#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/74/2017426.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2017426
loop_
_publ_author_name
'Grigoriev, Mikhail S.'
'Krot, Nikolai N.'
_publ_section_title
;
 Novel heptavalent actinide compounds: tetrasodium
 dihydroxidotetraoxidoneptunate(VII) hydroxide dihydrate and its
 plutonium analogue
;
_journal_coeditor_code           FA3208
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i91
_journal_page_last               i93
_journal_paper_doi               10.1107/S0108270109044394
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'Na4 [Np O4 (O H)2] (O H), 2H2 O'
_chemical_formula_moiety         '4(Na +), H2 Np O6 3-, 2(H2 O), H O -'
_chemical_formula_sum            'H7 Na4 Np O9'
_chemical_formula_weight         480.02
_chemical_name_systematic
;
Tetrasodium dihydroxidotetraoxidoneptunate(VII) hydroxide dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.007(2)
_cell_angle_beta                 101.213(2)
_cell_angle_gamma                105.935(2)
_cell_formula_units_Z            2
_cell_length_a                   5.9632(2)
_cell_length_b                   8.1157(2)
_cell_length_c                   10.9434(3)
_cell_measurement_reflns_used    8013
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.00
_cell_measurement_theta_min      2.01
_cell_volume                     471.36(3)
_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, 2008)'
_computing_publication_material  'SHELXTL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
'Bruker Kappa  APEXII area-detector diffractometer'
_diffrn_measurement_method       'ω- and φ-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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22639
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.325
_exptl_absorpt_correction_T_max  0.625
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Sheldrick, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.158
_refine_diff_density_min         -1.824
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         4029
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0215
_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/[σ²(Fo²)+(0.0277P)²+0.1404P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                3812
_reflns_number_total             4029
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fa3208.cif
_cod_data_source_block           I
_cod_original_cell_volume        471.36(2)
_cod_database_code               2017426
_cod_database_fobs_code          2017426
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Np Np1 0.63709(2) 0.414646(15) 0.247923(11) 0.00968(3) Uani d . 1 . .
Na Na1 0.2127(2) 0.46725(19) 0.41560(13) 0.0193(3) Uani d . 1 . .
Na Na2 1.0543(2) 0.3396(2) 0.07342(14) 0.0211(3) Uani d . 1 . .
Na Na3 0.5236(3) 0.72145(19) 0.09527(14) 0.0211(3) Uani d . 1 . .
Na Na4 0.6165(3) 0.8535(2) 0.42625(15) 0.0253(3) Uani d . 1 . .
O O1 0.8539(4) 0.2829(3) 0.2395(3) 0.0178(4) Uani d . 1 . .
O O2 0.3952(4) 0.2286(3) 0.1023(2) 0.0172(4) Uani d . 1 . .
O O3 0.4227(4) 0.5527(3) 0.2527(3) 0.0151(4) Uani d . 1 . .
O O4 0.8743(4) 0.6025(3) 0.3929(2) 0.0180(4) Uani d . 1 . .
O O5 0.4867(5) 0.3026(3) 0.4010(2) 0.0171(4) Uani d D 1 . .
H H5 0.421(7) 0.193(3) 0.373(5) 0.021 Uiso d D 1 . .
O O6 0.7915(4) 0.5368(3) 0.0952(2) 0.0155(4) Uani d D 1 . .
H H6 0.907(5) 0.624(4) 0.138(4) 0.019 Uiso d D 1 . .
O O7 0.2470(5) -0.0813(3) 0.3625(3) 0.0218(5) Uani d D 1 . .
H H7 0.186(8) -0.155(5) 0.392(5) 0.026 Uiso d D 1 . .
O O8 0.2420(5) -0.1323(4) 0.1170(3) 0.0249(5) Uani d D 1 . .
H H8A 0.244(9) -0.113(6) 0.197(2) 0.037 Uiso d D 1 . .
H H8B 0.279(9) -0.027(4) 0.110(5) 0.037 Uiso d D 1 . .
O O9 0.8145(5) 0.9542(4) 0.2823(3) 0.0251(5) Uani d D 1 . .
H H9A 0.835(7) 1.059(4) 0.276(5) 0.038 Uiso d D 1 . .
H H9B 0.952(5) 0.958(6) 0.320(5) 0.038 Uiso d D 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Np1 O2 . . 91.52(10) ?
O1 Np1 O3 . . 177.96(10) ?
O1 Np1 O4 . . 89.53(10) ?
O1 Np1 O5 . . 93.62(9) ?
O1 Np1 O6 . . 87.44(9) ?
O2 Np1 O3 . . 88.67(10) ?
O2 Np1 O4 . . 178.95(9) ?
O2 Np1 O5 . . 93.47(10) ?
O2 Np1 O6 . . 87.60(9) ?
O3 Np1 O4 . . 90.28(10) ?
O3 Np1 O5 . . 88.40(9) ?
O3 Np1 O6 . . 90.54(9) ?
O4 Np1 O5 . . 86.58(10) ?
O4 Np1 O6 . . 92.33(9) ?
O5 Np1 O6 . . 178.47(8) ?
O5 Na1 O5 2_666 . 88.77(9) ?
O5 Na1 O1 2_666 1_455 166.05(10) ?
O5 Na1 O1 . 1_455 105.19(10) ?
O5 Na1 O4 2_666 2_666 74.58(9) ?
O5 Na1 O4 . 2_666 93.43(9) ?
O1 Na1 O4 1_455 2_666 104.25(9) ?
