#------------------------------------------------------------------------------ #$Date: 2012-08-12 00:44:28 +0300 (Sun, 12 Aug 2012) $ #$Revision: 64333 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/98/7019865.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_7019865 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_volume 41 _journal_year 2012 _chemical_formula_sum 'S3 Tl2 Zr' _chemical_formula_weight 596.14 _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 97.476(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.9159(10) _cell_length_b 3.7651(5) _cell_length_c 10.2756(13) _cell_measurement_temperature 293(2) _cell_volume 303.65(7) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _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 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 2327 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 3.06 _exptl_absorpt_coefficient_mu 55.502 _exptl_absorpt_correction_T_max 0.403 _exptl_absorpt_correction_T_min 0.215 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_crystal_colour black _exptl_crystal_density_diffrn 6.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 500 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.393 _refine_diff_density_min -1.379 _refine_diff_density_rms 0.300 _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_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 38 _refine_ls_number_reflns 1007 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0269 _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^)+(0.0186P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.0589 _reflns_number_gt 850 _reflns_number_total 1007 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c2dt30782k.txt _[local]_cod_data_source_block Tl2ZrS3 _[local]_cod_cif_authors_sg_H-M P21/m _cod_database_code 7019865 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 0.06374(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 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' 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 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 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 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