#Supplementary Material (ESI) for Chemical Communications #This journal is © The Royal Society of Chemistry 2006 data_s152_ms_compound_1 _database_code_depnum_ccdc_archive 'CCDC 262592' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris[mu2-bis(trimethylsilyl)stibido]-tris-dimethylthallan ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H72 Sb3 Si6 Tl3' _chemical_formula_sum 'C24 H72 Sb3 Si6 Tl3' _chemical_formula_weight 1507.72 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n #(No.14) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6404(4) _cell_length_b 20.7836(9) _cell_length_c 24.7602(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.761(2) _cell_angle_gamma 90.00 _cell_volume 4926.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7535 _cell_measurement_theta_min 1 _cell_measurement_theta_max 26.4 _exptl_crystal_description rods _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.033 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 11.557 _exptl_absorpt_correction_type 'empirical from multiple refl.' _exptl_absorpt_correction_T_min 0.1877 _exptl_absorpt_correction_T_max 0.2356 _exptl_absorpt_process_details 'MULABS (Platon, cf. Blessing, 1995)' _exptl_special_details ; dx = 40 mm, 240 sec./deg., 0.5 deg., 2 sets, 440 frames, mos.= 1.158(2) deg. ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 0.5 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20129 _diffrn_reflns_av_R_equivalents 0.0841 _diffrn_reflns_av_sigmaI/netI 0.1425 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8547 _reflns_number_gt 4722 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-NT _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^+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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8547 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1077 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.824 _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 Tl1 Tl 0.25683(5) 0.36025(2) 0.22971(2) 0.03631(14) Uani 1 1 d . . . Tl2 Tl 0.30216(5) 0.11801(2) 0.24147(2) 0.03560(14) Uani 1 1 d . . . Tl3 Tl 0.51450(5) 0.24192(2) 0.08459(2) 0.03627(14) Uani 1 1 d . . . Sb1 Sb 0.36944(8) 0.24502(3) 0.28492(3) 0.0306(2) Uani 1 1 d . . . Sb2 Sb 0.38900(8) 0.13220(3) 0.13214(3) 0.0306(2) Uani 1 1 d . . . Sb3 Sb 0.39115(8) 0.35284(3) 0.13062(3) 0.0324(2) Uani 1 