Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_cmpd 1 _database_code_CSD 167523 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cole, Marcus L.' 'Davies, Aaron J.' 'Jones, Cameron' _publ_contact_author_name 'Dr Cameron Jones' _publ_contact_author_address ; Department of Chemistry University of Wales P.O. Box 912 Park Place Cardiff CF10 3TB UNITED KINGDOM ; _publ_contact_author_email 'JONESCA6@CARDIFF.AC.UK' _publ_section_title ; Synthesis and CHaracterisation of the First Carbene-Thallium Complexes: Molecular Structure of [TlCl3{CN(Mes)C2H2N(Mes)}], Mes = C6H2Me3-2,4,6 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H24 Cl3 N2 Tl' _chemical_formula_weight 615.14 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' 'Cl' 'Cl' 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 16.475(3) _cell_length_b 16.546(3) _cell_length_c 17.215(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4692.7(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 7.233 _exptl_absorpt_correction_type difabs _exptl_absorpt_correction_T_min 0.22 _exptl_absorpt_correction_T_max 0.14 _exptl_absorpt_process_details ? _exptl_special_details ; The crystal contained two molecules in the asymmetric unit both with very similar geometries. The structure was solved in the non-centrosymmetric space group Pca2(1) and it was found to be a racemic twin and was refined successfully using the TWIN command of ShelxL. The possibility of the being centrosymmetric was explored but no suitable refinement could be achieved using the centrosymmetric setting. ; _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 CAD4-turbo _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9064 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.21 _reflns_number_total 4380 _reflns_number_gt 3819 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000019(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.605(14) _refine_ls_number_reflns 4380 _refine_ls_number_parameters 501 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0489 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.004 _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 -1.409469(19) -1.487875(13) -1.835907(13) 0.02346(8) Uani 1 1 d . . . Tl2 Tl -1.658838(18) -1.020928(14) -1.664162(13) 0.02177(8) Uani 1 1 d . . . Cl1 Cl -1.43118(18) -1.49478(15) -1.69688(16) 0.0484(6) Uani 1 1 d . . . Cl2 Cl -1.32159(15) -1.37401(12) -1.86148(17) 0.0397(6) Uani 1 1 d . . . Cl3 Cl -1.33038(14) -1.60684(12) -1.86568(17) 0.0367(5) Uani 1 1 d . . . Cl4 Cl -1.68023(15) -1.03914(13) -1.80164(15) 0.0394(5) Uani 1 1 d . . . Cl5 Cl -1.56290(14) -1.12489(12) -1.62618(17) 0.0359(5) Uani 1 1 d . . . Cl6 Cl -1.58589(13) -0.89489(11) -1.64808(17) 0.0375(5) Uani 1 1 d . . . N1 N -1.5759(4) -1.5437(3) -1.9117(4) 0.0257(16) Uani 1 1 d . . . N2 N -1.5629(4) -1.4136(4) -1.9194(5) 0.0271(17) Uani 1 1 d . . . N3 N -1.8232(4) -0.9615(4) -1.5826(4) 0.0255(16) Uani 1 1 d . . . N4 N -1.8154(4) -1.0935(4) -1.5833(4) 0.0225(16) Uani 1 1 d . . . C1 C -1.5248(5) -1.4819(4) -1.8976(5) 0.0205(16) Uani 1 1 d . . . C2 C -1.6454(6) -1.5141(5) -1.9430(7) 0.035(3) Uani 1 1 d . . . H2 H -1.6896 -1.5447 -1.9593 0.042 Uiso 1 1 calc R . . C3 C -1.6402(5) -1.4348(5) -1.9465(6) 0.037(2) Uani 1 1 d . . . H3 H -1.6802 -1.3995 -1.9638 0.044 Uiso 1 1 calc R . . C4 C -1.5555(5) -1.6291(4) -1.9000(5) 0.0227(18) Uani 1 1 d . . . C5 C -1.5762(4) -1.6639(4) -1.8299(6) 0.0268(17) Uani 1 1 d . . . C6 C -1.5583(6) -1.7477(5) -1.8211(6) 0.034(2) Uani 1 1 d . . . H6 H -1.5703 -1.7737 -1.7746 0.040 Uiso 1 1 calc R . . C7 C -1.5235(5) -1.7901(4) -1.8807(6) 0.029(2) Uani 1 1 d . . . C8 C -1.5074(5) -1.7531(5) -1.9493(6) 0.033(2) Uani 1 1 d . . . H8 H -1.4859 -1.7835 -1.9898 0.039 Uiso 1 1 calc R . . C9 C -1.5219(5) -1.6716(5) -1.9613(5) 0.032(2) Uani 1 1 d . . . C10 C -1.6144(6) -1.6170(6) -1.7634(5) 0.042(2) Uani 1 1 d . . . H10A H -1.5743 -1.5829 -1.7397 0.062 Uiso 1 1 calc R . . H10B H -1.6352 -1.6542 -1.7254 0.062 Uiso 1 1 calc R . . H10C H -1.6580 -1.5843 -1.7829 0.062 Uiso 1 1 calc R . . C11 C -1.5063(6) -1.8787(4) -1.8699(6) 0.042(2) Uani 1 1 d . . . H11A H -1.5542 -1.9093 -1.8819 0.064 Uiso 1 1 calc R . . H11B H -1.4907 -1.8886 -1.8170 0.064 Uiso 1 1 calc R . . H11C H -1.4630 -1.8947 -1.9039 0.064 Uiso 1 1 calc R . . C12 C -1.5021(6) -1.6299(5) -2.0376(5) 0.039(2) Uani 1 1 d . . . H12A H -1.4660 -1.6633 -2.0674 0.058 Uiso 1 1 calc R . . H12B H -1.4765 -1.5789 -2.0273 0.058 Uiso 1 1 calc R . . H12C H -1.5512 -1.6211 -2.0664 0.058 Uiso 1 1 calc R . . C13 C -1.5341(5) -1.3313(4) -1.9131(4) 0.0181(16) Uani 1 1 d . . . C14 C -1.5516(5) -1.2875(4) -1.8461(6) 0.029(2) Uani 1 1 d . . . C15 C -1.5263(5) -1.2065(4) -1.8461(6) 0.031(2) Uani 1 1 d . . . H15 H -1.5383 -1.1746 -1.8032 0.037 Uiso 1 1 calc R . . C16 C -1.4842(5) -1.1725(4) -1.9072(5) 0.0286(19) Uani 1 1 d . . . C17 C -1.4681(5) -1.2199(4) -1.9711(5) 0.031(2) Uani 1 1 d . . . H17 H -1.4397 -1.1973 -2.0124 0.037 Uiso 1 1 calc R . . C18 C -1.4923(5) -1.2996(4) -1.9764(5) 0.028(2) Uani 1 1 d . . . C19 C -1.5965(7) -1.3226(5) -1.7794(6) 0.046(2) Uani 1 1 d . . . H19A H -1.6028 -1.2823 -1.7397 0.069 Uiso 1 1 calc R . . H19B H -1.5668 -1.3677 -1.7590 0.069 Uiso 1 1 calc R . . H19C H -1.6490 -1.3403 -1.7964 0.069 Uiso 1 1 calc R . . C20 C -1.4624(6) -1.0848(4) -1.9057(6) 0.040(2) Uani 1 1 d . . . H20A H -1.4207 -1.0759 -1.8677 0.059 Uiso 1 1 calc R . . H20B H -1.5095 -1.0535 -1.8924 0.059 Uiso 1 1 calc R . . H20C H -1.4430 -1.0687 -1.9559 0.059 Uiso 1 1 calc R . . C21 C -1.4746(6) -1.3505(5) -2.0488(6) 0.043(2) Uani 1 1 d . . . H21A H -1.4570 -1.4034 -2.0332 0.065 Uiso 1 1 calc R . . H21B H -1.4327 -1.3251 -2.0788 0.065 Uiso 1 1 calc R . . H21C H -1.5229 -1.3550 -2.0796 0.065 Uiso 1 1 calc R . . C22 C -1.7744(6) -1.0252(4) -1.6012(5) 0.0223(19) Uani 1 1 d . . . C23 C -1.8895(5) -1.0733(5) -1.5513(6) 0.041(2) Uani 1 1 d . . . H23 H -1.9284 -1.1092 -1.5328 0.049 Uiso 1 1 calc R . . C24 C -1.8954(7) -0.9911(5) -1.5518(8) 0.042(3) Uani 1 1 d . . . H24 H -1.9394 -0.9606 -1.5348 0.051 Uiso 1 1 calc R . . C25 C -1.8045(5) -0.8774(4) -1.5882(5) 0.0209(18) Uani 1 1 d . . . C26 C -1.7742(5) -0.8383(4) -1.5237(5) 0.0304(19) Uani 1 1 d . . . C27 C -1.7592(5) -0.7554(4) -1.5312(6) 0.037(2) Uani 1 1 d . . . H27 H -1.7395 -0.7268 -1.4886 0.044 Uiso 1 1 calc R . . C28 C -1.7731(5) -0.7143(4) -1.6010(5) 0.032(2) Uani 1 1 d . . . C29 C -1.8031(5) -0.7580(4) -1.6624(7) 0.037(2) Uani 1 1 d . . . H29 H -1.8136 -0.7309 -1.7086 0.044 Uiso 1 1 calc R . . C30 C -1.8185(4) -0.8395(4) -1.6596(6) 0.0302(18) Uani 1 1 d . . . C31 C -1.7590(7) -0.8800(6) -1.4478(6) 0.049(3) Uani 1 1 d . . . H31A H -1.7313 -0.8438 -1.4132 0.074 Uiso 1 1 calc R . . H31B H -1.7261 -0.9271 -1.4564 0.074 Uiso 1 1 calc R . . H31C H -1.8099 -0.8958 -1.4252 0.074 Uiso 1 1 calc R . . C32 C -1.7579(7) -0.6236(4) -1.6046(7) 0.056(3) Uani 1 1 d . . . H32A H -1.7768 -0.6029 -1.6534 0.084 Uiso 1 1 calc R . . H32B H -1.7008 -0.6133 -1.5995 0.084 Uiso 1 1 calc R . . H32C H -1.7865 -0.5975 -1.5630 0.084 Uiso 1 1 calc R . . C33 C -1.8515(6) -0.8812(6) -1.7279(6) 0.043(2) Uani 1 1 d . . . H33A H -1.8988 -0.9113 -1.7131 0.064 Uiso 1 1 calc R . . H33B H -1.8113 -0.9175 -1.7484 0.064 Uiso 1 1 calc R . . H33C H -1.8658 -0.8422 -1.7668 0.064 Uiso 1 1 calc R . . C34 C -1.7876(5) -1.1747(4) -1.5928(5) 0.0281(19) Uani 1 1 d . . . C35 C -1.8114(5) -1.2153(4) -1.6610(7) 0.0273(17) Uani 