Revealing hydrogen atoms in a highly-absorbing material: an X-ray diffraction study and Torque method calculations for lead-uranyl-oxide mineral curite
Ghazisaeed, Seyedayat; Kiefer, Boris; Plášil, Jakub; RSC Advances 9 (2019) 10058–; doi:10.1039/C8RA09557D

data_7232555
_publ_section_title
;
 Revealing hydrogen atoms in a highly-absorbing material: an X-ray
 diffraction study and Torque method calculations for lead-uranyl-oxide
 mineral curite
;
_journal_issue                   18
_journal_name_full               'RSC Advances'
_journal_page_first              10058
_journal_paper_doi               10.1039/C8RA09557D
_journal_volume                  9
_journal_year                    2019
_chemical_compound_source        Mineral
_chemical_formula_sum            'H8 O32 Pb3.017 U8'
_chemical_formula_weight         3049.4
_chemical_name_systematic        Curite
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2018-11-20 deposited with the CCDC.    2019-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5510(10)
_cell_length_b                   8.3760(4)
_cell_length_c                   13.0107(9)
_cell_measurement_reflns_used    5238
_cell_measurement_temperature    297.4(3)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      3.51
_cell_volume                     1367.78(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_diffrn_ambient_temperature      297.4
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4054
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.94
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, 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  0.0633
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15611
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    65.779
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.3829
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   Jana2006
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    7.4041
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             2495
_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.008
_refine_diff_density_max         5.93
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.67
_refine_ls_goodness_of_fit_ref   1.56
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1732
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0358
_refine_ls_shift/su_mean         0.0027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0004I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                1374
_reflns_number_total             1732
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            c8ra09557d2.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-P -2xabc;-2yb;-2zac'
_cod_database_code               7232555