Reinvestigation of trisodium dihydroxidotetraoxidoneptunate(VII) dihydrate
Grigoriev, Mikhail S.; Krot, Nikolai N.; Acta Crystallographica Section E 64 (2008) i6–i6; doi:10.1107/S1600536807066962

data_2217287
_publ_section_title
;
 Reinvestigation of trisodium dihydroxidotetraoxidoneptunate(VII)
 dihydrate
;
_journal_coeditor_code           SG2217
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i6
_journal_page_last               i6
_journal_paper_doi               10.1107/S1600536807066962
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'Na3 [Np O4 (O H)2], 2H2 O'
_chemical_formula_moiety         '3(Na +), H2 Np O6 3-, 2(H2 O)'
_chemical_formula_sum            'H6 Na3 Np O8'
_chemical_formula_weight         440.02
_chemical_name_systematic
;
trisodium dihydroxidotetraoxidoneptunate(VII) dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.9139(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8166(3)
_cell_length_b                   7.7703(2)
_cell_length_c                   6.8211(2)
_cell_measurement_reflns_used    5517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.00
_cell_measurement_theta_min      3.86
_cell_volume                     381.60(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1998)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL97 (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL97 (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEXII area-detector'
_diffrn_measurement_method       '\w and \f'
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16264
_diffrn_reflns_theta_full        40.00
_diffrn_reflns_theta_max         40.00
_diffrn_reflns_theta_min         3.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.790
_exptl_absorpt_correction_T_max  0.7700
_exptl_absorpt_correction_T_min  0.5219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.829
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.882
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         2357
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0142
_refine_ls_R_factor_gt           0.0095
_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^)+(0.0059P)^2^+0.087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0199
_refine_ls_wR_factor_ref         0.0213
_reflns_number_gt                1920
_reflns_number_total             2357
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sg2217.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2217287
_cod_database_fobs_code          2217287