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_2108804
_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_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            'As0.195 O21 P0.805 Pb2 U3'
_chemical_formula_weight         1578.9
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_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_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 108.90(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0189(7)
_cell_length_b                   17.137(1)
_cell_length_c                   8.131(1)
_cell_measurement_temperature    296.8
_cell_volume                     925.29(17)
_diffrn_ambient_temperature      296.8
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.93
_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  0.148
_diffrn_reflns_av_unetI/netI     0.1056
_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            21107
_diffrn_reflns_theta_full        28.58
_diffrn_reflns_theta_max         29.48
_diffrn_reflns_theta_min         2.9
_exptl_absorpt_coefficient_mu    46.588
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    5.6671
_exptl_crystal_F_000             1319
_exptl_crystal_size_max          0.038
_exptl_crystal_size_mid          0.013
_exptl_crystal_size_min          0.007
_refine_diff_density_max         6.61
_refine_diff_density_min         -4.02
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.6968
_refine_ls_goodness_of_fit_ref   1.4900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    13
_refine_ls_number_parameters     134
_refine_ls_number_reflns         4200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.0247
_refine_ls_shift/su_mean         0.0013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0036I^2^)
_refine_ls_weighting_scheme      sigma
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_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ra5095sup2.txt
_cod_data_source_block           I
_cod_original_cell_volume        925.3(2)
_cod_original_formula_sum        'Pb2 U3 As.195 O21 P0.805'
_cod_database_code               2108804