# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email kleinke@uwaterloo.ca _publ_contact_author_name 'Holger Kleinke ' _publ_author_name 'Holger Kleinke' data_Tl2HfSe3 _database_code_depnum_ccdc_archive 'CCDC 876405' #TrackingRef '- Tl2HfSe3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Hf Se3 Tl2' _chemical_formula_weight 824.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 '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 P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.1544(11) _cell_length_b 3.8812(5) _cell_length_c 10.6224(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.435(2) _cell_angle_gamma 90.00 _cell_volume 333.36(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 8.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 79.992 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.027 _exptl_absorpt_correction_T_max 0.298 _exptl_absorpt_process_details SADABS _exptl_special_details ; APEX2 ; _diffrn_ambient_temperature 296(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 ? _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 2237 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 30.00 _reflns_number_total 1061 _reflns_number_gt 967 _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^)+(0.0558P)^2^+2.4979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0065(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1061 _refine_ls_number_parameters 39 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _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 Tl1 Tl 0.06445(9) 0.2500 0.65805(7) 0.0228(2) Uani 1 2 d S . . Tl2 Tl 0.74973(8) 0.2500 0.00293(6) 0.0217(2) Uani 1 2 d S . . Hf1 Hf 0.40960(7) 0.2500 0.33423(5) 0.0078(2) Uani 1 2 d S . . Se1 Se 0.13036(18) 0.2500 0.19044(15) 0.0130(4) Uani 1 2 d S . . Se2 Se 0.45271(17) 0.2500 0.78917(13) 0.0086(3) Uani 1 2 d S . . Se3 Se 0.69076(16) 0.2500 0.51355(12) 0.0066(3) Uani 1 2 d S . . 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 0.0223(4) 0.0216(4) 0.0246(4) 0.000 0.0033(3) 0.000 Tl2 0.0275(4) 0.0222(4) 0.0149(4) 0.000 0.0015(3) 0.000 Hf1 0.0101(3) 0.0067(3) 0.0064(4) 0.000 0.0005(2) 0.000 Se1 0.0116(7) 0.0125(7) 0.0134(7) 0.000 -0.0040(5) 0.000 Se2 0.0121(6) 0.0059(6) 0.0084(7) 0.000 0.0037(5) 0.000 Se3 0.0085(6) 0.0053(6) 0.0060(6) 0.000 0.0014(5) 0.000 _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 Se1 3.0888(14) 3_566 ? Tl1 Se1 3.0888(14) 3_556 ? Tl1 Se3 3.2297(16) 1_455 ? Tl1 Se2 3.2898(16) . ? Tl2 Se1 3.0759(14) 3_655 ? Tl2 Se1 3.0759(14) 3_665 ? Tl2 Se2 3.0981(15) 1_554 ? Hf1 Se1 2.5725(16) . ? Hf1 Se2 2.6694(10) 3_656 ? Hf1 Se2 2.6694(10) 3_666 ? Hf1 Se3 2.7189(10) 3_666 ? Hf1 Se3 2.7189(10) 3_656 ? Hf1 Se3 2.7847(14) . ? Se1 Tl2 3.0759(14) 3_655 ? Se1 Tl2 3.0759(14) 3_665 ? Se1 Tl1 3.0888(14) 3_556 ? Se1 Tl1 3.0888(14) 3_566 ? Se2 Hf1 2.6694(10) 3_656 ? Se2 Hf1 2.6694(10) 3_666 ? Se2 Tl2 3.0981(15) 1_556 ? Se3 Hf1 2.7189(10) 3_666 ? Se3 Hf1 2.7189(10) 3_656 ? Se3 Tl1 3.2297(16) 1_655 ? 