#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/74/2017427.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_2017427
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 [Pu O4 (O H)2] (O H), 2H2 O'
_chemical_formula_moiety         '4(Na +), H2 Pu O6 3-, 2(H2 O), H O -'
_chemical_formula_sum            'H7 Na4 O9 Pu'
_chemical_formula_weight         482.02
_chemical_name_systematic
;
Tetrasodium dihydroxidotetraoxidoplutonate(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                 101.224(2)
_cell_angle_gamma                105.760(2)
_cell_formula_units_Z            2
_cell_length_a                   5.9177(2)
_cell_length_b                   8.0736(2)
_cell_length_c                   10.8696(3)
_cell_measurement_reflns_used    7446
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.00
_cell_measurement_theta_min      2.02
_cell_volume                     462.72(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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            31123
_diffrn_reflns_theta_full        40.00
_diffrn_reflns_theta_max         40.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.793
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Sheldrick, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.543
_refine_diff_density_min         -1.986
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.855
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         5736
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0281
_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)+(0.0086P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0368
_refine_ls_wR_factor_ref         0.0386
_reflns_number_gt                4796
_reflns_number_total             5736
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fa3208.cif
_cod_data_source_block           II
_cod_original_cell_volume        462.72(2)
_cod_database_code               2017427
_cod_database_fobs_code          2017427
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
Pu Pu1 0.636080(17) 0.414739(13) 0.247926(10) 0.00471(2) Uani d . 1 . .
Na Na1 0.21183(19) 0.46774(15) 0.41582(10) 0.0100(2) Uani d . 1 . .
Na Na2 1.05366(18) 0.34046(15) 0.07393(11) 0.0099(2) Uani d . 1 . .
Na Na3 0.52187(18) 0.71929(14) 0.09431(10) 0.0100(2) Uani d . 1 . .
Na Na4 0.61628(18) 0.85254(14) 0.42687(10) 0.0119(2) Uani d . 1 . .
O O1 0.8529(3) 0.2821(2) 0.24009(18) 0.0091(3) Uani d . 1 . .
O O2 0.3938(3) 0.2289(2) 0.10200(18) 0.0092(3) Uani d . 1 . .
O O3 0.4207(3) 0.5534(2) 0.25272(18) 0.0086(3) Uani d . 1 . .
O O4 0.8756(3) 0.6042(2) 0.39297(19) 0.0093(4) Uani d . 1 . .
O O5 0.4857(3) 0.3035(3) 0.40065(19) 0.0093(4) Uani d D 1 . .
H H5 0.449(5) 0.200(2) 0.386(3) 0.011 Uiso d D 1 . .
O O6 0.7897(3) 0.5351(3) 0.0951(2) 0.0080(4) Uani d D 1 . .
H H6 0.891(4) 0.620(3) 0.145(3) 0.010 Uiso d D 1 . .
O O7 0.2480(3) -0.0810(2) 0.36329(18) 0.0105(3) Uani d D 1 . .
H H7 0.174(5) -0.162(3) 0.376(3) 0.013 Uiso d D 1 . .
O O8 0.2410(4) -0.1325(3) 0.1161(2) 0.0124(4) Uani d D 1 . .
H H8A 0.229(5) -0.122(4) 0.193(2) 0.019 Uiso d D 1 . .
H H8B 0.290(5) -0.035(3) 0.109(3) 0.019 Uiso d D 1 . .
O O9 0.8122(3) 0.9519(2) 0.28120(18) 0.0121(3) Uani d D 1 . .
H H9A 0.832(5) 1.056(3) 0.275(3) 0.018 Uiso d D 1 . .
H H9B 0.962(3) 0.956(4) 0.308(3) 0.018 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'
Pu Pu -9.4100 4.3056 '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 Pu1 O2 . . 91.50(7) ?
O1 Pu1 O3 . . 178.24(8) ?
O1 Pu1 O4 . . 89.58(7) ?
O1 Pu1 O5 . . 93.39(7) ?
O1 Pu1 O6 . . 87.62(7) ?
O2 Pu1 O3 . . 88.68(7) ?
O2 Pu1 O4 . . 178.79(8) ?
O2 Pu1 O5 . . 93.42(7) ?
O2 Pu1 O6 . . 87.49(8) ?
O3 Pu1 O4 . . 90.23(7) ?
O3 Pu1 O5 . . 88.35(7) ?
O3 Pu1 O6 . . 90.63(7) ?
O4 Pu1 O5 . . 87.07(8) ?
O4 Pu1 O6 . . 92.01(7) ?
O5 Pu1 O6 . . 178.62(7) ?
O5 Na1 O5 2_666 . 88.49(7) ?
O5 Na1 O1 2_666 1_455 166.70(7) ?
O5 Na1 O1 . 1_455 104.81(7) ?
O5 Na1 O4 2_666 2_666 74.91(7) ?
O5 Na1 O4 . 2_666 93.27(7) ?
O1 Na1 O4 1_455 2_666 103.77(7) ?
O5 Na1 O3 2_666 . 93.69(7) ?
O5 Na1 O3 . . 74.79(6) ?
O1 Na1 O3 1_455 . 89.93(7) ?
O4 Na1 O3 2_666 . 163.89(7) ?
O5 Na1 O4 2_666 1_455 101.20(7) ?