1 1 d . . . C36 C -1.7857(5) -1.2970(4) -1.6656(7) 0.0364(19) Uani 1 1 d . . . H36 H -1.8019 -1.3273 -1.7083 0.044 Uiso 1 1 calc R . . C37 C -1.7388(5) -1.3330(4) -1.6112(5) 0.0306(19) Uani 1 1 d . . . C38 C -1.7161(5) -1.2894(4) -1.5453(5) 0.0286(19) Uani 1 1 d . . . H38 H -1.6838 -1.3137 -1.5077 0.034 Uiso 1 1 calc R . . C39 C -1.7418(5) -1.2083(4) -1.5353(5) 0.0260(19) Uani 1 1 d . . . C40 C -1.8622(5) -1.1782(5) -1.7214(5) 0.042(2) Uani 1 1 d . . . H40A H -1.8814 -1.2193 -1.7563 0.062 Uiso 1 1 calc R . . H40B H -1.8307 -1.1394 -1.7499 0.062 Uiso 1 1 calc R . . H40C H -1.9076 -1.1517 -1.6977 0.062 Uiso 1 1 calc R . . C41 C -1.7118(6) -1.4199(4) -1.6195(6) 0.040(2) Uani 1 1 d . . . H41A H -1.7204 -1.4479 -1.5713 0.061 Uiso 1 1 calc R . . H41B H -1.6551 -1.4214 -1.6325 0.061 Uiso 1 1 calc R . . H41C H -1.7426 -1.4456 -1.6599 0.061 Uiso 1 1 calc R . . C42 C -1.7181(6) -1.1636(5) -1.4630(5) 0.036(2) Uani 1 1 d . . . H42A H -1.7653 -1.1389 -1.4405 0.054 Uiso 1 1 calc R . . H42B H -1.6791 -1.1226 -1.4757 0.054 Uiso 1 1 calc R . . H42C H -1.6947 -1.2007 -1.4264 0.054 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 0.02395(16) 0.02410(12) 0.02234(15) -0.00210(15) -0.00260(16) 0.00191(11) Tl2 0.02304(15) 0.02125(12) 0.02100(15) 0.00031(12) 0.00229(15) -0.00141(12) Cl1 0.0511(15) 0.0711(15) 0.0230(11) -0.0091(10) 0.0019(11) -0.0008(12) Cl2 0.0355(12) 0.0300(9) 0.0536(15) 0.0036(9) -0.0039(11) -0.0076(8) Cl3 0.0361(12) 0.0346(10) 0.0395(12) -0.0049(9) 0.0009(10) 0.0131(9) Cl4 0.0502(13) 0.0446(11) 0.0233(10) -0.0062(9) -0.0013(10) 0.0009(11) Cl5 0.0317(12) 0.0338(10) 0.0421(12) 0.0092(9) -0.0014(10) 0.0055(9) Cl6 0.0426(12) 0.0303(9) 0.0398(13) -0.0039(8) 0.0015(11) -0.0142(9) N1 0.027(4) 0.014(3) 0.035(4) -0.005(3) -0.007(3) 0.005(3) N2 0.032(4) 0.016(3) 0.034(4) 0.000(3) 0.001(3) 0.004(3) N3 0.022(4) 0.024(3) 0.031(4) 0.003(3) -0.002(3) 0.001(3) N4 0.024(4) 0.019(3) 0.024(4) -0.003(3) 0.006(3) 0.003(3) C1 0.020(4) 0.021(3) 0.020(4) 0.003(3) -0.001(4) -0.006(3) C2 0.027(6) 0.031(4) 0.046(7) -0.002(4) 0.001(6) -0.001(4) C3 0.015(4) 0.040(5) 0.054(6) 0.004(4) -0.006(4) -0.001(4) C4 0.031(5) 0.015(3) 0.022(4) -0.001(3) -0.004(4) -0.001(3) C5 0.031(4) 0.020(3) 0.029(4) 0.001(4) 0.000(4) -0.004(3) C6 0.043(5) 0.033(4) 0.026(5) 0.010(4) 0.001(4) -0.009(4) C7 0.027(4) 0.018(4) 0.043(5) 0.002(4) 0.000(4) -0.004(3) C8 0.031(5) 0.028(4) 0.039(5) -0.008(4) -0.008(4) 0.000(4) C9 0.024(4) 0.032(4) 0.039(5) 