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_1560345
_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            'Ba6 Pb Se13 Sn3'
_chemical_formula_weight         2413.78
_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                   12.73(3)
_cell_length_b                   24.65(5)
_cell_length_c                   9.24(2)
_cell_measurement_reflns_used    529
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.25
_cell_measurement_theta_min      3.32
_cell_volume                     2899(11)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1452
_diffrn_reflns_av_sigmaI/netI    0.1051
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13909
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    32.624
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3919
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    5.528
_exptl_crystal_description       block
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.069
_refine_diff_density_max         4.889
_refine_diff_density_min         -3.151
_refine_diff_density_rms         0.454
_refine_ls_extinction_coef       0.00020(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   0.977
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                1661
_reflns_number_total             2612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            mmc2.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        2900(11)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               1560345