1 d . . . Si1 Si 0.2571(3) 0.24605(15) 0.37293(14) 0.0369(9) Uani 1 1 d . . . Si2 Si 0.6293(3) 0.24818(15) 0.31721(15) 0.0399(9) Uani 1 1 d . . . Si3 Si 0.1796(3) 0.09824(15) 0.06442(15) 0.0361(9) Uani 1 1 d . . . Si4 Si 0.5720(4) 0.04736(15) 0.11623(16) 0.0399(10) Uani 1 1 d . . . Si5 Si 0.5863(4) 0.43667(15) 0.13284(17) 0.0426(10) Uani 1 1 d . . . Si6 Si 0.2148(4) 0.39786(15) 0.05517(16) 0.0440(10) Uani 1 1 d . . . C1 C 0.0395(10) 0.3337(6) 0.2004(6) 0.060(4) Uani 1 1 d . . . H1A H 0.0389 0.2940 0.1791 0.091 Uiso 1 1 calc R . . H1B H -0.0042 0.3684 0.1775 0.091 Uiso 1 1 calc R . . H1C H -0.0128 0.3270 0.2316 0.091 Uiso 1 1 calc R . . C2 C 0.3475(13) 0.4429(5) 0.2794(6) 0.058(4) Uani 1 1 d . . . H2A H 0.4496 0.4394 0.2844 0.087 Uiso 1 1 calc R . . H2B H 0.3126 0.4423 0.3151 0.087 Uiso 1 1 calc R . . H2C H 0.3201 0.4833 0.2608 0.087 Uiso 1 1 calc R . . C3 C 0.0716(10) 0.1197(5) 0.2317(6) 0.053(4) Uani 1 1 d . . . H3A H 0.0384 0.1578 0.2107 0.080 Uiso 1 1 calc R . . H3B H 0.0384 0.1212 0.2676 0.080 Uiso 1 1 calc R . . H3C H 0.0357 0.0809 0.2124 0.080 Uiso 1 1 calc R . . C4 C 0.4567(11) 0.0502(5) 0.2821(5) 0.045(4) Uani 1 1 d . . . H4A H 0.5511 0.0652 0.2777 0.068 Uiso 1 1 calc R . . H4B H 0.4419 0.0075 0.2657 0.068 Uiso 1 1 calc R . . H4C H 0.4457 0.0478 0.3209 0.068 Uiso 1 1 calc R . . C5 C 0.7427(10) 0.2438(5) 0.1125(5) 0.046(4) Uani 1 1 d . . . H5A H 0.7576 0.2429 0.1523 0.070 Uiso 1 1 calc R . . H5B H 0.7836 0.2832 0.0994 0.070 Uiso 1 1 calc R . . H5C H 0.7874 0.2063 0.0980 0.070 Uiso 1 1 calc R . . C6 C 0.4520(15) 0.2441(6) -0.0037(5) 0.065(4) Uani 1 1 d . . . H6A H 0.3499 0.2431 -0.0109 0.098 Uiso 1 1 calc R . . H6B H 0.4912 0.2067 -0.0206 0.098 Uiso 1 1 calc R . . H6C H 0.4871 0.2836 -0.0189 0.098 Uiso 1 1 calc R . . C7 C 0.0702(12) 0.2684(6) 0.3530(5) 0.056(4) Uani 1 1 d . . . H7A H 0.0653 0.3114 0.3366 0.083 Uiso 1 1 calc R . . H7B H 0.0205 0.2685 0.3853 0.083 Uiso 1 1 calc R . . H7C H 0.0268 0.2371 0.3266 0.083 Uiso 1 1 calc R . . C8 C 0.2659(13) 0.1632(6) 0.4041(5) 0.060(4) Uani 1 1 d . . . H8A H 0.3638 0.1510 0.4140 0.091 Uiso 1 1 calc R . . H8B H 0.2210 0.1322 0.3778 0.091 Uiso 1 1 calc R . . H8C H 0.2173 0.1633 0.4367 0.091 Uiso 1 1 calc R . . C9 C 0.3369(13) 0.3042(6) 0.4244(5) 0.067(4) Uani 1 1 d . . . H9A H 0.3339 0.3474 0.4086 0.101 Uiso 1 1 calc R . . H9B H 0.4342 0.2920 0.4357 0.101 Uiso 1 1 calc R . . H9C H 