[Journal logo]

Volume 69 
Part 12 
Pages m661-m662  
December 2013  

Received 11 October 2013
Accepted 8 November 2013
Online 16 November 2013

Key indicators
Single-crystal X-ray study
T = 298 K
Mean [sigma](C-C) = 0.014 Å
Disorder in main residue
R = 0.069
wR = 0.192
Data-to-parameter ratio = 31.8
Details
Open access

Bis(4-amino­pyridinium) [mu]6-oxido-dodeca-[mu]2-oxido-hexaoxido[rhenium(VII)tetratungsten(VI)vanadium(V)]ate hepta­hydrate

aLaboratoire de Chimie des Matériaux, Faculté des Sciences de Bizerte, 7021 Zarzouna Bizerte, Tunisia
Correspondence e-mail: samah.akriche@fsb.rnu.tn

In the title organic-inorganic hybrid compound, (C5H7N2)2[ReVW4O19]·7H2O, the Lindqvist-type polyoxido anion has crystallographically imposed mm2 symmetry and is built up by six MO6 (M = W, V, Re) edge-sharing distorted octa­hedra. The Re and V atoms share the same crystallographic site in a 0.5:0.5 ratio. The 4-amino­pyridinium cations lie on a mirror plane. Three of the four independent water O atoms in the asymmetric unit are located on a mirror plane whereas the remaining O atom has mm2 site symmetry. In the crystal, the cations, anions and water mol­ecules are linked into a three-dimensional network through O-H...O and N-H...O hydrogen-bonding inter­actions.

Related literature

For applications of polyoxidometalates, see: Pope & Müller (1991[Pope, M. T. & Müller, A. (1991). Angew. Chem. Int. Ed. 30, 34-38.], 1994[Pope, M. T. & Müller, A. (1994). Polyoxometalates: from platonic solids to anti-retroviral activity. Dordrecht: Kluwer Academic Publishers.]). For bond-valence calculations, see: Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]). For related structures, see: Lindqvist (1953[Lindqvist, I. (1953). Ark. Kemi 5, 247-250.]); Bannani et al. (2007[Bannani, F., Driss, H., Thouvenot, R. & Debbabi, M. (2007). J. Chem. Crystallogr. 37, 37-48.]); Besecker et al. (1982[Besecker, C. J., Klemperer, W. G. & Day, V. W. (1982). J. Am. Chem. Soc. 104, 6158-6159.]); Wang et al. (2011[Wang, C., Weng, L., Ren, Y., Du, C., Yue, B., Gu, M. & He, H. (2011). Z. Anorg. Allg. Chem. 637, 472-477.]); Wang et al. (2006[Wang, X., Zhou, B., Zhong, C. & Ji, M. (2006). Cryst. Res. Technol. 41, 874-879.]); Meng et al. (2006[Meng, F. X., Liu, K. & Chen, Y. G. (2006). Chin. J. Struct. Chem. 25, 837-843.]). For NMR investigations of related compounds, see: Chen et al. (2004[Chen, Y. G., Gong, J. & Qu, L. Y. (2004). Coord. Chem. Rev. 248, 245-260.]); Domaille (1984[Domaille, P. J. (1984). J. Am. Chem. Soc. 106, 7677-7687.]); Fedotov & Maksimovskaya (2006[Fedotov, M. A. & Maksimovskaya, R. I. (2006). J. Struct. Chem. 47, 952-978.]); Leparulo-Loftus & Pope (1987[Leparulo-Loftus, M. A. & Pope, M. T. (1987). Inorg. Chem. 26, 2112-2120.]).

