Crystal structure of the uranyl arsenate mineral hügelite, Pb~2~(UO~2~)~3~O~2~(AsO~4~)~2~(H~2~O)~5~, revisited: a correct unit cell, twinning and hydrogen bonding
Plášil, Jakub; Petříček, Václav; Škácha, Pavel; Acta Crystallographica Section B 77 (2021) –; doi:10.1107/S2052520621004091

data_2108803
_publ_section_title
;
 Crystal structure of the uranyl arsenate mineral h\"ugelite,
 Pb~2~(UO~2~)~3~O~2~(AsO~4~)~2~(H~2~O)~5~, revisited: a correct unit cell,
 twinning and hydrogen bonding
;
_journal_coeditor_code           RA5095SUP1
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520621004091
_journal_volume                  77
_journal_year                    2021
_chemical_formula_sum            'As0.201 H10 O21 P0.799 Pb2 U3'
_chemical_formula_weight         1587.7
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'Jana2020 Version : 02/02/2021'
_audit_update_record
;
2021-02-05 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 108.886(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0258(3)
_cell_length_b                   17.1769(5)
_cell_length_c                   8.1463(7)
_cell_measurement_reflns_used    7003
_cell_measurement_temperature    297.1(4)
_cell_measurement_theta_max      29.28
_cell_measurement_theta_min      2.65
_cell_volume                     930.18(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_diffrn_ambient_temperature      297.1
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4054
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.92
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19219
_diffrn_reflns_theta_full        28.52
_diffrn_reflns_theta_max         29.78
_diffrn_reflns_theta_min         2.38
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    46.295
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    5.6687
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1338
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.005
_refine_diff_density_max         5.04
_refine_diff_density_min         -4.02
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.1145
_refine_ls_goodness_of_fit_ref   1.0670
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    27
_refine_ls_number_parameters     141
_refine_ls_number_reflns         19152
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.0156
_refine_ls_shift/su_mean         0.0023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0036I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                12864
_reflns_number_total             19152
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ra5095sup1.cif
_cod_data_source_block           global
_cod_original_formula_sum        'Pb2 U3 As.201 O21 P0.799 H10'
_cod_database_code               2108803