0.2847 0.3037 0.4561 0.101 Uiso 1 1 calc R . . C10 C 0.6729(12) 0.1904(5) 0.3743(5) 0.051(4) Uani 1 1 d . . . H10A H 0.6247 0.2033 0.4054 0.076 Uiso 1 1 calc R . . H10B H 0.7740 0.1906 0.3851 0.076 Uiso 1 1 calc R . . H10C H 0.6429 0.1471 0.3626 0.076 Uiso 1 1 calc R . . C11 C 0.6857(11) 0.3304(5) 0.3409(5) 0.048(4) Uani 1 1 d . . . H11A H 0.6366 0.3426 0.3719 0.072 Uiso 1 1 calc R . . H11B H 0.6634 0.3612 0.3112 0.072 Uiso 1 1 calc R . . H11C H 0.7866 0.3304 0.3521 0.072 Uiso 1 1 calc R . . C12 C 0.7181(12) 0.2245(6) 0.2589(5) 0.053(4) Uani 1 1 d . . . H12A H 0.6949 0.2551 0.2291 0.079 Uiso 1 1 calc R . . H12B H 0.6876 0.1813 0.2469 0.079 Uiso 1 1 calc R . . H12C H 0.8193 0.2244 0.2694 0.079 Uiso 1 1 calc R . . C13 C 0.2156(12) 0.1032(5) -0.0067(5) 0.052(4) Uani 1 1 d . . . H13A H 0.2927 0.0742 -0.0123 0.078 Uiso 1 1 calc R . . H13B H 0.2412 0.1474 -0.0149 0.078 Uiso 1 1 calc R . . H13C H 0.1319 0.0906 -0.0307 0.078 Uiso 1 1 calc R . . C14 C 0.1212(12) 0.0152(5) 0.0768(6) 0.059(4) Uani 1 1 d . . . H14A H 0.1024 0.0110 0.1147 0.089 Uiso 1 1 calc R . . H14B H 0.1944 -0.0153 0.0697 0.089 Uiso 1 1 calc R . . H14C H 0.0357 0.0058 0.0525 0.089 Uiso 1 1 calc R . . C15 C 0.0350(12) 0.1530(6) 0.0748(6) 0.065(4) Uani 1 1 d . . . H15A H 0.0171 0.1512 0.1129 0.097 Uiso 1 1 calc R . . H15B H -0.0493 0.1398 0.0513 0.097 Uiso 1 1 calc R . . H15C H 0.0601 0.1970 0.0657 0.097 Uiso 1 1 calc R . . C16 C 0.6388(12) 0.0649(5) 0.0488(5) 0.054(4) Uani 1 1 d . . . H16A H 0.5613 0.0624 0.0195 0.081 Uiso 1 1 calc R . . H16B H 0.7103 0.0332 0.0423 0.081 Uiso 1 1 calc R . . H16C H 0.6795 0.1081 0.0496 0.081 Uiso 1 1 calc R . . C17 C 0.7231(11) 0.0525(6) 0.1703(5) 0.055(4) Uani 1 1 d . . . H17A H 0.7623 0.0961 0.1710 0.082 Uiso 1 1 calc R . . H17B H 0.7946 0.0214 0.1628 0.082 Uiso 1 1 calc R . . H17C H 0.6917 0.0429 0.2057 0.082 Uiso 1 1 calc R . . C18 C 0.5016(13) -0.0358(5) 0.1164(6) 0.066(5) Uani 1 1 d . . . H18A H 0.4214 -0.0397 0.0884 0.099 Uiso 1 1 calc R . . H18B H 0.4720 -0.0452 0.1521 0.099 Uiso 1 1 calc R . . H18C H 0.5742 -0.0664 0.1089 0.099 Uiso 1 1 calc R . . C19 C 0.6929(13) 0.4197(5) 0.0751(6) 0.062(4) Uani 1 1 d . . . H19A H 0.6335 0.4241 0.0404 0.093 Uiso 1 1 calc R . . H19B H 0.7300 0.3758 0.0786 0.093 Uiso 1 1 calc R . . H19C H 0.7704 0.4504 0.0765 0.093 Uiso 1 1 calc R . . C20 C 0.5132(13) 0.5202(5) 0.1273(6) 0.066(5) Uani 1 1 d . . . H20A