0.008(4) -0.010(4) -0.001(3) C10 0.046(6) 0.058(6) 0.021(4) 0.000(4) 0.006(4) -0.005(5) C11 0.055(6) 0.026(4) 0.046(5) -0.004(4) -0.002(5) -0.012(4) C12 0.040(5) 0.054(5) 0.022(4) 0.004(4) 0.010(4) 0.012(4) C13 0.020(4) 0.012(3) 0.023(4) -0.003(3) 0.001(3) 0.006(3) C14 0.030(4) 0.021(3) 0.036(5) 0.004(4) 0.003(4) 0.005(3) C15 0.038(4) 0.018(3) 0.036(5) -0.014(4) -0.011(5) 0.004(3) C16 0.028(4) 0.018(4) 0.040(5) 0.010(4) -0.013(4) 0.004(3) C17 0.039(5) 0.025(4) 0.028(5) 0.015(3) -0.005(4) 0.002(4) C18 0.032(5) 0.029(4) 0.024(5) 0.001(3) -0.007(4) 0.015(4) C19 0.067(6) 0.035(5) 0.037(5) -0.008(4) 0.023(5) 0.006(5) C20 0.049(5) 0.026(4) 0.044(5) 0.005(4) -0.021(5) 0.007(4) C21 0.053(6) 0.047(5) 0.030(5) -0.009(4) 0.017(5) -0.006(5) C22 0.037(5) 0.011(3) 0.019(4) -0.002(3) -0.007(4) -0.006(3) C23 0.034(5) 0.029(4) 0.061(6) 0.007(4) 0.021(5) -0.003(4) C24 0.029(7) 0.037(5) 0.062(8) 0.005(5) 0.025(6) 0.009(4) C25 0.018(4) 0.023(4) 0.021(4) 0.002(3) 0.004(3) 0.009(3) C26 0.030(5) 0.033(4) 0.028(4) 0.001(4) 0.006(4) 0.002(3) C27 0.043(5) 0.030(4) 0.037(5) -0.005(4) 0.000(4) -0.003(4) C28 0.039(5) 0.017(3) 0.040(5) 0.000(3) 0.013(4) 0.005(3) C29 0.052(5) 0.029(4) 0.030(4) 0.018(5) 0.010(5) 0.016(4) C30 0.032(4) 0.026(3) 0.032(4) 0.001(4) 0.015(4) 0.011(3) C31 0.057(7) 0.053(5) 0.038(5) 0.006(5) -0.004(5) 0.006(5) C32 0.065(7) 0.020(4) 0.084(9) 0.000(4) 0.038(7) 0.001(5) C33 0.042(6) 0.050(5) 0.035(5) 0.002(4) -0.014(5) 0.015(4) C34 0.030(5) 0.015(3) 0.040(5) 0.004(3) 0.004(4) 0.000(3) C35 0.029(4) 0.021(3) 0.032(4) -0.005(4) 0.008(5) -0.006(3) C36 0.050(5) 0.026(3) 0.033(4) -0.001(4) -0.003(5) -0.016(4) C37 0.033(5) 0.022(4) 0.038(5) 0.001(3) 0.004(4) -0.003(4) C38 0.034(5) 0.018(3) 0.034(5) 0.009(3) 0.002(4) -0.006(3) C39 0.034(5) 0.021(3) 0.022(4) 0.001(3) 0.006(4) -0.008(4) C40 0.047(6) 0.044(5) 0.034(5) -0.002(4) -0.008(5) -0.003(4) C41 0.057(6) 0.017(3) 0.047(5) -0.005(4) 0.008(5) 0.002(4) C42 0.049(6) 0.031(4) 0.028(5) 0.000(4) -0.005(4) 0.000(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 Tl1 C1 2.179(9) . ? Tl1 Cl3 2.416(2) . ? Tl1 Cl2 2.417(2) . ? Tl1 Cl1 2.423(3) . ? Tl2 C22 2.192(10) . ? Tl2 Cl4 2.412(3) . ? Tl2 Cl6 2.4229(19) . ? Tl2 Cl5 2.426(2) . ? N1 C1 1.347(11) . ? N1 C2 1.359(13) . ? N1 C4 1.466(9) . ? N2 C1 1.345(10) . ? N2 C3 1.400(10) . ? N2 C13 1.447(9) . ? N3 C22 1.365(10) . ? N3 C24 1.392(13) . ? N3 C25 1.428(10) . ? N4 C22 1.351(9) . ? N4 C23 1.381(11) . ? N4 C34 1.430(10) . ? C2 C3 1.315(13) . ? C4 