[Journal logo]

Volume 68 
Part 12 
Page m1467  
December 2012  

Received 29 October 2012
Accepted 6 November 2012
Online 10 November 2012

Key indicators
Single-crystal X-ray study
T = 93 K
Mean [sigma](C-C) = 0.003 Å
R = 0.029
wR = 0.080
Data-to-parameter ratio = 22.3
Details
Open access

Bis(trimethylphenylammonium) [mu]-oxalato-bis[oxidodiperoxidomolybdate(VI)]

aDepartment of Material Science and Chemistry, Faculty of Systems Engineering, Wakayama University, Sakaedani 930, Wakayama 640-8510, Japan
Correspondence e-mail: mh1043@center.wakayama-u.ac.jp

A trimethylphenylammonium salt of a dinuclear [mu]-oxalate complex of diperoxidomonomolybdate units, (C9H14N)2[Mo2(C2O4)(O2)4O2], was obtained from an acidic aqueous solution; the dianion is located about a centre of inversion. Each Mo atom bears two peroxide groups together with one O atom from the oxalate group in its equatorial positions and one terminal O atom as well as another O atom from the oxalate in axial positions. The oxalate group acts as a tetradentate bridging ligand and bridges between the diperoxidomolybdate units.

Related literature

For the structure of the closely related tetrabutylammonium peroxidotungstate analogue, see Hashimoto et al. (1987[Hashimoto, M., Ozeki, T., Ichida, H., Sasaki, Y., Matsumoto, K. & Kudo, T. (1987). Chem. Lett. pp. 1873-1876.]). For the structures of related molybdate complexes, see Stomberg & Olson (1985[Stomberg, R. & Olson, S. (1985). Acta Chem. Scand. Ser. A, 39, 79-83.]); Bayot et al. (2004[Bayot, D., Tinant, B. & Devilers, M. (2004). Inorg. Chim. Acta, 357, 809-816.]).

[Scheme 1]

Experimental

Crystal data
  • (C9H14N)2[Mo2(C2O4)(O2)4O2]

  • Mr = 712.32

  • Monoclinic, P 21 /n

  • a = 9.860 (2) Å

  • b = 9.975 (2) Å

  • c = 13.691 (3) Å

  • [beta] = 94.023 (3)°

  • V = 1343.2 (5) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 1.00 mm-1

  • T = 93 K

  • 0.20 × 0.17 × 0.17 mm

Data collection
  • Rigaku Saturn724+ diffractometer

  • Absorption correction: numerical (NUMABS; Higashi, 2000[Higashi, T. (2000). NUMABS. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.888, Tmax = 0.914

  • 11791 measured reflections

  • 3843 independent reflections

  • 3621 reflections with I > 2[sigma](I)

  • Rint = 0.021

Refinement
  • R[F2 > 2[sigma](F2)] = 0.029

  • wR(F2) = 0.080

  • S = 1.06

  • 3843 reflections

  • 172 parameters

  • H-atom parameters not refined

  • [Delta][rho]max = 1.84 e Å-3

  • [Delta][rho]min = -0.69 e Å-3

Data collection: CrystalClear SM (Rigaku, 2008[Rigaku (2008). CrystalClear SM. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear SM; data reduction: CrystalClear SM; 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, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: SHELXL97.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IM2410 ).


Acknowledgements

Part of the work was supported financially by Grant in Aid No. 19550065 distributed by the Japan Society for the Promotion of Science (JSPS).

References

Bayot, D., Tinant, B. & Devilers, M. (2004). Inorg. Chim. Acta, 357, 809-816.  [ISI] [CSD] [CrossRef] [ChemPort]
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  [CrossRef] [details]
Hashimoto, M., Ozeki, T., Ichida, H., Sasaki, Y., Matsumoto, K. & Kudo, T. (1987). Chem. Lett. pp. 1873-1876.  [CrossRef] [ISI]
Higashi, T. (2000). NUMABS. Rigaku Corporation, Tokyo, Japan.
Rigaku (2008). CrystalClear SM. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Stomberg, R. & Olson, S. (1985). Acta Chem. Scand. Ser. A, 39, 79-83.  [CrossRef]


Acta Cryst (2012). E68, m1467  [ doi:10.1107/S1600536812045850 ]

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.