H 0.4542 0.5250 0.0925 0.099 Uiso 1 1 calc R . . H20B H 0.5900 0.5513 0.1293 0.099 Uiso 1 1 calc R . . H20C H 0.4572 0.5279 0.1572 0.099 Uiso 1 1 calc R . . C21 C 0.6990(13) 0.4290(6) 0.1984(6) 0.068(5) Uani 1 1 d . . . H21A H 0.7374 0.3853 0.2019 0.102 Uiso 1 1 calc R . . H21B H 0.6436 0.4374 0.2284 0.102 Uiso 1 1 calc R . . H21C H 0.7756 0.4601 0.1997 0.102 Uiso 1 1 calc R . . C22 C 0.3007(13) 0.4209(5) -0.0059(5) 0.052(4) Uani 1 1 d . . . H22A H 0.3712 0.4541 0.0042 0.078 Uiso 1 1 calc R . . H22B H 0.2303 0.4377 -0.0342 0.078 Uiso 1 1 calc R . . H22C H 0.3456 0.3830 -0.0198 0.078 Uiso 1 1 calc R . . C23 C 0.1272(12) 0.4703(5) 0.0793(6) 0.060(4) Uani 1 1 d . . . H23A H 0.1972 0.5036 0.0899 0.090 Uiso 1 1 calc R . . H23B H 0.0792 0.4588 0.1108 0.090 Uiso 1 1 calc R . . H23C H 0.0591 0.4867 0.0501 0.090 Uiso 1 1 calc R . . C24 C 0.0812(12) 0.3354(6) 0.0366(5) 0.061(4) Uani 1 1 d . . . H24A H 0.0366 0.3236 0.0688 0.091 Uiso 1 1 calc R . . H24B H 0.1256 0.2974 0.0228 0.091 Uiso 1 1 calc R . . H24C H 0.0105 0.3522 0.0084 0.091 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 Tl1 0.0364(3) 0.0391(3) 0.0337(3) -0.0003(2) 0.0053(2) 0.0025(2) Tl2 0.0365(3) 0.0354(3) 0.0350(3) 0.0013(2) 0.0042(3) -0.0011(2) Tl3 0.0380(3) 0.0391(3) 0.0326(3) -0.0020(2) 0.0078(3) -0.0002(2) Sb1 0.0312(5) 0.0347(5) 0.0252(5) -0.0011(4) 0.0005(4) -0.0006(3) Sb2 0.0308(5) 0.0327(4) 0.0283(5) -0.0015(4) 0.0030(4) 0.0016(3) Sb3 0.0353(5) 0.0336(4) 0.0288(6) 0.0003(4) 0.0061(4) -0.0003(4) Si1 0.041(2) 0.045(2) 0.025(2) -0.0016(18) 0.0023(18) -0.0014(16) Si2 0.034(2) 0.047(2) 0.037(2) -0.0021(19) -0.0006(19) -0.0016(16) Si3 0.034(2) 0.039(2) 0.035(3) 0.0010(17) -0.0003(19) -0.0011(15) Si4 0.039(2) 0.036(2) 0.045(3) -0.0044(18) 0.006(2) 0.0054(16) Si5 0.046(2) 0.037(2) 0.046(3) -0.0005(18) 0.010(2) -0.0053(17) Si6 0.050(2) 0.043(2) 0.037(3) -0.0009(19) -0.003(2) 0.0062(17) C1 0.012(7) 0.106(11) 0.059(12) 0.023(9) -0.013(7) 0.000(7) C2 0.080(11) 0.031(7) 0.064(12) -0.010(7) 0.017(9) 0.012(7) C3 0.023(7) 0.049(8) 0.083(12) 0.007(7) -0.013(7) -0.001(6) C4 0.046(8) 0.049(8) 0.041(10) 0.018(7) 0.004(7) 0.010(6) C5 0.009(6) 0.060(8) 0.068(11) 0.004(7) -0.005(6) -0.006(5) C6 0.096(12) 0.069(9) 0.037(10) 0.012(8) 0.035(9) 0.004(8) C7 0.053(9) 0.085(10) 0.032(9) 0.007(7) 0.019(7) 0.017(7) C8 0.048(9) 0.091(10) 0.045(11) 0.007(8) 0.017(8) -0.007(7) C9 0.069(11) 