New Quaternary Chalcogenides, Tl18Pb2M7Q25 (M= Ti, Zr, and Hf;Q= S and Se): Crystal Structure, Electronic Structure, and Electrical Transport Properties
Cheriyedath Raj Sankar; Anna Becker; Abdeljalil Assoud; Holger Kleinke; Inorganic Chemistry 52 (2013) 1895–1900; doi:10.1021/ic3020699

data_4333828
_publ_section_title
;
 New Quaternary Chalcogenides, Tl18Pb2M7Q25 (M= Ti, Zr, and Hf;Q= S and
 Se): Crystal Structure, Electronic Structure, and Electrical Transport
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1895
_journal_page_last               1900
_journal_paper_doi               10.1021/ic3020699
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'Pb2 S25 Tl18 Zr7'
_chemical_formula_weight         5533.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.463(3)
_cell_length_b                   17.463(3)
_cell_length_c                   17.463(3)
_cell_measurement_temperature    296(2)
_cell_volume                     5325.5(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1575
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30936
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    62.809
_exptl_absorpt_correction_T_max  0.3664
_exptl_absorpt_correction_T_min  0.1878
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    6.901
_exptl_crystal_description       plate
_exptl_crystal_F_000             9208
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.548
_refine_diff_density_min         -2.815
_refine_diff_density_rms         0.813
_refine_ls_extinction_coef       0.000114(9)
_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   1.087
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         2600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0479P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                1786
_reflns_number_total             2600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3020699_si_003_3.cif
_cod_data_source_block           Tl18Pb2Zr7S25
_cod_original_cell_volume        5325.3(14)
_cod_database_code               4333828