C5 1.380(12) . ? C4 C9 1.383(12) . ? C5 C6 1.427(10) . ? C5 C10 1.520(12) . ? C6 C7 1.369(12) . ? C7 C8 1.357(13) . ? C7 C11 1.504(10) . ? C8 C9 1.385(11) . ? C9 C12 1.519(12) . ? C13 C14 1.391(12) . ? C13 C18 1.392(12) . ? C14 C15 1.402(10) . ? C14 C19 1.484(12) . ? C15 C16 1.381(12) . ? C16 C17 1.377(12) . ? C16 C20 1.495(10) . ? C17 C18 1.380(11) . ? C18 C21 1.532(11) . ? C23 C24 1.363(12) . ? C25 C26 1.378(12) . ? C25 C30 1.399(12) . ? C26 C27 1.401(10) . ? C26 C31 1.499(12) . ? C27 C28 1.400(12) . ? C28 C29 1.373(14) . ? C28 C32 1.522(9) . ? C29 C30 1.373(10) . ? C30 C33 1.467(13) . ? C34 C39 1.362(12) . ? C34 C35 1.409(13) . ? C35 C36 1.418(10) . ? C35 C40 1.469(13) . ? C36 C37 1.352(12) . ? C37 C38 1.396(12) . ? C37 C41 1.512(10) . ? C38 C39 1.418(11) . ? C39 C42 1.500(11) . ? 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 Cl3 113.8(2) . . ? C1 Tl1 Cl2 113.4(2) . . ? Cl3 Tl1 Cl2 105.87(9) . . ? C1 Tl1 Cl1 110.8(2) . . ? Cl3 Tl1 Cl1 104.53(9) . . ? Cl2 Tl1 Cl1 107.77(10) . . ? C22 Tl2 Cl4 110.7(2) . . ? C22 Tl2 Cl6 113.73(17) . . ? Cl4 Tl2 Cl6 106.99(9) . . ? C22 Tl2 Cl5 114.2(2) . . ? Cl4 Tl2 Cl5 105.73(9) . . ? Cl6 Tl2 Cl5 104.85(8) . . ? C1 N1 C2 108.9(6) . . ? C1 N1 C4 124.4(7) . . ? C2 N1 C4 126.6(7) . . ? C1 N2 C3 107.9(7) . . ? C1 N2 C13 128.0(7) . . ? C3 N2 C13 124.0(7) . . ? C22 N3 C24 108.7(7) . . ? C22 N3 C25 127.6(8) . . ? C24 N3 C25 123.6(7) . . ? C22 N4 C23 109.3(7) . . ? C22 N4 C34 126.8(7) . . ? C23 N4 C34 123.8(7) . . ? N2 C1 N1 107.2(8) . . ? N2 C1 Tl1 125.5(6) . . ? N1 C1 Tl1 126.7(5) . . ? C3 C2 N1 108.8(8) . . ? C2 C3 N2 107.1(8) . . ? C5 C4 C9 123.7(7) . . ? C5 C4 N1 117.7(7) . . ? C9 C4 N1 118.5(7) . . ? C4 C5 C6 116.6(8) . . ? C4 C5 C10 123.3(6) . . ? C6 C5 C10 120.1(8) . . ? C7 C6 C5 120.4(8) . . ? C8 C7 C6 120.1(7) . . ? C8 C7 C11 120.8(8) . . ? C6 C7 C11 119.1(8) . . ? C7 C8 C9 122.5(9) . . ? C4 C9 C8 116.7(8) . . ? C4 C9 C12 121.0(7) . . ? C8 C9 C12 122.3(8) . . ? C14 C13 C18 123.6(7) . . ? C14 C13 N2 119.0(7) . . ? C18 C13 N2 117.3(7) . . ? C13 C14 C15 115.9(8) . . ? C13 C14 C19 122.7(6) . . ? C15 C14 C19 121.4(9) . . ? C16 C15 C14 122.6(9) . . ? C17 C16 C15 118.2(7) . . ? C17 C16 C20 121.4(8) . . ? C15 C16 C20 120.2(8) . . ? C16 C17 C18 122.8(8) . . ? C17 C18 C13 116.8(8) . . ? C17 C18 C21 121.6(8) . . ? C13 C18 C21 121.5(7) . . ? N4 C22 N3 107.4(8) . . ? N4 C22 Tl2 125.0(5) . . ? N3 C22 Tl2 127.1(5) . . ? C24 C23 N4 107.6(8) . . ? C23 C24 N3 107.0(8) . . ? C26 C25 C30 