[Scheme 1]

Experimental

Crystal data
  • (C5H7N2)2[ReVW4O19]·7H2O

  • Mr = 1592.90

  • Orthorhombic, P m m a

  • a = 17.837 (2) Å

  • b = 9.163 (4) Å

  • c = 10.552 (3) Å

  • V = 1724.5 (9) Å3

  • Z = 2

  • Ag K[alpha] radiation

  • [lambda] = 0.56087 Å

  • [mu] = 9.22 mm-1

  • T = 298 K

  • 0.43 × 0.27 × 0.15 mm

Data collection
  • Enraf-Nonius CAD-4 diffractometer

  • Absorption correction: multi-scan (Blessing, 1995[Blessing, R. H. (1995). Acta Cryst. A51, 33-38.]) Tmin = 0.100, Tmax = 0.306

  • 6539 measured reflections

  • 4385 independent reflections

  • 2083 reflections with I > 2[sigma](I)

  • Rint = 0.052

  • 2 standard reflections every 120 min intensity decay: none

Refinement
  • R[F2 > 2[sigma](F2)] = 0.069

  • wR(F2) = 0.192

  • S = 1.03

  • 4385 reflections

  • 138 parameters

  • 17 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 2.94 e Å-3

  • [Delta][rho]min = -2.83 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H1A...O1W 0.86 2.40 3.078 (14) 136
N1-H1A...O1E 0.86 2.58 3.184 (14) 129
N2-H2A...O3i 0.86 2.39 3.181 (12) 152
O1W-H1W1...O1E 0.81 2.50 3.188 (18) 144
O2W-H1W2...O3Eii 0.85 2.10 2.836 (18) 144
O4W-H1W4...O2W 0.85 1.87 2.40 (7) 119
O4W-H2W4...O4Wiii 0.85 2.31 2.65 (15) 106
Symmetry codes: (i) [x+{\script{1\over 2}}, y, -z+1]; (ii) -x+1, -y, -z+1; (iii) -x+1, -y, -z+2.

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994[Enraf-Nonius (1994). CAD-4 EXPRESS. Enraf-Nonius, Delft, The Netherlands.]); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1996[Harms, K. & Wocadlo, S. (1996). XCAD4. University of Marburg, Germany.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]) and DIAMOND (Brandenburg & Putz, 2005[Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: RZ5088 ).


References

Bannani, F., Driss, H., Thouvenot, R. & Debbabi, M. (2007). J. Chem. Crystallogr. 37, 37-48.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Besecker, C. J., Klemperer, W. G. & Day, V. W. (1982). J. Am. Chem. Soc. 104, 6158-6159.  [CSD] [CrossRef] [ChemPort] [Web of Science]
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.  [CrossRef] [IUCr Journals]
Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.  [CrossRef] [Web of Science] [IUCr Journals]
Chen, Y. G., Gong, J. & Qu, L. Y. (2004). Coord. Chem. Rev. 248, 245-260.  [Web of Science] [CrossRef] [ChemPort]
Domaille, P. J. (1984). J. Am. Chem. Soc. 106, 7677-7687.  [CrossRef] [ChemPort] [Web of Science]
Enraf-Nonius (1994). CAD-4 EXPRESS. Enraf-Nonius, Delft, The Netherlands.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Fedotov, M. A. & Maksimovskaya, R. I. (2006). J. Struct. Chem. 47, 952-978.  [Web of Science] [CrossRef] [ChemPort]
Harms, K. & Wocadlo, S. (1996). XCAD4. University of Marburg, Germany.
Leparulo-Loftus, M. A. & Pope, M. T. (1987). Inorg. Chem. 26, 2112-2120.  [ChemPort]
Lindqvist, I. (1953). Ark. Kemi 5, 247-250.  [ChemPort]
Meng, F. X., Liu, K. & Chen, Y. G. (2006). Chin. J. Struct. Chem. 25, 837-843.  [ChemPort]
Pope, M. T. & Müller, A. (1991). Angew. Chem. Int. Ed. 30, 34-38.
Pope, M. T. & Müller, A. (1994). Polyoxometalates: from platonic solids to anti-retroviral activity. Dordrecht: Kluwer Academic Publishers.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Wang, C., Weng, L., Ren, Y., Du, C., Yue, B., Gu, M. & He, H. (2011). Z. Anorg. Allg. Chem. 637, 472-477.  [CSD] [CrossRef] [ChemPort]
Wang, X., Zhou, B., Zhong, C. & Ji, M. (2006). Cryst. Res. Technol. 41, 874-879.  [Web of Science] [CrossRef] [ChemPort]


Acta Cryst (2013). E69, m661-m662   [ doi:10.1107/S1600536813030687 ]

This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.