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 Se1 Tl1 Se1 77.84(4) 3_566 3_556 ? Se1 Tl1 Se3 74.36(4) 3_566 1_455 ? Se1 Tl1 Se3 74.36(4) 3_556 1_455 ? Se1 Tl1 Se2 108.12(4) 3_566 . ? Se1 Tl1 Se2 108.12(4) 3_556 . ? Se3 Tl1 Se2 176.71(4) 1_455 . ? Se1 Tl2 Se1 78.23(4) 3_655 3_665 ? Se1 Tl2 Se2 78.26(4) 3_655 1_554 ? Se1 Tl2 Se2 78.26(4) 3_665 1_554 ? Se1 Hf1 Se2 96.01(4) . 3_656 ? Se1 Hf1 Se2 96.01(4) . 3_666 ? Se2 Hf1 Se2 93.27(4) 3_656 3_666 ? Se1 Hf1 Se3 92.39(4) . 3_666 ? Se2 Hf1 Se3 171.49(5) 3_656 3_666 ? Se2 Hf1 Se3 87.21(3) 3_666 3_666 ? Se1 Hf1 Se3 92.39(4) . 3_656 ? Se2 Hf1 Se3 87.21(3) 3_656 3_656 ? Se2 Hf1 Se3 171.49(5) 3_666 3_656 ? Se3 Hf1 Se3 91.08(4) 3_666 3_656 ? Se1 Hf1 Se3 173.36(5) . . ? Se2 Hf1 Se3 88.54(4) 3_656 . ? Se2 Hf1 Se3 88.54(4) 3_666 . ? Se3 Hf1 Se3 82.98(4) 3_666 . ? Se3 Hf1 Se3 82.98(4) 3_656 . ? Hf1 Se1 Tl2 93.61(4) . 3_655 ? Hf1 Se1 Tl2 93.61(4) . 3_665 ? Tl2 Se1 Tl2 78.23(4) 3_655 3_665 ? Hf1 Se1 Tl1 99.56(5) . 3_556 ? Tl2 Se1 Tl1 100.424(16) 3_655 3_556 ? Tl2 Se1 Tl1 166.82(6) 3_665 3_556 ? Hf1 Se1 Tl1 99.56(5) . 3_566 ? Tl2 Se1 Tl1 166.82(6) 3_655 3_566 ? Tl2 Se1 Tl1 100.424(17) 3_665 3_566 ? Tl1 Se1 Tl1 77.84(4) 3_556 3_566 ? Hf1 Se2 Hf1 93.27(4) 3_656 3_666 ? Hf1 Se2 Tl2 91.22(4) 3_656 1_556 ? Hf1 Se2 Tl2 91.22(4) 3_666 1_556 ? Hf1 Se2 Tl1 103.59(4) 3_656 . ? Hf1 Se2 Tl1 103.59(4) 3_666 . ? Tl2 Se2 Tl1 158.21(5) 1_556 . ? Hf1 Se3 Hf1 91.08(4) 3_666 3_656 ? Hf1 Se3 Hf1 97.02(4) 3_666 . ? Hf1 Se3 Hf1 97.02(4) 3_656 . ? Hf1 Se3 Tl1 93.18(4) 3_666 1_655 ? Hf1 Se3 Tl1 93.18(4) 3_656 1_655 ? Hf1 Se3 Tl1 165.41(5) . 1_655 ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 3.594 _refine_diff_density_min -4.451 _refine_diff_density_rms 0.688 # Attachment '- Tl2ZrS3.cif' data_Tl2ZrS3 _database_code_depnum_ccdc_archive 'CCDC 876406' #TrackingRef '- Tl2ZrS3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'S3 Tl2 Zr' _chemical_formula_weight 596.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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 P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.9159(10) _cell_length_b 3.7651(5) _cell_length_c 10.2756(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.476(2) _cell_angle_gamma 90.00 _cell_volume 303.65(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 55.502 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.215 _exptl_absorpt_correction_T_max 0.403 _exptl_absorpt_process_details SADABS _exptl_special_details ; APEX2 ; _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 ? _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 2327 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 30.00 _reflns_number_total 1007 _reflns_number_gt 850 _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^)+(0.0186P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1007 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0589 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 Tl1 Tl 0.06374(5) 0.2500 0.66029(4) 0.02600(14) Uani 1 2 d S . . Tl2 Tl 0.75009(5) 0.2500 0.00227(3) 0.02429(14) Uani 1 2 d S . . Zr1 Zr 0.41111(10) 0.2500 0.33548(7) 0.01063(17) Uani 1 2 d S . . S1 S 0.1362(3) 0.2500 0.1927(2) 0.0161(5) Uani 1 2 d S . . S2 S 0.4565(3) 0.2500 0.7868(2) 0.0131(4) Uani 1 2 d S . . S3 S 0.6888(3) 0.2500 0.51506(19) 0.0105(4) Uani 1 2 d S . . 