123.9(7) . . ? C26 C25 N3 118.7(7) . . ? C30 C25 N3 117.4(7) . . ? C25 C26 C27 116.7(8) . . ? C25 C26 C31 123.2(7) . . ? C27 C26 C31 120.1(8) . . ? C28 C27 C26 121.8(8) . . ? C29 C28 C27 117.6(7) . . ? C29 C28 C32 123.3(9) . . ? C27 C28 C32 119.1(9) . . ? C30 C29 C28 124.0(10) . . ? C29 C30 C25 116.1(9) . . ? C29 C30 C33 120.2(9) . . ? C25 C30 C33 123.6(7) . . ? C39 C34 C35 124.4(7) . . ? C39 C34 N4 118.6(8) . . ? C35 C34 N4 117.0(7) . . ? C34 C35 C36 114.6(9) . . ? C34 C35 C40 123.4(7) . . ? C36 C35 C40 121.9(9) . . ? C37 C36 C35 123.5(9) . . ? C36 C37 C38 119.3(7) . . ? C36 C37 C41 121.5(8) . . ? C38 C37 C41 119.2(8) . . ? C37 C38 C39 120.4(7) . . ? C34 C39 C38 117.7(7) . . ? C34 C39 C42 123.1(7) . . ? C38 C39 C42 119.3(7) . . ? 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 C3 N2 C1 N1 0.8(10) . . . . ? C13 N2 C1 N1 177.6(7) . . . . ? C3 N2 C1 Tl1 -171.1(6) . . . . ? C13 N2 C1 Tl1 5.7(13) . . . . ? C2 N1 C1 N2 0.8(10) . . . . ? C4 N1 C1 N2 176.4(8) . . . . ? C2 N1 C1 Tl1 172.5(7) . . . . ? C4 N1 C1 Tl1 -11.8(12) . . . . ? Cl3 Tl1 C1 N2 -149.6(7) . . . . ? Cl2 Tl1 C1 N2 -28.5(8) . . . . ? Cl1 Tl1 C1 N2 92.9(7) . . . . ? Cl3 Tl1 C1 N1 40.1(8) . . . . ? Cl2 Tl1 C1 N1 161.2(6) . . . . ? Cl1 Tl1 C1 N1 -77.4(7) . . . . ? C1 N1 C2 C3 -2.1(11) . . . . ? C4 N1 C2 C3 -177.6(9) . . . . ? N1 C2 C3 N2 2.5(11) . . . . ? C1 N2 C3 C2 -2.1(11) . . . . ? C13 N2 C3 C2 -179.0(9) . . . . ? C1 N1 C4 C5 94.1(10) . . . . ? C2 N1 C4 C5 -91.0(11) . . . . ? C1 N1 C4 C9 -90.3(10) . . . . ? C2 N1 C4 C9 84.6(12) . . . . ? C9 C4 C5 C6 2.4(12) . . . . ? N1 C4 C5 C6 177.8(7) . . . . ? C9 C4 C5 C10 -178.9(8) . . . . ? N1 C4 C5 C10 -3.5(12) . . . . ? C4 C5 C6 C7 -1.0(13) . . . . ? C10 C5 C6 C7 -179.7(8) . . . . ? C5 C6 C7 C8 -1.5(14) . . . . ? C5 C6 C7 C11 -179.3(8) . . . . ? C6 C7 C8 C9 2.7(14) . . . . ? C11 C7 C8 C9 -179.6(8) . . . . ? C5 C4 C9 C8 -1.3(13) . . . . ? N1 C4 C9 C8 -176.7(7) . . . . ? C5 C4 C9 C12 178.7(8) . . . . ? N1 C4 C9 C12 3.4(12) . . . . ? C7 C8 C9 C4 -1.3(13) . . . . ? C7 C8 C9 C12 178.6(8) . . . . ? C1 N2 C13 C14 -90.5(11) . . . . ? C3 N2 C13 C14 85.9(11) . . . . ? C1 N2 C13 C18 91.7(11) . . . . ? C3 N2 C13 C18 -92.0(10) . . . . ? C18 C13 C14 C15 1.6(12) . . . . ? N2 C13 C14 C15 -176.1(7) . . . . ? C18 C13 C14 C19 179.8(8) . . . . ? N2 C13 C14 C19 2.1(12) . . . . ? C13 C14 C15 C16 -2.1(13) . . . . ? C19 C14 C15 C16 179.8(8) . . . . ? C14 C15 C16 C17 1.3(13) . . . . ? C14 C15 C16 C20 176.9(8) . . . . ? C15 C16 