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Volume 64 
Part 1 
Page i6  
January 2008  

Received 11 December 2007
Accepted 14 December 2007
Online 21 December 2007


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Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](Np-O) = 0.001 Å
R = 0.010
wR = 0.021
Data-to-parameter ratio = 33.7
Details

Reinvestigation of trisodium dihydroxidotetraoxidoneptunate(VII) dihydrate

Mikhail S. Grigorieva* and Nikolai N. Krota

aA. N. Frumkin Institute of Physical Chemistry and Electrochemistry, Russian Academy of Sciences, 31 Leninsky prospekt, 119991 Moscow, Russian Federation
Correspondence e-mail: grigoriev@ipc.rssi.ru

The title compound, Na3[NpO4(OH)2]·2H2O, contains distorted tetragonal-bipyramidal centrosymmetric [NpO4(OH)2]3- complex anions. The Np-O distances are 1.8975 (7) and 1.8891 (7) Å in the NpO4 group and 2.3451 (7) Å to the OH group. Both Na atoms (one in a general position, the second in a special position on an inversion centre) have a distorted octahedral oxygen environment.

Related literature

The structure of Na3[NpO4(OH)2]·2H2O was investigated by photographic technique with visual estimation of reflection intensities by Tomilin et al. (1981a[Tomilin, S. V., Volkov, Yu. F., Kapshukov, I. I. & Rykov, A. G. (1981a). Radiokhimiya, 23, 710-715.]). Several other NpVII compounds containing [NpO4(OH)2]3- anions have been studied by photographic techniques, viz. Na3[NpO4(OH)2] (Tomilin et al., 1981b[Tomilin, S. V., Volkov, Yu. F., Kapshukov, I. I. & Rykov, A. G. (1981b). Radiokhimiya, 23, 704-709.]), Na3[NpO4(OH)2]·4H2O (Tomilin et al., 1981c[Tomilin, S. V., Volkov, Yu. F., Kapshukov, I. I. & Rykov, A. G. (1981c). Radiokhimiya, 23, 862-867.]), K3[NpO4(OH)2]·2H2O (Tomilin et al., 1983[Tomilin, S. V., Volkov, Yu. F., Visyashcheva, G. I. & Kapshukov, I. I. (1983). Radiokhimiya, 25, 58-62.]). Diffractometric structure determinations have been made for [Co(NH3)6][NpO4(OH)2]·2H2O (Grigor'ev et al., 1986[Grigor'ev, M. S., Gulev, B. F. & Krot, N. N. (1986). Radiokhimiya, 28, 690-694.]), Cs3[NpO4(OH)2]·3H2O (Grigor'ev et al., 1993[Grigor'ev, M. S., Baturin, N. A., Tananaev, I. G. & Krot, N. N. (1993). Radiokhimiya, 35, 12-16.]), K3[NpO4(OH)2]·2H2O (Charushnikova et al., 2007[Charushnikova, I. A., Krot, N. N., Starikova, Z. A. & Poliakova, I. N. (2007). Radiokhimiya, 49, 12-16.]) and Na3[NpO4(OH)2] (Grigoriev & Krot, 2007[Grigoriev, M. S. & Krot, N. N. (2007). Acta Cryst. E63, i176.]).[link]

[Scheme 1]

Experimental

Crystal data

  • Na3[NpO4(OH)2]·2H2O

  • Mr = 440.02

  • Monoclinic, P 21 /c

  • a = 7.8166 (3) Å

  • b = 7.7703 (2) Å

  • c = 6.8211 (2) Å

  • [beta] = 112.9139 (14)°

  • V = 381.60 (2) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 13.79 mm-1

  • T = 100 (2) K

  • 0.12 × 0.08 × 0.02 mm
Data collection

  • Bruker Kappa APEXII area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2004[Sheldrick, G. M. (2004). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.522, Tmax = 0.770

  • 16264 measured reflections

  • 2357 independent reflections

  • 1920 reflections with I > 2[sigma](I)

  • Rint = 0.024
Refinement

  • R[F2 > 2[sigma](F2)] = 0.010

  • wR(F2) = 0.021

  • S = 1.04

  • 2357 reflections

  • 70 parameters

  • 3 restraints

  • All H-atom parameters refined

  • [Delta][rho]max = 0.75 e Å-3

  • [Delta][rho]min = -0.88 e Å-3

Table 1
Selected geometric parameters (Å, °)

Np-O1 1.8975 (7)
Np-O2 1.8891 (7)
Np-O3 2.3451 (7)
O1-Np-O2 91.41 (3)
O1-Np-O3 90.82 (3)
O2-Np-O3 94.67 (3)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O3-H3...O1i 0.815 (15) 1.976 (16) 2.7866 (10) 173 (2)
O4-H4A...O3 0.856 (17) 1.799 (17) 2.6538 (12) 178 (2)
O4-H4B...O3ii 0.840 (16) 1.931 (16) 2.7612 (12) 169 (2)
Symmetry codes: (i) [x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]; (ii) -x+2, -y+1, -z+1.

Data collection: APEX2 (Bruker, 2006[Bruker (2006). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 1998[Bruker (1998). SMART (Version 5.059) and SAINT-Plus (Version 6.01). Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a[Sheldrick, G. M. (1997a). SHELXS97 and SHELXL97. University of Göttingen, Germany.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a[Sheldrick, G. M. (1997a). SHELXS97 and SHELXL97. University of Göttingen, Germany.]); molecular graphics: SHELXTL97 (Sheldrick, 1997b[Sheldrick, G. M. (1997b). SHELXTL. Version 5.10. Bruker AXS Inc., Madison, Wisconsin, USA.]); software used to prepare material for publication: SHELXTL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SG2217 ).

References

Bruker (1998). SMART (Version 5.059) and SAINT-Plus (Version 6.01). Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2006). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Charushnikova, I. A., Krot, N. N., Starikova, Z. A. & Poliakova, I. N. (2007). Radiokhimiya, 49, 12-16.
Grigor'ev, M. S., Baturin, N. A., Tananaev, I. G. & Krot, N. N. (1993). Radiokhimiya, 35, 12-16.
Grigor'ev, M. S., Gulev, B. F. & Krot, N. N. (1986). Radiokhimiya, 28, 690-694.  [ChemPort]
Grigoriev, M. S. & Krot, N. N. (2007). Acta Cryst. E63, i176.
Sheldrick, G. M. (1997a). SHELXS97 and SHELXL97. University of Göttingen, Germany.
Sheldrick, G. M. (1997b). SHELXTL. Version 5.10. Bruker AXS Inc., Madison, Wisconsin, USA.
Sheldrick, G. M. (2004). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Tomilin, S. V., Volkov, Yu. F., Kapshukov, I. I. & Rykov, A. G. (1981a). Radiokhimiya, 23, 710-715.
Tomilin, S. V., Volkov, Yu. F., Kapshukov, I. I. & Rykov, A. G. (1981b). Radiokhimiya, 23, 704-709.
Tomilin, S. V., Volkov, Yu. F., Kapshukov, I. I. & Rykov, A. G. (1981c). Radiokhimiya, 23, 862-867.  [ChemPort]
Tomilin, S. V., Volkov, Yu. F., Visyashcheva, G. I. & Kapshukov, I. I. (1983). Radiokhimiya, 25, 58-62.  [ChemPort]

Acta Cryst (2008). E64, i6  [ doi:10.1107/S1600536807066962 ]

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