#------------------------------------------------------------------------------
#$Date: 2024-12-07 19:05:51 +0200 (Sat, 07 Dec 2024) $
#$Revision: 296760 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312719.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312719
loop_
_publ_author_name
'Xu, Mingyu'
'Wang, Haozhe'
'Vojvodin, Cameron'
'Yarava, Jayasubba Reddy'
'Wang, Tuo'
'Xie, Weiwei'
_publ_section_title
;
 Polymorphism of
 Pb₅(PO₄)₃OH<sub>δ</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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0195P)²] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.07377(2) 0.55577(2) 0.29630(2) 0.01897(6) Uani 1 1 d . . . . .
Pb2 Pb 0.02043(2) 0.750000 -0.02842(3) 0.01674(6) Uani 1 2 d S T P . .
Pb3 Pb 0.23350(3) 0.750000 -0.30356(4) 0.02470(8) Uani 1 2 d S T P . .
Pb4 Pb 0.27499(19) 0.750000 0.1556(2) 0.0285(2) Uani 0.71 2 d S T P . .
Pb5 Pb 0.2703(5) 0.750000 0.1277(6) 0.0496(14) Uani 0.29 2 d S T P . .
P1 P -0.16310(10) 0.53243(13) 0.07074(14) 0.0123(2) Uani 1 1 d . . . . .
P2 P 0.00299(15) 0.750000 -0.4252(2) 0.0153(4) Uani 1 2 d S T P . .
O1 O -0.0913(6) 0.750000 -0.3461(8) 0.0402(19) Uani 1 2 d S T P . .
O2 O -0.0171(5) 0.750000 0.4179(6) 0.0257(13) Uani 1 2 d S T P . .
O3 O 0.1089(4) 0.750000 0.1753(5) 0.0134(10) Uani 1 2 d S T P . .
O4 O -0.1751(4) 0.3859(4) 0.0955(4) 0.0248(9) Uani 1 1 d . . . . .
O5 O -0.1685(4) 0.5588(5) -0.0902(5) 0.0297(11) Uani 1 1 d . . . . .
O6 O -0.0618(3) 0.5794(5) 0.1249(6) 0.0311(11) Uani 1 1 d . . . . .
O7 O -0.2451(4) 0.6053(5) 0.1488(6) 0.0333(12) Uani 1 1 d . . . . .
O8 O 0.0635(4) 0.8677(5) -0.3915(7) 0.0406(14) Uani 1 1 d . . . . .
H8 H 0.099291 0.852435 -0.322954 0.061 Uiso 0.5 1 calc R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Pb4 Pb1 Pb5 4.13(11) . . ?
O2 Pb1 Pb4 95.16(11) . . ?
O2 Pb1 Pb5 96.41(12) . . ?
O3 Pb1 Pb4 37.09(13) . . ?
O3 Pb1 Pb5 35.30(14) . . ?
O3 Pb1 O2 69.77(15) . . ?
O3 Pb1 O5 85.80(15) . 5_565 ?
O3 Pb1 O6 75.47(17) . . ?
O3 Pb1 O7 74.55(17) . 6_656 ?
O5 Pb1 Pb4 67.03(12) 5_565 . ?
O5 Pb1 Pb5 64.62(13) 5_565 . ?
O5 Pb1 O2 154.68(15) 5_565 . ?
O6 Pb1 Pb4 105.49(12) . . ?
O6 Pb1 Pb5 101.73(14) . . ?
O6 Pb1 O2 81.89(19) . . ?
O6 Pb1 O5 85.71(17) . 5_565 ?
O6 Pb1 O7 146.06(16) . 6_656 ?
O7 Pb1 Pb4 40.88(12) 6_656 . ?
O7 Pb1 Pb5 44.49(14) 6_656 . ?
O7 Pb1 O2 102.13(18) 6_656 . ?
O7 Pb1 O5 76.61(17) 6_656 5_565 ?
O3 Pb2 Pb5 34.53(16) . . ?
O3 Pb2 O4 77.19(15) . 5_565 ?
O3 Pb2 O4 77.19(15) . 3 ?
O3 Pb2 O6 75.55(14) . 7_575 ?
