3(4) . . . . ? C5 N3 C4 S4 -175.9(4) . . . . ? C14 N3 C4 S4 -6.6(6) . . . . ? Sn1 S3 C4 N3 -161.6(4) . . . . ? Sn1 S3 C4 S4 16.4(2) . . . . ? Sn1 S4 C4 N3 160.8(4) . . . . ? Sn1 S4 C4 S3 -17.1(3) . . . . ? C4 N3 C5 C6 90.1(6) . . . . ? C14 N3 C5 C6 -80.1(5) . . . . ? C6 N4 C6 C5 87.0(8) 3_665 . . . ? C6 N4 C6 C5 -140.3(6) 2_655 . . . ? N3 C5 C6 N4 -166.8(4) . . . . ? C1 N1 C7 C8 -107.9(5) . . . . ? C2 N1 C7 C8 71.0(5) . . . . ? N1 C7 C8 C13 -116.9(5) . . . . ? N1 C7 C8 C9 64.8(6) . . . . ? C13 C8 C9 C10 -2.6(7) . . . . ? C7 C8 C9 C10 175.7(4) . . . . ? C8 C9 C10 C11 0.8(7) . . . . ? C9 C10 C11 C12 1.0(8) . . . . ? C10 C11 C12 C13 -0.9(8) . . . . ? C9 C8 C13 C12 2.7(7) . . . . ? C7 C8 C13 C12 -175.7(4) . . . . ? C11 C12 C13 C8 -0.9(7) . . . . ? C4 N3 C14 C15 119.4(5) . . . . ? C5 N3 C14 C15 -70.6(6) . . . . ? N3 C14 C15 C16 -73.2(6) . . . . ? N3 C14 C15 C20 107.3(5) . . . . ? C20 C15 C16 C17 0.7(9) . . . . ? C14 C15 C16 C17 -178.9(6) . . . . ? C15 C16 C17 C18 -0.1(12) . . . . ? C16 C17 C18 C19 -1.4(12) . . . . ? C17 C18 C19 C20 2.2(10) . . . . ? C18 C19 C20 C15 -1.5(9) . . . . ? C16 C15 C20 C19 0.1(8) . . . . ? C14 C15 C20 C19 179.6(5) . . . . ? C27 Sn1 C21 C26 54.3(5) . . . . ? S1 Sn1 C21 C26 -49.2(5) . . . . ? S4 Sn1 C21 C26 151.8(4) . . . . ? S2 Sn1 C21 C26 -82.9(6) . . . . ? S3 Sn1 C21 C26 -141.0(5) . . . . ? C27 Sn1 C21 C22 -125.9(4) . . . . ? S1 Sn1 C21 C22 130.6(4) . . . . ? S4 Sn1 C21 C22 -28.4(4) . . . . ? S2 Sn1 C21 C22 97.0(5) . . . . ? S3 Sn1 C21 C22 38.8(4) . . . . ? C26 C21 C22 C23 -2.2(8) . . . . ? Sn1 C21 C22 C23 178.0(4) . . . . ? C21 C22 C23 C24 1.0(9) . . . . ? C22 C23 C24 C25 1.1(10) . . . . ? C23 C24 C25 C26 -1.9(11) . . . . ? C22 C21 C26 C25 1.3(9) . . . . ? Sn1 C21 C26 C25 -178.8(5) . . . . ? C24 C25 C26 C21 0.7(11) . . . . ? C21 Sn1 C27 C32 -129.0(4) . . . . ? S1 Sn1 C27 C32 -29.6(4) . . . . ? S4 Sn1 C27 C32 125.5(4) . . . . ? S2 Sn1 C27 C32 38.3(4) . . . . ? S3 Sn1 C27 C32 99.8(5) . . . . ? C21 Sn1 C27 C28 49.7(5) . . . . ? S1 Sn1 C27 C28 149.2(5) . . . . ? S4 Sn1 C27 C28 -55.8(5) . . . . ? S2 Sn1 C27 C28 -142.9(5) . . . . ? S3 Sn1 C27 C28 -81.5(6) . . . . ? C32 C27 C28 C29 -1.6(10) . . . . ? Sn1 C27 C28 C29 179.6(6) . . . . ? C27 C28 C29 C30 0.3(13) . . . . ? C28 C29 C30 C31 1.8(13) . . . . ? C29 C30 C31 C32 -2.5(10) . . . . ? C28 C27 C32 C31 1.0(8) . . . . ? Sn1 C27 C32 C31 179.7(4) . . . . ? C30 C31 C32 C27 1.1(9) . . . . ? C38 C33 C34 C35 -1.0(10) . . . . ? C33 C34 C35 C36 2.8(10) . . . . ? C34 C35 C36 C37 -3.6(12) . . . . ? C35 C36 C37 C38 2.6(12) . . . . ? C34 C33 C38 C37 0.0(11) . . . . ? C36 C37 C38 C33 -0.8(12) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.260 _refine_diff_density_min -1.350 _refine_diff_density_rms 0.112 # Attachment 'Comp-4.cif' data_bromom _database_code_depnum_ccdc_archive 'CCDC 691815' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H96 N8 S12 Sn3, 2(C H Br3)' _chemical_formula_sum 'C74 H98 Br6 N8 S12 Sn3' _chemical_formula_weight 2319.85 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' Br Br -0.2901 2.4595 '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 Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 16.423(5) _cell_length_b 16.423(5) _cell_length_c 59.95(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14005(9) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6728 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 25.65 _exptl_crystal_description rhombohedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6900 _exptl_absorpt_coefficient_mu 3.675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3435 _exptl_absorpt_correction_T_max 0.4438 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 21255 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -71 _diffrn_reflns_limit_l_max 71 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2757 _reflns_number_gt 2278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+22.2803P] 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 2757 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 0.28986(2) 0.3333 0.0833 0.04953(18) Uani 1 2 d S . . S1 S 0.40776(9) 0.48252(9) 0.06237(2) 0.0599(3) Uani 1 1 d . . . S2 S 0.40091(9) 0.30231(9) 0.05542(2) 0.0622(4) Uani 1 1 d . . . N1 N 0.5348(2) 0.4646(2) 0.03847(6) 0.0468(8) Uani 1 1 d . . . N2 N 0.6667 0.3333 0.04026(11) 0.0483(15) Uani 1 3 d S . . C1 C 0.4567(3) 0.4208(3) 0.05066(7) 0.0496(11) Uani 1 1 d . . . C2 C 0.5787(3) 0.4118(3) 0.03037(7) 0.0477(10) Uani 1 1 d . . . H2A H 0.6149 0.4421 0.0171 0.057 Uiso 1 1 calc R . . H2B H 0.5299 0.3490 0.0262 0.057 Uiso 1 1 calc R . . C3 C 0.6428(3) 0.4042(3) 0.04741(7) 0.0478(10) Uani 1 1 d . . . H3A H 0.6998 0.4646 0.0490 0.057 Uiso 1 1 calc R . . H3B H 0.6116 0.3867 0.0618 0.057 Uiso 1 1 calc R . . C4 C 0.5831(4) 0.5679(3) 0.03488(8) 0.0575(12) Uani 1 1 d . . . H4 H 0.5337 0.5847 0.0355 0.069 Uiso 1 1 calc R . . C5 C 0.6471(5) 0.6183(4) 0.05353(13) 0.107(2) Uani 1 1 d . . . H5A H 0.6176 0.5888 0.0674 0.161 Uiso 1 1 calc R . . H5B H 0.6613 0.6825 0.0536 0.161 Uiso 1 1 calc R . . H5C H 0.7042 0.6163 0.0518 0.161 Uiso 1 1 calc R . . C6 C 0.6261(5) 0.5962(5) 0.01180(11) 0.095(2) Uani 1 1 d . . . H6A H 0.6844 0.5959 0.0114 0.142 Uiso 1 1 calc R . . H6B H 0.6374 0.6581 0.0084 0.142 Uiso 1 1 calc R . . H6C H 0.5836 0.5523 0.0010 0.142 Uiso 1 1 calc R . . C7 C 0.1726(3) 0.2608(3) 0.06085(8) 0.0540(11) Uani 1 1 d . . . C8 C 0.1790(5) 0.2713(5) 0.03805(9) 