Mixed-Valence Uranium(V,VI) and Uranyl Oxyhydroxides Synthesized under High-Temperature, High-Pressure Hydrothermal Conditions: Na5[U5O16(OH)2] and Na5[U5O17(OH)]
Hsin-Kuang Liu; Kwang-Hwa Lii; Inorganic Chemistry 52 (2013) 9172–9174; doi:10.1021/ic401690s

data_4335800
_publ_section_title
;
 Mixed-Valence Uranium(V,VI) and Uranyl Oxyhydroxides Synthesized under
 High-Temperature, High-Pressure Hydrothermal Conditions: Na5[U5O16(OH)2]
 and Na5[U5O17(OH)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9172
_journal_page_last               9174
_journal_paper_doi               10.1021/ic401690s
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'H2 Na5 O18 U5'
_chemical_formula_weight         1595.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.4140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2675(4)
_cell_length_b                   19.7275(6)
_cell_length_c                   6.8643(6)
_cell_measurement_temperature    296(2)
_cell_volume                     1628.36(16)
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            14500
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    49.784
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS program'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    6.507
_exptl_crystal_description       foliated
_exptl_crystal_F_000             2644
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.133
_refine_diff_density_min         -3.945
_refine_diff_density_rms         0.783
_refine_ls_extinction_coef       0.000089(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+4.7270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                1723
_reflns_number_total             2013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401690s_si_002.cif
_cod_data_source_block           nauo
_cod_database_code               4335800