Synthesis and characterization of two lead-containing metal chalcogenides: Ba5Pb2Sn3S13 and Ba6PbSn3Se13
Abudurusuli, Ailijiang; Ding, Hanqin; Wu, Kui; Journal of Solid State Chemistry 255 (2017) 133–138; doi:10.1016/j.jssc.2017.08.019

data_1560346
_publ_section_title
;
 Synthesis and characterization of two lead-containing metal
 chalcogenides: Ba5Pb2Sn3S13 and Ba6PbSn3Se13
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              133
_journal_page_last               138
_journal_paper_doi               10.1016/j.jssc.2017.08.019
_journal_volume                  255
_journal_year                    2017
_chemical_formula_sum            'Ba5.25 Pb1.75 S13 Sn3'
_chemical_formula_weight         1856.47
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.208(5)
_cell_length_b                   23.499(10)
_cell_length_c                   8.838(4)
_cell_measurement_reflns_used    2022
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.46
_cell_volume                     2535.4(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12179
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    23.544
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.863
_exptl_crystal_description       block
_exptl_crystal_F_000             3182
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.078
_refine_diff_density_max         2.670
_refine_diff_density_min         -5.654
_refine_diff_density_rms         0.361
_refine_ls_extinction_coef       0.00016(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   1.110
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0433P)^2^+61.5890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                1873
_reflns_number_total             2293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            mmc5.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the built-in table derived from
the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        2535.4(18)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               1560346