New Layered-Type Quaternary Chalcogenides, Tl2PbMQ4 (M= Zr, Hf;Q= S, Se): Structure, Electronic Structure, and Electrical Transport Properties
Cheriyedath Raj Sankar; Abdeljalil Assoud; Holger Kleinke; Inorganic Chemistry 52 (2013) 13869–13874; doi:10.1021/ic4025316

data_4337052
_publ_section_title
;
 New Layered-Type Quaternary Chalcogenides, Tl2PbMQ4 (M= Zr, Hf;Q= S, Se):
 Structure, Electronic Structure, and Electrical Transport Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13869
_journal_page_last               13874
_journal_paper_doi               10.1021/ic4025316
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'Hf Pb Se4 Tl2'
_chemical_formula_weight         1110.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 109.121(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9480(6)
_cell_length_b                   8.4720(3)
_cell_length_c                   6.9733(2)
_cell_measurement_temperature    296(2)
_cell_volume                     890.19(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4863
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    82.832
_exptl_absorpt_correction_T_max  0.29
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    8.284
_exptl_crystal_description       plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.188
_refine_diff_density_min         -2.094
_refine_diff_density_rms         0.272
_refine_ls_extinction_coef       0.00074(3)
_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   1.106
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         1055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0171
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0152P)^2^+7.8481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0425
_reflns_number_gt                986
_reflns_number_total             1055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4025316_si_002_4.cif
_cod_data_source_block           Tl2PbHfSe4
_cod_database_code               4337052