Reinvestigation of trisodium dihydroxidotetraoxidoneptunate(VII)
Grigoriev, Mikhail S.; Krot, Nikolai N.; Acta Crystallographica Section E 63 (2007) i176–i176; doi:10.1107/S1600536807039025

data_2215262
_publ_section_title
;
 Reinvestigation of trisodium dihydroxidotetraoxidoneptunate(VII)
;
_journal_coeditor_code           SG2188
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i176
_journal_page_last               i176
_journal_paper_doi               10.1107/S1600536807039025
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'Na3 [Np O4 (O H)2]'
_chemical_formula_moiety         '3Na + , H2 Np O6 3-'
_chemical_formula_sum            'H2 Na3 Np O6'
_chemical_formula_weight         403.99
_chemical_name_systematic
;
trisodium dihydroxidotetraoxidoneptunate(VII)
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.0791(6)
_cell_length_b                   5.9534(2)
_cell_length_c                   10.2062(3)
_cell_measurement_reflns_used    8824
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.00
_cell_measurement_theta_min      4.06
_cell_volume                     1220.04(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1998)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21081
_diffrn_reflns_theta_full        45.00
_diffrn_reflns_theta_max         45.00
_diffrn_reflns_theta_min         4.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.209
_exptl_absorpt_correction_T_max  0.5460
_exptl_absorpt_correction_T_min  0.3779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.071
_refine_diff_density_min         -1.490
_refine_ls_abs_structure_details 'Flack (1983), with 1136 Friedel pairs'
_refine_ls_abs_structure_Flack   0.039(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         2442
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.0141
_refine_ls_R_factor_gt           0.0116
_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^)+2.58P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0219
_refine_ls_wR_factor_ref         0.0222
_reflns_number_gt                2258
_reflns_number_total             2442
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sg2188.cif
_cod_data_source_block           I
_cod_database_code               2215262
_cod_database_fobs_code          2215262