Hexakis(dimethyl­ammonium) di-μ6-oxido-tetra-μ3-oxido-tetra­deca-μ2-oxido-octa­oxidodeca­vanadate(V) monohydrate

Wang, S.; Lu, L.; Feng, S.; Zhu, M.

doi:10.1107/S1600536810016442

Volume 66
Part 6
Page m632
June 2010

Received 27 April 2010
Accepted 5 May 2010
Online 8 May 2010

Key indicators
Single-crystal X-ray study
T = 203 K
Mean (N-C) = 0.022 Å
R = 0.096
wR = 0.177
Data-to-parameter ratio = 11.7
Details

Hexakis(dimethylammonium) di-₆-oxido-tetra-₃-oxido-tetradeca-₂-oxido-octaoxidodecavanadate(V) monohydrate

Sulian Wang,^a Liping Lu,^a ^* Sisi Feng ^a and Miaoli Zhu ^a ^*

^aInstitute of Molecular Science, Key Laboratory of Chemical Biology and Molecular Engineering of the Education Ministry, Shanxi University, Taiyuan, Shanxi 030006, People's Republic of China
Correspondence e-mail: luliping@sxu.edu.cn, miaoli@sxu.edu.cn

In the title compound, (C₂H₈N)₆[V₁₀O₂₈]·H₂O, the [V₁₀O₂₈]^6- polymetalate anion has crystallographic mirror symmetry with six V atoms and 12 O atoms lying on the mirror plane. Each of the V^V atoms adopts a distorted octahedral geometry. Eight terminal O atoms are bonded to V^V atoms with double bonds and the others act as bridging atoms. In the crystal structure, a network of N-HO and O-HO hydrogen bonds helps to establish the packing.

Related literature

For the biological activity of oxovanadates and vanadium complexes, see: Pacigová et al. (2007); Yuan, Lu, Gao et al. (2009). For a related structure, see: Yuan, Lu, Zhu et al. (2009).

Experimental

Crystal data

(C₂H₈N)₆[V₁₀O₂₈]·H₂O
M_r = 1251.98
Orthorhombic, C m c a
a = 13.6149 (18) Å
b = 18.629 (3) Å
c = 30.235 (2) Å
V = 7668.5 (16) Å³
Z = 8
Mo K radiation
= 2.42 mm^-1
T = 203 K
0.35 × 0.11 × 0.05 mm

Data collection

Bruker SMART 1K CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T_min = 0.484, T_max = 0.888
18064 measured reflections
3464 independent reflections
2951 reflections with I > 2(I)
R_int = 0.078

Refinement

R[F² > 2(F²)] = 0.096
wR(F²) = 0.177
S = 1.26
3464 reflections
296 parameters
6 restraints
H-atom parameters constrained
_max = 1.70 e Å^-3
_min = -0.83 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O21-H21BO10ⁱ	0.85	2.30	2.950 (19)	133
O21-H21AO16	0.85	2.26	3.101 (18)	171
N4-H4DO5ⁱⁱ	0.91	1.77	2.673 (8)	170
N4-H4EO5	0.91	1.77	2.673 (8)	170
N2-H2DO6	0.91	1.88	2.759 (10)	162
N2-H2EO6ⁱⁱⁱ	0.91	2.22	2.986 (10)	141
N2-H2EO7ⁱⁱⁱ	0.91	2.05	2.812 (9)	140
N1-H1AO8^iv	0.91	1.86	2.732 (10)	161
N1-H1BO3	0.91	1.79	2.674 (10)	164
Symmetry codes: (i) $[x, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (ii) $[-x+{\script{3\over 2}}, y, -z+{\script{3\over 2}}]$ ; (iii) $[-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, -z+2]$ ; (iv) $[-x+{\script{3\over 2}}, y+{\script{1\over 2}}, z]$ .

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2304 ).

Acknowledgements

MZ acknowledges the National Natural Science Foundation of China (No. 20471033) and the Natural Science Foundation of Shanxi Province (No. 2010011011-2), LL thanks the Overseas Returned Scholar Foundation of Shanxi Province in 2008 and SF thanks the Natural Science Foundation for Young Scientists of Shanxi Province (No. 2010021010-1) and the Doctoral Startup Foundation of Shanxi University for financial support.

References

Bruker (2007). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Pacigová, S., Rakovský, E., Sivák, M. & Zák, Z. (2007). Acta Cryst. C63, m419-m422.
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Yuan, C.-X., Lu, L.-P., Gao, X.-L., Wu, Y.-B., Guo, M.-L., Li, Y., Fu, X.-Q. & Zhu, M.-L. (2009). J. Biol. Inorg. Chem. 14, 841-851.
Yuan, C., Lu, L., Zhu, M., Ma, Q. & Wu, Y. (2009). Acta Cryst. E65, m267-m268.