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

Oba, A.; Hashimoto, M.

doi:10.1107/S1600536812045850

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 (C-C) = 0.003 Å
R = 0.029
wR = 0.080
Data-to-parameter ratio = 22.3
Details

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

Ayaka Oba ^a and Masato Hashimoto ^a ^*

^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). For the structures of related molybdate complexes, see Stomberg & Olson (1985); Bayot et al. (2004).

Experimental

Crystal data

(C₉H₁₄N)₂[Mo₂(C₂O₄)(O₂)₄O₂]
M_r = 712.32
Monoclinic, P 2₁ /n
a = 9.860 (2) Å
b = 9.975 (2) Å
c = 13.691 (3) Å
= 94.023 (3)°
V = 1343.2 (5) Å³
Z = 2
Mo K radiation
= 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) T_min = 0.888, T_max = 0.914
11791 measured reflections
3843 independent reflections
3621 reflections with I > 2(I)
R_int = 0.021

Refinement

R[F² > 2(F²)] = 0.029
wR(F²) = 0.080
S = 1.06
3843 reflections
172 parameters
H-atom parameters not refined
_max = 1.84 e Å^-3
_min = -0.69 e Å^-3

Data collection: CrystalClear SM (Rigaku, 2008); cell refinement: CrystalClear SM; data reduction: CrystalClear SM; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); 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.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Hashimoto, M., Ozeki, T., Ichida, H., Sasaki, Y., Matsumoto, K. & Kudo, T. (1987). Chem. Lett. pp. 1873-1876.
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.
Stomberg, R. & Olson, S. (1985). Acta Chem. Scand. Ser. A, 39, 79-83.

metal-organic compounds