Bis[1,1′-(1,3-phenyl­enedimethyl­ene)di(1H-imidazol-3-ium)] β-octa­molybdate

Wang, X.-D.; Hou, G.-F.; Yu, Y.-H.; Gao, J.-S.

doi:10.1107/S1600536811053050

Volume 68
Part 1
Page m50
January 2012

Received 24 November 2011
Accepted 9 December 2011
Online 14 December 2011

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.006 Å
R = 0.026
wR = 0.057
Data-to-parameter ratio = 16.2
Details

Bis[1,1'-(1,3-phenylenedimethylene)di(1H-imidazol-3-ium)] -octamolybdate

Xiao-Dan Wang,^a Guang-Feng Hou,^a Ying-Hui Yu ^a and Jin-Sheng Gao ^a ^*

^aEngineering Research Center of Pesticides of Heilongjiang University, Heilongjiang University, Harbin 150050, People's Republic of China, and College of Chemistry and Materials Science, Heilongjiang University, Harbin 150080, People's Republic of China
Correspondence e-mail: hgf1000@163.com

In the title compound, (C₁₄H₁₆N₄)₂[Mo₈O₂₆], the [beta] -octamolybdate anion is centrosymmetric. N-HO hydrogen bonds link the diimidazolium cations and the polyoxidoanions into a chain structure along [100]. [pi] - [pi] interactions between the imidazole rings and between the imidazole and benzene rings [centroid-centroid distances = 3.611 (2) and 3.689 (3) Å, respectively] connect the chains.

Related literature

For general background to polyoxidometalate-based organic-inorganic hybrid compounds, see: Xie et al. (2011); Xu et al. (1999). For the synthesis of the ligand, see: Yang et al. (2006).

Experimental

Crystal data

(C₁₄H₁₆N₄)₂[Mo₈O₂₆]
M_r = 1664.14
Monoclinic, P 2₁ /c
a = 12.163 (2) Å
b = 12.785 (3) Å
c = 14.937 (3) Å
= 96.82 (3)°
V = 2306.3 (8) Å³
Z = 2
Mo K radiation
= 2.20 mm^-1
T = 293 K
0.12 × 0.10 × 0.10 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) T_min = 0.780, T_max = 0.809
21595 measured reflections
5261 independent reflections
4579 reflections with I > 2(I)
R_int = 0.032

Refinement

R[F² > 2(F²)] = 0.026
wR(F²) = 0.057
S = 1.01
5261 reflections
324 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 1.12 e Å^-3
_min = -1.30 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N2-H21O12ⁱ	0.90 (1)	1.96 (2)	2.844 (4)	168 (4)
N4-H41O5ⁱⁱ	0.90 (1)	2.51 (5)	3.003 (5)	115 (4)
N4-H41O8ⁱⁱ	0.90 (1)	2.23 (4)	2.909 (5)	132 (5)
Symmetry codes: (i) -x+1, -y+1, -z+2; (ii) x+1, y-1, z.

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); 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: HY2492 ).

Acknowledgements

The authors thank the Project of Innovation Service Platform of Heilongjiang Province (PG09J001) and Heilongjiang University for supporting this work.

References

Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.
Rigaku/MSC (2002). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Xie, Y.-M., Yu, R.-M., Wu, X.-Y., Wang, F., Zhang, J. & Lu, C.-Z. (2011). Cryst. Growth Des. 11, 4739-4741.
Xu, Q., Wang, R.-Z., Yang, G.-Y., Xing, Y.-H., Li, D.-M., Bu, W.-M., Ye, L., Fan, Y.-G., Yang, G.-D., Xong, Y., Lin, Y.-H. & Jia, H.-Q. (1999). Chem. Commun. pp. 983-984.
Yang, J., Ma, J.-F., Liu, Y.-Y., Ma, J.-C., Jia, H.-Q. & Hu, N.-H. (2006). Eur. J. Inorg. Chem. pp. 1208-1215.

metal-organic compounds