0.088(10) 0.043(11) 0.008(8) -0.002(9) -0.018(8) C10 0.039(8) 0.049(8) 0.060(11) 0.005(7) -0.014(8) 0.009(6) C11 0.034(8) 0.047(8) 0.060(11) -0.011(7) -0.009(7) 0.002(6) C12 0.044(9) 0.072(9) 0.043(10) 0.008(7) 0.008(8) -0.002(7) C13 0.055(9) 0.064(9) 0.034(10) 0.002(7) -0.006(8) -0.011(7) C14 0.056(9) 0.062(9) 0.053(12) 0.014(7) -0.020(8) -0.019(7) C15 0.051(9) 0.079(10) 0.063(12) 0.018(8) 0.002(8) 0.016(7) C16 0.061(9) 0.055(8) 0.046(11) -0.008(7) 0.008(8) 0.013(7) C17 0.033(8) 0.083(10) 0.048(11) 0.021(8) 0.006(7) 0.023(7) C18 0.070(10) 0.054(9) 0.076(13) 0.003(8) 0.014(9) 0.016(7) C19 0.057(10) 0.052(8) 0.081(13) 0.016(8) 0.025(9) 0.003(7) C20 0.070(10) 0.050(8) 0.087(14) -0.009(8) 0.049(10) -0.012(7) C21 0.062(10) 0.062(9) 0.082(14) 0.005(8) 0.016(10) -0.024(7) C22 0.082(11) 0.043(8) 0.029(9) -0.003(6) 0.001(8) 0.005(7) C23 0.054(9) 0.058(9) 0.068(13) 0.004(8) 0.015(9) 0.019(7) C24 0.059(10) 0.091(10) 0.031(10) -0.005(8) -0.003(8) -0.004(8) _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 Tl1 C1 2.205(10) . ? Tl1 C2 2.231(11) . ? Tl1 Sb1 2.9040(9) . ? Tl1 Sb3 2.9100(9) . ? Tl2 C4 2.205(10) . ? Tl2 C3 2.207(10) . ? Tl2 Sb1 2.8952(8) . ? Tl2 Sb2 2.9410(9) . ? Tl3 C6 2.199(13) . ? Tl3 C5 2.227(10) . ? Tl3 Sb3 2.8891(8) . ? Tl3 Sb2 2.8956(8) . ? Sb1 Si2 2.539(3) . ? Sb1 Si1 2.545(3) . ? Sb2 Si4 2.558(3) . ? Sb2 Si3 2.566(3) . ? Sb3 Si6 2.551(4) . ? Sb3 Si5 2.560(3) . ? Si1 C9 1.856(13) . ? Si1 C7 1.870(12) . ? Si1 C8 1.885(12) . ? Si2 C12 1.831(12) . ? Si2 C10 1.865(11) . ? Si2 C11 1.866(10) . ? Si3 C13 1.836(13) . ? Si3 C15 1.841(11) . ? Si3 C14 1.853(11) . ? Si4 C18 1.857(11) . ? Si4 C17 1.862(12) . ? Si4 C16 1.895(13) . ? Si5 C21 1.851(14) . ? Si5 C20 1.872(11) . ? Si5 C19 1.888(13) . ? Si6 C24 1.848(12) . ? Si6 C23 1.859(11) . ? Si6 C22 1.870(12) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 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 C1 Tl1 C2 132.0(5) . . ? C1 Tl1 Sb1 103.7(3) . . ? C2 Tl1 Sb1 105.9(3) . . ? C1 Tl1 Sb3 102.1(4) . . ? C2 Tl1 Sb3 108.8(3) . . ? Sb1 Tl1 Sb3 100.04(2) . . ? C4 Tl2 C3 132.7(4) . . ? C4 Tl2 Sb1 107.7(3) . . ? C3 Tl2 Sb1 101.8(3) . . ? C4 Tl2 Sb2 103.5(3) . . ? C3 Tl2 Sb2 106.8(4) . . ? Sb1 Tl2 Sb2 100.08(2) . . ? C6 Tl3 C5 116.9(5) . . ? C6 Tl3 Sb3 107.4(3) . . ? C5 Tl3 Sb3 107.5(3) . . ? C6 Tl3 Sb2 110.0(3) . . ? C5 Tl3 Sb2 109.4(3) . . ? Sb3 Tl3 Sb2 104.89(3) . . ? Si2 Sb1 