0.0819(17) Uani 1 1 d . . . H8 H 0.2359 0.3142 0.0315 0.098 Uiso 1 1 calc R . . C9 C 0.1006(7) 0.2181(7) 0.02477(11) 0.115(3) Uani 1 1 d . . . H9 H 0.1053 0.2260 0.0094 0.138 Uiso 1 1 calc R . . C10 C 0.0165(7) 0.1541(6) 0.03411(17) 0.116(3) Uani 1 1 d . . . H10 H -0.0354 0.1177 0.0251 0.139 Uiso 1 1 calc R . . C11 C 0.0095(5) 0.1442(5) 0.05658(15) 0.100(2) Uani 1 1 d . . . H11 H -0.0476 0.1011 0.0630 0.120 Uiso 1 1 calc R . . C12 C 0.0863(4) 0.1973(4) 0.06999(10) 0.0697(14) Uani 1 1 d . . . H12 H 0.0800 0.1905 0.0854 0.084 Uiso 1 1 calc R . . C13 C 0.3333 0.6667 0.01610(15) 0.061(2) Uani 1 3 d S . . H13 H 0.3333 0.6667 -0.0002 0.074 Uiso 1 3 calc SR . . Br1 Br 0.25962(4) 0.53847(4) 0.025521(10) 0.0770(2) 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 0.0415(2) 0.0562(3) 0.0558(3) 0.0088(2) 0.00439(10) 0.02812(15) S1 0.0643(8) 0.0571(8) 0.0738(8) 0.0140(6) 0.0232(6) 0.0419(7) S2 0.0521(7) 0.0483(7) 0.0922(9) 0.0099(6) 0.0190(6) 0.0296(6) N1 0.049(2) 0.046(2) 0.053(2) 0.0092(16) 0.0110(17) 0.0292(18) N2 0.034(2) 0.034(2) 0.076(4) 0.000 0.000 0.0172(10) C1 0.051(3) 0.052(3) 0.054(3) 0.004(2) 0.002(2) 0.032(2) C2 0.052(3) 0.051(3) 0.048(2) 0.004(2) 0.011(2) 0.033(2) C3 0.043(2) 0.041(2) 0.063(3) -0.003(2) 0.003(2) 0.023(2) C4 0.063(3) 0.052(3) 0.066(3) 0.012(2) 0.013(2) 0.035(3) C5 0.136(6) 0.059(4) 0.106(5) -0.007(4) -0.010(5) 0.033(4) C6 0.114(5) 0.067(4) 0.085(4) 0.024(3) 0.026(4) 0.031(4) C7 0.055(3) 0.065(3) 0.057(3) -0.003(2) -0.008(2) 0.041(3) C8 0.089(4) 0.121(5) 0.059(3) 0.001(3) 0.003(3) 0.069(4) C9 0.151(8) 0.187(9) 0.062(4) -0.045(5) -0.039(5) 0.126(7) C10 0.111(6) 0.124(7) 0.131(8) -0.053(6) -0.062(6) 0.073(6) C11 0.073(4) 0.081(5) 0.135(7) -0.007(4) -0.027(4) 0.030(4) C12 0.059(3) 0.073(4) 0.076(3) 0.002(3) -0.011(3) 0.032(3) C13 0.060(3) 0.060(3) 0.064(5) 0.000 0.000 0.0300(16) Br1 0.0752(4) 0.0638(4) 0.0862(4) 0.0165(3) 0.0047(3) 0.0305(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C7 2.156(5) 17_554 ? Sn1 C7 2.156(5) . ? Sn1 S1 2.5667(14) 17_554 ? Sn1 S1 2.5667(14) . ? Sn1 S2 2.7047(14) 17_554 ? Sn1 S2 2.7047(14) . ? S1 C1 1.727(4) . ? S2 C1 1.710(5) . ? N1 C1 1.332(5) . ? N1 C2 1.462(5) . ? N1 C4 1.486(6) . ? N2 C3 1.465(5) 3_665 ? N2 C3 1.465(5) 2_655 ? N2 C3 1.465(5) . ? C2 C3 1.516(6) . ? C4 C5 1.473(8) . ? C4 C6 1.517(7) . ? C7 C8 1.375(7) . ? C7 C12 1.386(7) . ? C8 C9 1.389(10) . ? C9 C10 1.370(11) . ? C10 C11 1.355(11) . ? C11 C12 1.377(8) . ? C13 Br1 1.915(3) 3_565 ? C13 Br1 1.915(3) . ? C13 Br1 1.915(3) 2_665 ? 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 C7 Sn1 C7 103.8(2) 17_554 . ? C7 Sn1 S1 105.09(14) 17_554 17_554 ? C7 Sn1 S1 94.68(13) . 