C17 C18 0.1(13) . . . . ? C20 C16 C17 C18 -175.5(8) . . . . ? C16 C17 C18 C13 -0.5(12) . . . . ? C16 C17 C18 C21 179.1(9) . . . . ? C14 C13 C18 C17 -0.4(12) . . . . ? N2 C13 C18 C17 177.3(7) . . . . ? C14 C13 C18 C21 180.0(8) . . . . ? N2 C13 C18 C21 -2.3(12) . . . . ? C23 N4 C22 N3 -1.6(9) . . . . ? C34 N4 C22 N3 -179.7(8) . . . . ? C23 N4 C22 Tl2 -173.5(6) . . . . ? C34 N4 C22 Tl2 8.4(12) . . . . ? C24 N3 C22 N4 0.6(10) . . . . ? C25 N3 C22 N4 177.2(8) . . . . ? C24 N3 C22 Tl2 172.3(8) . . . . ? C25 N3 C22 Tl2 -11.1(12) . . . . ? Cl4 Tl2 C22 N4 78.2(7) . . . . ? Cl6 Tl2 C22 N4 -161.3(6) . . . . ? Cl5 Tl2 C22 N4 -41.0(8) . . . . ? Cl4 Tl2 C22 N3 -92.1(7) . . . . ? Cl6 Tl2 C22 N3 28.4(7) . . . . ? Cl5 Tl2 C22 N3 148.7(6) . . . . ? C22 N4 C23 C24 1.9(11) . . . . ? C34 N4 C23 C24 -179.8(10) . . . . ? N4 C23 C24 N3 -1.5(12) . . . . ? C22 N3 C24 C23 0.6(12) . . . . ? C25 N3 C24 C23 -176.2(9) . . . . ? C22 N3 C25 C26 -93.8(10) . . . . ? C24 N3 C25 C26 82.3(12) . . . . ? C22 N3 C25 C30 86.4(10) . . . . ? C24 N3 C25 C30 -97.5(11) . . . . ? C30 C25 C26 C27 1.8(13) . . . . ? N3 C25 C26 C27 -178.0(7) . . . . ? C30 C25 C26 C31 -179.5(8) . . . . ? N3 C25 C26 C31 0.6(12) . . . . ? C25 C26 C27 C28 -0.9(13) . . . . ? C31 C26 C27 C28 -179.6(8) . . . . ? C26 C27 C28 C29 0.7(13) . . . . ? C26 C27 C28 C32 178.3(9) . . . . ? C27 C28 C29 C30 -1.4(13) . . . . ? C32 C28 C29 C30 -178.8(9) . . . . ? C28 C29 C30 C25 2.2(13) . . . . ? C28 C29 C30 C33 179.3(8) . . . . ? C26 C25 C30 C29 -2.4(12) . . . . ? N3 C25 C30 C29 177.4(7) . . . . ? C26 C25 C30 C33 -179.4(8) . . . . ? N3 C25 C30 C33 0.5(12) . . . . ? C22 N4 C34 C39 85.4(11) . . . . ? C23 N4 C34 C39 -92.5(11) . . . . ? C22 N4 C34 C35 -96.1(10) . . . . ? C23 N4 C34 C35 86.0(11) . . . . ? C39 C34 C35 C36 1.5(12) . . . . ? N4 C34 C35 C36 -176.9(7) . . . . ? C39 C34 C35 C40 178.7(8) . . . . ? N4 C34 C35 C40 0.3(13) . . . . ? C34 C35 C36 C37 -2.9(13) . . . . ? C40 C35 C36 C37 179.8(8) . . . . ? C35 C36 C37 C38 2.1(14) . . . . ? C35 C36 C37 C41 -178.9(9) . . . . ? C36 C37 C38 C39 0.1(12) . . . . ? C41 C37 C38 C39 -178.8(8) . . . . ? C35 C34 C39 C38 0.5(13) . . . . ? N4 C34 C39 C38 178.9(7) . . . . ? C35 C34 C39 C42 -179.4(8) . . . . ? N4 C34 C39 C42 -1.0(12) . . . . ? C37 C38 C39 C34 -1.4(12) . . . . ? C37 C38 C39 C42 178.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.21 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.615 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.101