Polymorphism of Pb<sub>5</sub>(PO<sub>4</sub>)<sub>3</sub>OH<sub>δ</sub> within the LK-99 mixture.
Xu, Mingyu; Wang, Haozhe; Vojvodin, Cameron; Yarava, Jayasubba Reddy; Wang, Tuo; Xie, Weiwei; Acta crystallographica Section B, Structural science, crystal engineering and materials 80 (2024) 746–750; doi:10.1107/S2052520624010023

data_2312719
_publ_section_title
;
 Polymorphism of
 Pb<sub>5</sub>(PO<sub>4</sub>)<sub>3</sub>OH<sub>&#x3b4;</sub> within the
 LK-99 mixture.
;
_journal_coeditor_code           RM5078
_journal_issue                   6
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              746
_journal_page_last               750
_journal_paper_doi               10.1107/S2052520624010023
_journal_volume                  80
_journal_year                    2024
_chemical_formula_moiety         'H O13 P3 Pb5'
_chemical_formula_sum            'Cu0 H O13 P3 Pb5'
_chemical_formula_weight         1337.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5137(4)
_cell_length_b                   10.2904(4)
_cell_length_c                   9.3838(3)
_cell_measurement_reflns_used    15385
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41.0250
_cell_measurement_theta_min      2.6200
_cell_volume                     1304.92(8)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'XtalLAB Synergy, Dualflex, Hypix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1257
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48595
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         41.236
_diffrn_reflns_theta_min         2.643
_exptl_absorpt_coefficient_mu    64.731
_exptl_absorpt_correction_T_max  0.177
_exptl_absorpt_correction_T_min  0.057
_exptl_absorpt_correction_type   analytical
_exptl_crystal_density_diffrn    6.810
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.049
_refine_diff_density_max         3.786
_refine_diff_density_min         -5.989
_refine_diff_density_rms         0.511
_refine_ls_extinction_coef       0.00025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         4458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2940
_reflns_number_total             4458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rm5078.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2312719.cif.'
_cod_original_cell_volume        1304.93(7)
_cod_database_code               2312719
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.140
_shelx_estimated_absorpt_t_min   0.079
_olex2_refinement_description
;
1. Others
 Fixed Sof: Pb4(0.355) Pb5(0.145) H8(0.5)
2.a Tetrahedral OH refined with riding coordinates:
 O8(H8)
;
_shelx_res_checksum              61433
_shelx_hkl_checksum              32103
_olex2_submission_special_instructions 'No special instructions were received'