17_554 ? C7 Sn1 S1 94.68(13) 17_554 . ? C7 Sn1 S1 105.09(14) . . ? S1 Sn1 S1 147.83(6) 17_554 . ? C7 Sn1 S2 90.53(13) 17_554 17_554 ? C7 Sn1 S2 159.85(12) . 17_554 ? S1 Sn1 S2 67.61(4) 17_554 17_554 ? S1 Sn1 S2 87.43(5) . 17_554 ? C7 Sn1 S2 159.85(12) 17_554 . ? C7 Sn1 S2 90.52(13) . . ? S1 Sn1 S2 87.42(5) 17_554 . ? S1 Sn1 S2 67.60(4) . . ? S2 Sn1 S2 79.56(7) 17_554 . ? C1 S1 Sn1 89.38(16) . . ? C1 S2 Sn1 85.24(15) . . ? C1 N1 C2 119.3(3) . . ? C1 N1 C4 121.0(4) . . ? C2 N1 C4 119.3(3) . . ? C3 N2 C3 111.8(3) 3_665 2_655 ? C3 N2 C3 111.8(3) 3_665 . ? C3 N2 C3 111.8(3) 2_655 . ? N1 C1 S2 122.0(3) . . ? N1 C1 S1 120.8(3) . . ? S2 C1 S1 117.3(3) . . ? N1 C2 C3 113.2(4) . . ? N2 C3 C2 109.9(4) . . ? C5 C4 N1 110.8(4) . . ? C5 C4 C6 115.3(5) . . ? N1 C4 C6 112.5(4) . . ? C8 C7 C12 118.2(5) . . ? C8 C7 Sn1 124.1(4) . . ? C12 C7 Sn1 117.6(4) . . ? C7 C8 C9 120.2(7) . . ? C10 C9 C8 120.7(7) . . ? C11 C10 C9 119.4(7) . . ? C10 C11 C12 120.6(7) . . ? C11 C12 C7 120.9(6) . . ? Br1 C13 Br1 111.7(2) 3_565 . ? Br1 C13 Br1 111.7(2) 3_565 2_665 ? Br1 C13 Br1 111.7(2) . 2_665 ? 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 C7 Sn1 S1 C1 165.9(2) 17_554 . . . ? C7 Sn1 S1 C1 -88.4(2) . . . . ? S1 Sn1 S1 C1 37.52(15) 17_554 . . . ? S2 Sn1 S1 C1 75.55(16) 17_554 . . . ? S2 Sn1 S1 C1 -4.21(16) . . . . ? C7 Sn1 S2 C1 -25.6(4) 17_554 . . . ? C7 Sn1 S2 C1 110.4(2) . . . . ? S1 Sn1 S2 C1 -154.95(16) 17_554 . . . ? S1 Sn1 S2 C1 4.27(16) . . . . ? S2 Sn1 S2 C1 -87.26(16) 17_554 . . . ? C2 N1 C1 S2 -5.0(6) . . . . ? C4 N1 C1 S2 -178.9(3) . . . . ? C2 N1 C1 S1 174.9(3) . . . . ? C4 N1 C1 S1 1.0(6) . . . . ? Sn1 S2 C1 N1 173.3(4) . . . . ? Sn1 S2 C1 S1 -6.6(2) . . . . ? Sn1 S1 C1 N1 -173.0(4) . . . . ? Sn1 S1 C1 S2 6.9(3) . . . . ? C1 N1 C2 C3 -83.8(5) . . . . ? C4 N1 C2 C3 90.2(5) . . . . ? C3 N2 C3 C2 147.5(4) 3_665 . . . ? C3 N2 C3 C2 -86.2(6) 2_655 . . . ? N1 C2 C3 N2 167.0(3) . . . . ? C1 N1 C4 C5 84.9(6) . . . . ? C2 N1 C4 C5 -89.0(6) . . . . ? C1 N1 C4 C6 -144.4(5) . . . . ? C2 N1 C4 C6 41.7(6) . . . . ? C7 Sn1 C7 C8 123.5(5) 17_554 . . . ? S1 Sn1 C7 C8 -129.7(4) 17_554 . . . ? S1 Sn1 C7 C8 24.7(4) . . . . ? S2 Sn1 C7 C8 -102.2(5) 17_554 . . . ? S2 Sn1 C7 C8 -42.3(4) . . . . ? C7 Sn1 C7 C12 -58.8(4) 17_554 . . . ? S1 Sn1 C7 C12 48.0(4) 17_554 . . . ? S1 Sn1 C7 C12 -157.6(4) . . . . ? S2 Sn1 C7 C12 75.5(6) 17_554 . . . ? S2 Sn1 C7 C12 135.5(4) . . . . ? C12 C7 C8 C9 -1.0(8) . . . . ? Sn1 C7 C8 C9 176.7(5) . . . . ? C7 C8 C9 C10 -0.6(11) . . . . ? C8 C9 C10 C11 1.3(12) . . . . ? C9 C10 C11 C12 -0.4(12) . . . . ? C10 C11 C12 C7 -1.2(10) . . . . ? C8 C7 C12 C11 1.9(8) . . . . ? Sn1 C7 C12 C11 -176.0(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.039 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.095