O5 Na1 O4 . 1_455 170.09(8) ?
O1 Na1 O4 1_455 1_455 65.51(6) ?
O4 Na1 O4 2_666 1_455 91.29(7) ?
O3 Na1 O4 . 1_455 102.23(7) ?
O8 Na2 O2 2_655 1_655 106.36(7) ?
O8 Na2 O1 2_655 . 99.93(8) ?
O2 Na2 O1 1_655 . 106.13(7) ?
O8 Na2 O3 2_655 1_655 169.47(8) ?
O2 Na2 O3 1_655 1_655 65.82(6) ?
O1 Na2 O3 . 1_655 89.32(7) ?
O8 Na2 O6 2_655 . 89.68(7) ?
O2 Na2 O6 1_655 . 163.64(8) ?
O1 Na2 O6 . . 73.37(6) ?
O3 Na2 O6 1_655 . 97.86(7) ?
O8 Na2 O6 2_655 2_765 81.32(8) ?
O2 Na2 O6 1_655 2_765 87.78(7) ?
O1 Na2 O6 . 2_765 164.86(7) ?
O3 Na2 O6 1_655 2_765 91.08(7) ?
O6 Na2 O6 . 2_765 91.60(7) ?
O8 Na3 O9 1_565 . 90.06(7) ?
O8 Na3 O2 1_565 2_665 99.22(7) ?
O9 Na3 O2 . 2_665 108.73(7) ?
O8 Na3 O6 1_565 . 170.25(9) ?
O9 Na3 O6 . . 90.17(7) ?
O2 Na3 O6 2_665 . 89.94(7) ?
O8 Na3 O6 1_565 2_665 90.27(7) ?
O9 Na3 O6 . 2_665 177.04(8) ?
O2 Na3 O6 2_665 2_665 74.11(7) ?
O6 Na3 O6 . 2_665 89.02(7) ?
O8 Na3 O3 1_565 . 94.71(7) ?
O9 Na3 O3 . . 85.98(7) ?
O2 Na3 O3 2_665 . 159.59(7) ?
O6 Na3 O3 . . 75.58(6) ?
O6 Na3 O3 2_665 . 91.07(7) ?
O9 Na4 O7 . 2_666 110.84(8) ?
O9 Na4 O7 . 1_565 98.80(7) ?
O7 Na4 O7 2_666 1_565 92.77(7) ?
O9 Na4 O3 . . 87.94(7) ?
O7 Na4 O3 2_666 . 160.69(8) ?
O7 Na4 O3 1_565 . 88.57(7) ?
O9 Na4 O5 . 2_666 160.74(7) ?
O7 Na4 O5 2_666 2_666 72.19(7) ?
O7 Na4 O5 1_565 2_666 100.05(7) ?
O3 Na4 O5 . 2_666 88.61(7) ?
O9 Na4 O4 . . 82.43(6) ?
O7 Na4 O4 2_666 . 115.77(7) ?
O7 Na4 O4 1_565 . 149.16(7) ?
O3 Na4 O4 . . 60.61(6) ?
O5 Na4 O4 2_666 . 79.37(6) ?
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
Pu1 O1 . 1.8824(15) y
Pu1 O2 . 1.8805(18) y
Pu1 O3 . 1.9109(15) y
Pu1 O4 . 1.8811(19) y
Pu1 O5 . 2.2952(19) y
Pu1 O6 . 2.339(2) y
Na1 O5 2_666 2.345(2) ?
Na1 O5 . 2.360(2) ?
Na1 O1 1_455 2.370(2) ?
Na1 O4 2_666 2.410(2) ?
Na1 O3 . 2.484(2) ?
Na1 O4 1_455 2.5247(19) ?
Na2 O8 2_655 2.310(2) ?
Na2 O2 1_655 2.4174(18) ?
Na2 O1 . 2.422(2) ?
Na2 O3 1_655 2.459(2) ?
Na2 O6 . 2.5002(19) ?
Na2 O6 2_765 2.522(2) ?
Na3 O8 1_565 2.310(2) ?
Na3 O9 . 2.349(2) ?
Na3 O2 2_665 2.396(2) ?
Na3 O6 . 2.4501(19) ?
Na3 O6 2_665 2.477(2) ?
Na3 O3 . 2.505(2) ?
Na4 O9 . 2.316(2) ?
Na4 O7 2_666 2.357(2) ?
Na4 O7 1_565 2.3992(19) ?
Na4 O3 . 2.453(2) ?
Na4 O5 2_666 2.592(2) ?
Na4 O4 . 2.8319(19) ?
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 . 0.770(16) 2.177(18) 2.921(3) 163(3) y
O6 H6 O8 1_665 0.760(17) 2.59(3) 3.152(3) 132(3) y
O7 H7 O4 1_445 0.745(17) 2.281(18) 3.013(2) 167(3) y
O8 H8A O7 . 0.836(16) 1.770(17) 2.600(3) 172(3) y
O8 H8B O2 . 0.793(16) 2.076(17) 2.865(3) 174(3) y
O9 H9A O1 1_565 0.836(16) 1.938(16) 2.770(2) 174(3) y
O9 H9B O7 1_665 0.866(16) 1.812(16) 2.667(2) 169(3) 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 . . . . -139(3) ?