Si1 103.52(12) . . ? Si2 Sb1 Tl2 108.07(8) . . ? Si1 Sb1 Tl2 103.09(7) . . ? Si2 Sb1 Tl1 115.29(8) . . ? Si1 Sb1 Tl1 102.88(8) . . ? Tl2 Sb1 Tl1 121.47(3) . . ? Si4 Sb2 Si3 102.33(11) . . ? Si4 Sb2 Tl3 98.71(8) . . ? Si3 Sb2 Tl3 106.56(8) . . ? Si4 Sb2 Tl2 110.42(9) . . ? Si3 Sb2 Tl2 106.66(8) . . ? Tl3 Sb2 Tl2 129.13(3) . . ? Si6 Sb3 Si5 101.00(12) . . ? Si6 Sb3 Tl3 105.87(8) . . ? Si5 Sb3 Tl3 102.47(8) . . ? Si6 Sb3 Tl1 105.88(9) . . ? Si5 Sb3 Tl1 110.17(9) . . ? Tl3 Sb3 Tl1 128.28(3) . . ? C9 Si1 C7 109.2(6) . . ? C9 Si1 C8 108.5(6) . . ? C7 Si1 C8 109.3(5) . . ? C9 Si1 Sb1 114.2(4) . . ? C7 Si1 Sb1 105.7(4) . . ? C8 Si1 Sb1 109.9(4) . . ? C12 Si2 C10 109.9(5) . . ? C12 Si2 C11 110.4(6) . . ? C10 Si2 C11 108.6(6) . . ? C12 Si2 Sb1 106.3(4) . . ? C10 Si2 Sb1 110.4(4) . . ? C11 Si2 Sb1 111.3(4) . . ? C13 Si3 C15 109.3(6) . . ? C13 Si3 C14 107.8(6) . . ? C15 Si3 C14 107.6(6) . . ? C13 Si3 Sb2 112.9(4) . . ? C15 Si3 Sb2 106.8(4) . . ? C14 Si3 Sb2 112.3(4) . . ? C18 Si4 C17 107.9(6) . . ? C18 Si4 C16 110.1(6) . . ? C17 Si4 C16 107.8(6) . . ? C18 Si4 Sb2 112.5(4) . . ? C17 Si4 Sb2 110.2(4) . . ? C16 Si4 Sb2 108.4(4) . . ? C21 Si5 C20 108.7(6) . . ? C21 Si5 C19 109.4(6) . . ? C20 Si5 C19 110.6(6) . . ? C21 Si5 Sb3 108.3(4) . . ? C20 Si5 Sb3 111.1(4) . . ? C19 Si5 Sb3 108.7(4) . . ? C24 Si6 C23 108.6(6) . . ? C24 Si6 C22 110.0(6) . . ? C23 Si6 C22 108.3(5) . . ? C24 Si6 Sb3 108.0(4) . . ? C23 Si6 Sb3 110.5(5) . . ? C22 Si6 Sb3 111.5(4) . . ? Tl1 C1 H1A 109.5 . . ? Tl1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Tl1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Tl1 C2 H2A 109.5 . . ? Tl1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Tl1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Tl2 C3 H3A 109.5 . . ? Tl2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Tl2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Tl2 C4 H4A 109.5 . . ? Tl2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Tl2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Tl3 C5 H5A 109.5 . . ? Tl3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Tl3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Tl3 C6 H6A 109.5 . . ? Tl3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Tl3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si3 C13 H13A 109.5 . . ? Si3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si3 C14 H14A 109.5 . . ? Si3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si4 C16 H16A 109.5 . . ? Si4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si4 C17 H17A 109.5 . . ? Si4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si4 C18 H18A 109.5 . . ? Si4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si5 C19 H19A 109.5 . . ? Si5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si5 C20 H20A 109.5 . . ? Si5 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si5 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si5 C21 H21A 109.5 . . ? Si5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si6 C22 H22A 109.5 . . ? Si6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si6 C23 H23A 109.5 . . ? Si6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si6 C24 H24A 109.5 . . ? Si6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 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 C4 Tl2 Sb1 Si2 26.7(3) . . . . ? C3 Tl2 Sb1 Si2 169.1(4) . . . . ? Sb2 Tl2 Sb1 Si2 -81.13(9) . . . . ? C4 Tl2 Sb1 Si1 -82.5(3) . . . . ? C3 Tl2 Sb1 Si1 60.0(4) . . . . ? Sb2 Tl2 Sb1 Si1 169.70(8) . . . . ? C4 Tl2 Sb1 Tl1 163.2(3) . . . . ? C3 Tl2 Sb1 Tl1 -54.3(4) . . . . ? Sb2 Tl2 Sb1 Tl1 55.46(4) . . . . ? C1 Tl1 Sb1 Si2 173.5(4) . . . . ? C2 Tl1 Sb1 Si2 -44.6(4) . . . . ? Sb3 Tl1 Sb1 Si2 68.37(10) . . . . ? C1 Tl1 Sb1 Si1 -74.5(4) . . . . ? C2 Tl1 Sb1 Si1 67.3(4) . . . . ? Sb3 Tl1 Sb1 Si1 -179.71(8) . . . . ? C1 Tl1 Sb1 Tl2 39.8(4) . . . . ? C2 Tl1 Sb1 Tl2 -178.3(3) . . . . ? Sb3 Tl1 Sb1 Tl2 -65.36(4) . . . . ? C6 Tl3 Sb2 Si4 85.2(4) . . . . ? C5 Tl3 Sb2 Si4 -44.5(4) . . . . ? Sb3 Tl3 Sb2 Si4 -159.61(9) . . . . ? C6 Tl3 Sb2 Si3 -20.5(4) . . . . ? C5 Tl3 Sb2 Si3 -150.2(4) . . . . ? Sb3 Tl3 Sb2 Si3 94.67(8) . . . . ? C6 Tl3 Sb2 Tl2 -149.4(4) . . . . ? C5 Tl3 Sb2 Tl2 80.9(3) . . . . ? Sb3 Tl3 Sb2 Tl2 -34.19(5) . . . . ? C4 Tl2 Sb2 Si4 11.5(3) . . . . ? C3 Tl2 Sb2 Si4 -131.7(3) . . . . ? Sb1 Tl2 Sb2 Si4 122.54(9) . . . . ? C4 Tl2 Sb2 Si3 121.9(3) . . . . ? C3 Tl2 Sb2 Si3 -21.3(3) . . . . ? Sb1 Tl2 Sb2 Si3 -127.02(8) . . . . ? C4 Tl2 Sb2 Tl3 -109.3(3) . . . . ? C3 Tl2 Sb2 Tl3 107.5(3) . . . . ? Sb1 Tl2 Sb2 Tl3 1.80(4) . . . . ? C6 Tl3 Sb3 Si6 11.9(4) . . . . ? C5 Tl3 Sb3 Si6 138.5(3) . . . . ? Sb2 Tl3 Sb3 Si6 -105.09(9) . . . . ? C6 Tl3 Sb3 Si5 -93.5(4) . . . . ? C5 Tl3 Sb3 Si5 33.1(3) . . . . ? Sb2 Tl3 Sb3 Si5 149.48(10) . . . . ? C6 Tl3 Sb3 Tl1 