α-Na6Pb3(PS4)4, a Noncentrosymmetric Thiophosphate with the Novel, Saucer-Shaped [Pb3(PS4)4]6- Cluster, and Its Metastable, 3-Dimensionally Polymerized Allotrope β-Na6Pb3(PS4)4
Jennifer A. Aitken; Mercouri G. Kanatzidis; Inorganic Chemistry 40 (2001) 2938–2939; doi:10.1021/ic015511g

data_4319887
_publ_section_title
;
 \a-Na6Pb3(PS4)4, a Noncentrosymmetric Thiophosphate with the Novel,
 Saucer-Shaped [Pb3(PS4)4]6- Cluster, and Its Metastable, 3-Dimensionally
 Polymerized Allotrope \b-Na6Pb3(PS4)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2938
_journal_page_last               2939
_journal_paper_doi               10.1021/ic015511g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'Na1.5 P Pb0.75 S4'
_chemical_formula_weight         349.09
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_atom_sites_solution_hydrogens   geom
_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            16
_cell_length_a                   13.730(2)
_cell_length_b                   13.730(2)
_cell_length_c                   13.730(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2588.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Platform CCD '
_diffrn_measurement_method       'omega scan'
_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  0.0787
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9019
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    21.104
_exptl_absorpt_correction_type   Sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.015(15)
_refine_ls_extinction_coef       0.00016(5)
_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   1.162
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.459
_refine_ls_shift/su_mean         0.110
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+8.3091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                420
_reflns_number_total             483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic015511g_s1_2.cif
_cod_data_source_block           b-Na6Pb3P4S16
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        2588.1(7)
_cod_original_formula_sum        'Na1.50 P Pb0.75 S4'
_cod_database_code               4319887