O3 Pb2 O6 75.55(14) . . ?
O4 Pb2 Pb5 49.98(12) 3 . ?
O4 Pb2 Pb5 49.98(12) 5_565 . ?
O4 Pb2 O4 65.31(18) 3 5_565 ?
O6 Pb2 Pb5 100.19(12) . . ?
O6 Pb2 Pb5 100.19(12) 7_575 . ?
O6 Pb2 O4 150.17(14) . 3 ?
O6 Pb2 O4 150.17(14) 7_575 5_565 ?
O6 Pb2 O4 96.77(15) 7_575 3 ?
O6 Pb2 O4 96.77(15) . 5_565 ?
O6 Pb2 O6 88.0(3) 7_575 . ?
O4 Pb3 O1 82.81(18) 3 6_655 ?
O4 Pb3 O1 82.81(18) 5_565 6_655 ?
O4 Pb3 O4 67.17(19) 3 5_565 ?
O4 Pb3 O5 92.11(15) 5_565 6_655 ?
O4 Pb3 O5 92.11(14) 3 4_564 ?
O4 Pb3 O5 152.01(14) 5_565 4_564 ?
O4 Pb3 O5 152.01(14) 3 6_655 ?
O4 Pb3 O8 74.03(16) 3 . ?
O4 Pb3 O8 74.03(16) 5_565 7_575 ?
O4 Pb3 O8 102.50(18) 3 7_575 ?
O4 Pb3 O8 102.50(18) 5_565 . ?
O5 Pb3 O1 75.81(15) 6_655 6_655 ?
O5 Pb3 O1 75.81(15) 4_564 6_655 ?
O5 Pb3 O5 99.8(2) 4_564 6_655 ?
O5 Pb3 O8 131.03(16) 6_655 . ?
O5 Pb3 O8 88.65(17) 6_655 7_575 ?
O5 Pb3 O8 131.03(16) 4_564 7_575 ?
O5 Pb3 O8 88.65(17) 4_564 . ?
O8 Pb3 O1 151.60(12) 7_575 6_655 ?
O8 Pb3 O1 151.60(12) . 6_655 ?
O8 Pb3 O8 52.8(2) . 7_575 ?
Pb1 Pb4 Pb1 66.95(4) 7_575 . ?
O3 Pb4 Pb1 38.94(7) . . ?
O3 Pb4 Pb1 38.94(7) . 7_575 ?
O3 Pb4 O7 79.79(17) . 4_565 ?
O3 Pb4 O7 79.79(17) . 6_656 ?
O7 Pb4 Pb1 88.76(15) 4_565 . ?
O7 Pb4 Pb1 88.76(15) 6_656 7_575 ?
O7 Pb4 Pb1 44.60(13) 6_656 . ?
O7 Pb4 Pb1 44.60(13) 4_565 7_575 ?
O7 Pb4 O7 77.5(3) 4_565 6_656 ?
Pb1 Pb5 Pb1 65.77(11) 7_575 . ?
Pb2 Pb5 Pb1 60.61(10) . . ?
Pb2 Pb5 Pb1 60.61(10) . 7_575 ?
O3 Pb5 Pb1 37.53(9) . . ?
O3 Pb5 Pb1 37.53(9) . 7_575 ?
O3 Pb5 Pb2 35.03(16) . . ?
O3 Pb5 O7 76.0(2) . 4_565 ?
O3 Pb5 O7 76.0(2) . 6_656 ?
O7 Pb5 Pb1 84.6(2) 4_565 . ?
O7 Pb5 Pb1 43.88(14) 6_656 . ?
O7 Pb5 Pb1 43.88(14) 4_565 7_575 ?
O7 Pb5 Pb1 84.6(2) 6_656 7_575 ?
O7 Pb5 Pb2 104.4(2) 6_656 . ?
O7 Pb5 Pb2 104.4(2) 4_565 . ?
O7 Pb5 O7 70.5(3) 4_565 6_656 ?
O4 P1 O5 108.5(2) . . ?
O4 P1 O6 110.6(3) . . ?
O5 P1 O6 108.2(3) . . ?