O5 Na1 O3 2_666 . 93.78(9) ?
O5 Na1 O3 . . 74.72(8) ?
O1 Na1 O3 1_455 . 89.78(9) ?
O4 Na1 O3 2_666 . 163.76(9) ?
O5 Na1 O4 2_666 1_455 101.00(9) ?
O5 Na1 O4 . 1_455 170.10(10) ?
O1 Na1 O4 1_455 1_455 65.05(8) ?
O4 Na1 O4 2_666 1_455 90.80(9) ?
O3 Na1 O4 . 1_455 102.70(9) ?
O8 Na2 O1 2_655 . 100.12(11) ?
O8 Na2 O2 2_655 1_655 106.87(10) ?
O1 Na2 O2 . 1_655 106.27(9) ?
O8 Na2 O3 2_655 1_655 169.56(11) ?
O1 Na2 O3 . 1_655 89.14(9) ?
O2 Na2 O3 1_655 1_655 65.46(8) ?
O8 Na2 O6 2_655 2_765 80.99(10) ?
O1 Na2 O6 . 2_765 164.46(9) ?
O2 Na2 O6 1_655 2_765 88.01(9) ?
O3 Na2 O6 1_655 2_765 91.40(9) ?
O8 Na2 O6 2_655 . 89.56(9) ?
O1 Na2 O6 . . 73.19(8) ?
O2 Na2 O6 1_655 . 163.23(10) ?
O3 Na2 O6 1_655 . 97.81(9) ?
O6 Na2 O6 2_765 . 91.36(8) ?
O8 Na3 O9 1_565 . 90.37(10) ?
O8 Na3 O2 1_565 2_665 99.31(10) ?
O9 Na3 O2 . 2_665 109.28(11) ?
O8 Na3 O6 1_565 . 170.16(12) ?
O9 Na3 O6 . . 90.16(9) ?
O2 Na3 O6 2_665 . 89.78(9) ?
O8 Na3 O6 1_565 2_665 90.08(10) ?
O9 Na3 O6 . 2_665 176.70(11) ?
O2 Na3 O6 2_665 2_665 73.86(9) ?
O6 Na3 O6 . 2_665 88.84(9) ?
O8 Na3 O3 1_565 . 94.84(10) ?
O9 Na3 O3 . . 86.15(10) ?
O2 Na3 O3 2_665 . 158.84(10) ?
O6 Na3 O3 . . 75.39(8) ?
O6 Na3 O3 2_665 . 90.56(9) ?
O9 Na4 O7 . 2_666 110.87(11) ?
O9 Na4 O7 . 1_565 99.20(10) ?
O7 Na4 O7 2_666 1_565 93.10(10) ?
O9 Na4 O3 . . 88.29(10) ?
O7 Na4 O3 2_666 . 160.11(11) ?
O7 Na4 O3 1_565 . 88.85(9) ?
O9 Na4 O5 . 2_666 160.69(11) ?
O7 Na4 O5 2_666 2_666 71.66(9) ?
O7 Na4 O5 1_565 2_666 99.76(10) ?
O3 Na4 O5 . 2_666 88.50(9) ?
O9 Na4 O4 . . 82.73(9) ?
O7 Na4 O4 2_666 . 115.40(10) ?
O7 Na4 O4 1_565 . 148.90(10) ?
O3 Na4 O4 . . 60.09(8) ?
O5 Na4 O4 2_666 . 79.18(8) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Np1 O1 . 1.891(2) y
Np1 O2 . 1.888(2) y
Np1 O3 . 1.917(2) y
Np1 O4 . 1.880(2) y
Np1 O5 . 2.315(2) y
Np1 O6 . 2.362(2) y
Na1 O5 2_666 2.356(3) ?
Na1 O5 . 2.381(3) ?
Na1 O1 1_455 2.382(3) ?
Na1 O4 2_666 2.420(3) ?
Na1 O3 . 2.501(3) ?
Na1 O4 1_455 2.550(3) ?
Na2 O8 2_655 2.327(3) ?
Na2 O1 . 2.433(3) ?
Na2 O2 1_655 2.439(3) ?
Na2 O3 1_655 2.479(3) ?
Na2 O6 2_765 2.524(3) ?
Na2 O6 . 2.529(3) ?
Na3 O8 1_565 2.321(3) ?
Na3 O9 . 2.363(3) ?
Na3 O2 2_665 2.413(3) ?
Na3 O6 . 2.472(3) ?
Na3 O6 2_665 2.514(3) ?
Na3 O3 . 2.526(3) ?
Na4 O9 . 2.325(3) ?
Na4 O7 2_666 2.377(3) ?
Na4 O7 1_565 2.420(3) ?
Na4 O3 . 2.469(3) ?
Na4 O5 2_666 2.613(3) ?
Na4 O4 . 2.864(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O5 H5 O7 . 0.813(19) 2.14(2) 2.927(3) 162(5) y
O6 H6 O8 1_665 0.794(19) 2.49(3) 3.154(4) 142(4) y
O7 H7 O4 1_445 0.788(19) 2.31(3) 3.039(4) 154(5) y
O8 H8A O7 . 0.849(18) 1.755(19) 2.603(4) 178(4) y
O8 H8B O2 . 0.847(18) 2.03(2) 2.876(4) 175(5) y
O9 H9A O1 1_565 0.849(18) 1.937(19) 2.781(3) 173(5) y
O9 H9B O7 1_665 0.828(18) 1.87(2) 2.676(4) 165(5) y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
H5 O5 O6 H6 . . . . -149(4) ?
