Redetermination of the crystal structure of RhPb~2~ from single-crystal X-ray diffraction data, revealing a rhodium deficiency
Mochiku, Takashi; Matsushita, Yoshitaka; Subotić, Nikola; Kashiwagi, Takanari; Kadowaki, Kazuo; Acta Crystallographica Section E 77 (2021) 1327–1329; doi:10.1107/S2056989021012275

data_2243970
_publ_section_title
;
 Redetermination of the crystal structure of RhPb~2~ from single-crystal
 X-ray diffraction data, revealing a rhodium deficiency
;
_journal_coeditor_code           WM5626
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1327
_journal_page_last               1329
_journal_paper_doi               10.1107/S2056989021012275
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'Rh0.95 Pb2'
_chemical_formula_moiety         'Rh0.95 Pb2'
_chemical_formula_sum            'Pb2 Rh0.95'
_chemical_formula_weight         512.14
_chemical_name_systematic
;
Rhodium dilead
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7068(4)
_cell_length_b                   6.7068(4)
_cell_length_c                   5.8623(6)
_cell_measurement_reflns_used    295
_cell_measurement_temperature    295.15
_cell_measurement_theta_max      30.1980
_cell_measurement_theta_min      6.0470
_cell_volume                     263.69(3)
_computing_cell_refinement       'CrysAlisPro (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro (Rigaku OD, 2019)'
_computing_molecular_graphics    '<i>OLEX2</i> (Dolomanov et al., 2009)'
_computing_publication_material  '<i>OLEX2</i> (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      295.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            461
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.234
_diffrn_reflns_theta_min         4.297
_exptl_absorpt_coefficient_mu    132.868
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour            'metallic dark grey'
_exptl_crystal_density_diffrn    12.900
_exptl_crystal_description       irregular
_exptl_crystal_F_000             827
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.958
_refine_diff_density_min         -1.564
_refine_ls_extinction_coef       0.0030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL2018/3 (Sheldrick 2015b)'
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0130P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0395
_refine_ls_wR_factor_ref         0.0415
_reflns_number_gt                88
_reflns_number_total             117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5626sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        263.69(4)
_cod_original_formula_sum        'Rh0.95 Pb2 '
_cod_database_code               2243970
_shelx_estimated_absorpt_t_min   0.024
_shelx_estimated_absorpt_t_max   0.105
_shelx_hkl_checksum              87845
_shelx_res_checksum              46068
_cod_database_fobs_code 2243970