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 0.0263(2) 0.0236(3) 0.0279(2) 0.000 0.00271(16) 0.000 Tl2 0.0291(2) 0.0243(3) 0.01895(18) 0.000 0.00098(14) 0.000 Zr1 0.0111(4) 0.0097(4) 0.0108(3) 0.000 0.0005(3) 0.000 S1 0.0147(10) 0.0161(12) 0.0161(9) 0.000 -0.0035(8) 0.000 S2 0.0162(10) 0.0095(11) 0.0141(9) 0.000 0.0045(8) 0.000 S3 0.0100(9) 0.0108(11) 0.0109(8) 0.000 0.0015(7) 0.000 _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 S1 2.9924(18) 3_556 ? Tl1 S1 2.9924(18) 3_566 ? Tl1 S3 3.144(2) 1_455 ? Tl1 Tl1 3.7651(5) 1_545 ? Tl1 Tl1 3.7651(5) 1_565 ? Tl2 S1 2.9725(18) 3_655 ? Tl2 S1 2.9725(18) 3_665 ? Tl2 S2 2.994(2) 1_554 ? Tl2 Tl2 3.7651(5) 1_545 ? Tl2 Tl2 3.7651(5) 1_565 ? Zr1 S1 2.461(2) . ? Zr1 S2 2.5618(15) 3_656 ? Zr1 S2 2.5618(15) 3_666 ? Zr1 S3 2.6162(14) 3_666 ? Zr1 S3 2.6162(14) 3_656 ? Zr1 S3 2.680(2) . ? S1 Tl2 2.9725(18) 3_655 ? S1 Tl2 2.9725(18) 3_665 ? S1 Tl1 2.9924(18) 3_556 ? S1 Tl1 2.9924(18) 3_566 ? S2 Zr1 2.5618(15) 3_656 ? S2 Zr1 2.5618(15) 3_666 ? S2 Tl2 2.994(2) 1_556 ? S3 Zr1 2.6162(14) 3_666 ? S3 Zr1 2.6162(14) 3_656 ? S3 Tl1 3.144(2) 1_655 ? 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 S1 Tl1 S1 77.97(6) 3_556 3_566 ? S1 Tl1 S3 73.20(5) 3_556 1_455 ? S1 Tl1 S3 73.20(5) 3_566 1_455 ? S1 Tl1 Tl1 51.02(3) 3_556 1_545 ? S1 Tl1 Tl1 128.98(3) 3_566 1_545 ? S3 Tl1 Tl1 90.0 1_455 1_545 ? S1 Tl1 Tl1 128.98(3) 3_556 1_565 ? S1 Tl1 Tl1 51.02(3) 3_566 1_565 ? S3 Tl1 Tl1 90.0 1_455 1_565 ? Tl1 Tl1 Tl1 180.00(2) 1_545 1_565 ? S1 Tl2 S1 78.59(6) 3_655 3_665 ? S1 Tl2 S2 77.03(5) 3_655 1_554 ? S1 Tl2 S2 77.03(5) 3_665 1_554 ? S1 Tl2 Tl2 50.70(3) 3_655 1_545 ? S1 Tl2 Tl2 129.30(3) 3_665 1_545 ? S2 Tl2 Tl2 90.0 1_554 1_545 ? S1 Tl2 Tl2 129.30(3) 3_655 1_565 ? S1 Tl2 Tl2 50.70(3) 3_665 1_565 ? S2 Tl2 Tl2 90.0 1_554 1_565 ? Tl2 Tl2 Tl2 180.000(12) 1_545 1_565 ? S1 Zr1 S2 95.40(7) . 3_656 ? S1 Zr1 S2 95.40(7) . 3_666 ? S2 Zr1 S2 94.59(7) 3_656 3_666 ? S1 Zr1 S3 92.21(7) . 3_666 ? S2 Zr1 S3 172.24(7) 3_656 3_666 ? S2 Zr1 S3 86.18(5) 3_666 3_666 ? S1 Zr1 S3 92.21(7) . 3_656 ? S2 Zr1 S3 86.18(5) 3_656 3_656 ? S2 Zr1 S3 172.24(7) 3_666 3_656 ? S3 Zr1 S3 92.04(7) 3_666 3_656 ? S1 Zr1 S3 173.18(8) . . ? S2 Zr1 S3 89.22(6) 3_656 . ? S2 Zr1 S3 89.22(6) 3_666 . ? S3 Zr1 S3 83.07(6) 3_666 . ? S3 Zr1 S3 83.07(6) 3_656 . ? Zr1 S1 Tl2 94.60(7) . 3_655 ? Zr1 S1 Tl2 94.60(7) . 3_665 ? Tl2 S1 Tl2 78.59(6) 3_655 3_665 ? Zr1 S1 Tl1 100.59(6) . 3_556 ? Tl2 S1 Tl1 99.684(17) 3_655 3_556 ? Tl2 S1 Tl1 164.81(8) 3_665 3_556 ? Zr1 S1 Tl1 100.59(6) . 3_566 ? Tl2 S1 Tl1 164.81(8) 3_655 3_566 ? Tl2 S1 Tl1 99.684(17) 3_665 3_566 ? Tl1 S1 Tl1 77.97(6) 3_556 3_566 ? Zr1 S2 Zr1 94.59(7) 3_656 3_666 ? Zr1 S2 Tl2 92.00(6) 3_656 1_556 ? Zr1 S2 Tl2 92.00(6) 3_666 1_556 ? Zr1 S3 Zr1 92.04(6) 3_666 3_656 ? Zr1 S3 Zr1 96.93(6) 3_666 . ? Zr1 S3 Zr1 96.93(6) 3_656 . ? Zr1 S3 Tl1 93.45(5) 3_666 1_655 ? Zr1 S3 Tl1 93.45(5) 3_656 1_655 ? Zr1 S3 Tl1 165.02(8) . 1_655 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.393 _refine_diff_density_min -1.379 _refine_diff_density_rms 0.300