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_4337051
_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 S4 Tl2'
_chemical_formula_weight         922.66
_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                 109.265(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4695(19)
_cell_length_b                   8.2255(12)
_cell_length_c                   6.7103(7)
_cell_measurement_reflns_used    3259
_cell_measurement_temperature    296
_cell_measurement_theta_max      34.96
_cell_measurement_theta_min      5.58
_cell_volume                     806.03(18)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      ' 180 frames, detector distance = 60 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_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            4067
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         3.93
_diffrn_source
'sealed x-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    74.452
_exptl_absorpt_correction_T_max  0.490
_exptl_absorpt_correction_T_min  0.048
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-Shape
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    7.603
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.822
_refine_diff_density_min         -1.922
_refine_diff_density_rms         0.401
_refine_ls_extinction_coef       0.00010(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   1.011
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         1177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0268P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                799
_reflns_number_total             1177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4025316_si_002_3.cif
_cod_data_source_block           Tl2PbHfS4
_cod_original_cell_volume        806.04(17)
_cod_database_code               4337051