#------------------------------------------------------------------------------ #$Date: 2016-03-25 14:34:44 +0200 (Fri, 25 Mar 2016) $ #$Revision: 179902 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/98/7019864.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7019864 loop_ _publ_author_name 'Sankar, Cheriyedath Raj' 'Kuropatwa, Bryan A.' 'Assoud, Abdeljalil' 'Kleinke, Holger' _publ_section_title ; Structures and properties of the ternary thallium chalcogenides Tl(2)MQ(3) (M = Zr, Hf; Q = S, Se). ; _journal_issue 32 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 9646 _journal_page_last 9650 _journal_paper_doi 10.1039/c2dt30782k _journal_volume 41 _journal_year 2012 _chemical_formula_sum 'Hf Se3 Tl2' _chemical_formula_weight 824.11 _chemical_name_systematic ; ? ; _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _atom_sites_solution_hydrogens none _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 97.435(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.1544(11) _cell_length_b 3.8812(5) _cell_length_c 10.6224(14) _cell_measurement_temperature 296(2) _cell_volume 333.36(8) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.958 _diffrn_measured_fraction_theta_max 0.958 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 2237 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 3.37 _exptl_absorpt_coefficient_mu 79.992 _exptl_absorpt_correction_T_max 0.298 _exptl_absorpt_correction_T_min 0.027 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_crystal_colour black _exptl_crystal_density_diffrn 8.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 672 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _refine_diff_density_max 3.594 _refine_diff_density_min -4.451 _refine_diff_density_rms 0.688 _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_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 39 _refine_ls_number_reflns 1061 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.172 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0421 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+2.4979P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1245 _refine_ls_wR_factor_ref 0.1284 _reflns_number_gt 967 _reflns_number_total 1061 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c2dt30782k.txt _cod_data_source_block Tl2HfSe3 _cod_original_sg_symbol_H-M P21/m _cod_database_code 7019864 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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 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 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' 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 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 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 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