O7 P1 O4 109.5(3) . . ?
O7 P1 O5 110.5(3) . . ?
O7 P1 O6 109.5(3) . . ?
O1 P2 O2 109.8(4) . 1_554 ?
O1 P2 O8 111.5(3) . . ?
O1 P2 O8 111.5(3) . 7_575 ?
O8 P2 O2 107.9(3) . 1_554 ?
O8 P2 O2 107.9(3) 7_575 1_554 ?
O8 P2 O8 108.2(4) 7_575 . ?
P2 O1 Pb3 179.6(5) . 6 ?
Pb1 O2 Pb1 100.0(2) . 7_575 ?
P2 O2 Pb1 110.2(2) 1_556 7_575 ?
P2 O2 Pb1 110.2(2) 1_556 . ?
Pb1 O3 Pb1 116.8(2) 7_575 . ?
Pb2 O3 Pb1 107.63(14) . 7_575 ?
Pb2 O3 Pb1 107.63(14) . . ?
Pb4 O3 Pb1 103.97(15) . . ?
Pb4 O3 Pb1 103.96(15) . 7_575 ?
Pb4 O3 Pb2 117.3(2) . . ?
Pb5 O3 Pb1 107.17(16) . 7_575 ?
Pb5 O3 Pb1 107.17(16) . . ?
Pb5 O3 Pb2 110.4(3) . . ?
Pb5 O3 Pb4 6.87(18) . . ?
Pb3 O4 Pb2 98.09(15) 5_565 5_565 ?
P1 O4 Pb2 114.1(2) . 5_565 ?
P1 O4 Pb3 133.9(2) . 5_565 ?
Pb3 O5 Pb1 108.18(15) 6 5_565 ?
P1 O5 Pb1 128.9(3) . 5_565 ?
P1 O5 Pb3 122.7(3) . 6 ?
Pb1 O6 Pb2 96.54(15) . . ?
P1 O6 Pb1 148.3(3) . . ?
P1 O6 Pb2 114.9(3) . . ?
Pb1 O7 Pb5 91.6(2) 6_556 6_556 ?
Pb4 O7 Pb1 94.52(17) 6_556 6_556 ?
Pb4 O7 Pb5 4.14(13) 6_556 6_556 ?
P1 O7 Pb1 134.1(3) . 6_556 ?
P1 O7 Pb4 126.5(3) . 6_556 ?
P1 O7 Pb5 128.0(3) . 6_556 ?
P2 O8 Pb3 99.5(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Pb4 3.624(2) . ?
Pb1 Pb5 3.681(6) . ?
Pb1 O2 2.608(4) . ?
Pb1 O3 2.347(3) . ?
Pb1 O5 2.601(5) 5_565 ?
Pb1 O6 2.450(5) . ?
Pb1 O7 2.552(5) 6_656 ?
Pb2 Pb5 3.681(6) . ?
Pb2 O3 2.255(5) . ?
Pb2 O4 2.592(5) 5_565 ?
Pb2 O4 2.592(5) 3 ?
Pb2 O6 2.527(5) . ?
Pb2 O6 2.527(5) 7_575 ?
Pb3 O1 2.753(7) 6_655 ?
Pb3 O4 2.528(4) 5_565 ?
Pb3 O4 2.528(4) 3 ?
Pb3 O5 2.573(4) 6_655 ?
Pb3 O5 2.573(4) 4_564 ?
Pb3 O8 2.725(5) 7_575 ?
Pb3 O8 2.725(5) . ?
Pb4 O3 2.252(6) . ?
Pb4 O7 2.379(5) 6_656 ?
Pb4 O7 2.379(5) 4_565 ?
Pb5 O3 2.226(9) . ?
Pb5 O7 2.581(7) 4_565 ?
Pb5 O7 2.581(7) 6_656 ?
P1 O4 1.534(4) . ?
P1 O5 1.536(4) . ?
P1 O6 1.538(5) . ?
P1 O7 1.526(5) . ?
P2 O1 1.474(7) . ?
P2 O2 1.498(6) 1_554 ?
P2 O8 1.495(5) . ?
P2 O8 1.495(5) 7_575 ?