137.8(4) . . . . ? C5 Tl3 Sb3 Tl1 -95.6(3) . . . . ? Sb2 Tl3 Sb3 Tl1 20.85(5) . . . . ? C1 Tl1 Sb3 Si6 38.9(3) . . . . ? C2 Tl1 Sb3 Si6 -103.8(3) . . . . ? Sb1 Tl1 Sb3 Si6 145.38(8) . . . . ? C1 Tl1 Sb3 Si5 147.3(3) . . . . ? C2 Tl1 Sb3 Si5 4.6(3) . . . . ? Sb1 Tl1 Sb3 Si5 -106.21(9) . . . . ? C1 Tl1 Sb3 Tl3 -87.0(3) . . . . ? C2 Tl1 Sb3 Tl3 130.2(3) . . . . ? Sb1 Tl1 Sb3 Tl3 19.45(4) . . . . ? Si2 Sb1 Si1 C9 43.6(5) . . . . ? Tl2 Sb1 Si1 C9 156.1(5) . . . . ? Tl1 Sb1 Si1 C9 -76.8(5) . . . . ? Si2 Sb1 Si1 C7 163.5(4) . . . . ? Tl2 Sb1 Si1 C7 -83.9(4) . . . . ? Tl1 Sb1 Si1 C7 43.2(4) . . . . ? Si2 Sb1 Si1 C8 -78.7(4) . . . . ? Tl2 Sb1 Si1 C8 33.9(4) . . . . ? Tl1 Sb1 Si1 C8 161.0(4) . . . . ? Si1 Sb1 Si2 C12 164.1(4) . . . . ? Tl2 Sb1 Si2 C12 55.2(4) . . . . ? Tl1 Sb1 Si2 C12 -84.3(4) . . . . ? Si1 Sb1 Si2 C10 45.0(4) . . . . ? Tl2 Sb1 Si2 C10 -63.9(4) . . . . ? Tl1 Sb1 Si2 C10 156.5(4) . . . . ? Si1 Sb1 Si2 C11 -75.7(5) . . . . ? Tl2 Sb1 Si2 C11 175.5(5) . . . . ? Tl1 Sb1 Si2 C11 35.9(5) . . . . ? Si4 Sb2 Si3 C13 -63.4(4) . . . . ? Tl3 Sb2 Si3 C13 39.7(4) . . . . ? Tl2 Sb2 Si3 C13 -179.4(4) . . . . ? Si4 Sb2 Si3 C15 176.5(5) . . . . ? Tl3 Sb2 Si3 C15 -80.4(5) . . . . ? Tl2 Sb2 Si3 C15 60.5(5) . . . . ? Si4 Sb2 Si3 C14 58.7(5) . . . . ? Tl3 Sb2 Si3 C14 161.8(5) . . . . ? Tl2 Sb2 Si3 C14 -57.3(5) . . . . ? Si3 Sb2 Si4 C18 -48.7(5) . . . . ? Tl3 Sb2 Si4 C18 -157.9(5) . . . . ? Tl2 Sb2 Si4 C18 64.5(5) . . . . ? Si3 Sb2 Si4 C17 -169.1(4) . . . . ? Tl3 Sb2 Si4 C17 81.7(4) . . . . ? Tl2 Sb2 Si4 C17 -55.9(4) . . . . ? Si3 Sb2 Si4 C16 73.2(4) . . . . ? Tl3 Sb2 Si4 C16 -36.0(4) . . . . ? Tl2 Sb2 Si4 C16 -173.6(4) . . . . ? Si6 Sb3 Si5 C21 161.9(5) . . . . ? Tl3 Sb3 Si5 C21 -89.0(5) . . . . ? Tl1 Sb3 Si5 C21 50.3(5) . . . . ? Si6 Sb3 Si5 C20 42.5(5) . . . . ? Tl3 Sb3 Si5 C20 151.7(5) . . . . ? Tl1 Sb3 Si5 C20 -69.1(5) . . . . ? Si6 Sb3 Si5 C19 -79.4(4) . . . . ? Tl3 Sb3 Si5 C19 29.8(4) . . . . ? Tl1 Sb3 Si5 C19 169.0(4) . . . . ? Si5 Sb3 Si6 C24 168.0(4) . . . . ? Tl3 Sb3 Si6 C24 61.6(5) . . . . ? Tl1 Sb3 Si6 C24 -77.1(4) . . . . ? Si5 Sb3 Si6 C23 -73.3(5) . . . . ? Tl3 Sb3 Si6 C23 -179.8(4) . . . . ? Tl1 Sb3 Si6 C23 41.6(4) . . . . ? Si5 Sb3 Si6 C22 47.1(4) . . . . ? Tl3 Sb3 Si6 C22 -59.3(4) . . . . ? Tl1 Sb3 Si6 C22 162.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.331 _refine_diff_density_min -1.395 _refine_diff_density_rms 0.217