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Volume 68 
Part 7 
Pages m938-m939  
July 2012  

Received 10 May 2012
Accepted 7 June 2012
Online 16 June 2012

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Key indicators
Single-crystal X-ray study
T = 223 K
Mean [sigma](S-C) = 0.015 Å
Disorder in main residue
R = 0.060
wR = 0.159
Data-to-parameter ratio = 18.9
Details
Open access

Octakis(dimethyl sulfoxide-[kappa]O)cerium(III) [mu]6-oxido-dodeca-[mu]2-oxido-hexaoxidohexamolybdate(VI) dimethyl sulfoxide tetrasolvate

Arbia Ben Khélifa,a Michel Giorgib and Mohamed Salah Belkhiriaa*

aLaboratoire de Physico-Chimie des Matériaux, Université de Monastir, Faculté des Sciences de Monastir, Tunisia, and bSpectropole, Université d 'Aix-Marseille, Faculté des Science St-Jérôme, Avenue Escadrille Normandie-Niemen, 13397 Marseille cedex 20, France
Correspondence e-mail: salah_belkiria@yahoo.com

The title complex, [Ce(C2H6OS)8]2[Mo6O19]3·4C2H6OS, was obtained as a byproduct of the reaction of [(C4H9)4N]2[Mo6O19] with Ce(NO3)3·6H2O and phthalic acid in dimethylsulfoxide solution. The asymmetric unit consists of a complex [Ce(C2H6OS)8]3+ cation, one and a half of the Lindqvist-type [Mo6O19]2- polyanions and two dimethylsulfoxide solvent molecules; the half polyanion lies on an inversion center. The Ce3+ ion is coordinated by eight dimethylsulfoxide ligands through the O atoms in the form of a distorted square antiprism. The Ce-O bond lengths range from 2.429 (6) to 2.550 (5) Å. The cohesion of the structure is ensured by S...O [3.115 (6), 3.242 (10) and 3.12 (3) Å], O...O [3.037 (10) Å] and C-H...O interactions between cations and anions. The S and C atoms of a dmso ligand are disordered over three sites in a 0.45:0.30:0.25 ratio. The dimethylsulfoxide solvent molecules are highly disordered and could not be modelled successfully; their contribution was therefore removed from the refinement using the SQUEEZE routine in PLATON [Spek (2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]). Acta Cryst. D65, 148-155]. Potential solvent-accessible voids of 500.0 Å3 occur in the crystal structure.

Related literature

For general background, physical properties and applications of polyoxidometalates, see: Dolbecq et al. (2010[Dolbecq, A., Dumas, E., Mayer, C. R. & Mialane, P. (2010). Chem. Rev. 110, 6009-6048.]). For the synthesis of [(C4H9)4N]2[Mo6O19], see: Hur et al. (1990[Hur, N. H., Klemperer, W. G. & Wang, R.-C. (1990). Inorg. Synth. 27, 77-78.]). For related structures, see: Wang et al. (2003[Wang, X., Guo, Y., Li, Y., Wang, E., Hu, C. & Hu, N. (2003). Inorg. Chem. 42, 4135-4140.]); Koo & Lee (2006[Koo, B. & Lee, U. (2006). Inorg. Chim. Acta. 359, 2067-2071.]); Qiu et al. (2006[Qiu, Y., Xu, L., Gao, G., Wang, W. & Li, F. (2006). Inorg. Chim. Acta. 359, 451-458.]). For crystallographic analysis, see: Spek (2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]).

[Scheme 1]

Experimental

Crystal data

  • [Ce(C2H6OS)8]2[Mo6O19]3·4C2H6OS

  • Mr = 4481.72

  • Triclinic, [P \overline 1]

  • a = 13.4590 (2) Å

  • b = 15.4688 (3) Å

  • c = 17.6599 (4) Å

  • [alpha] = 90.281 (1)°

  • [beta] = 98.468 (1)°

  • [gamma] = 115.580 (1)°

  • V = 3270.48 (11) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 2.75 mm-1

  • T = 223 K

  • 0.20 × 0.16 × 0.08 mm
Data collection

  • Bruker-Nonius KappaCCD diffractometer

  • Absorption correction: multi-scan (SORTAV; Blessing, 1995[Blessing, R. H. (1995). Acta Cryst. A51, 33-38.]) Tmin = 0.691, Tmax = 0.739

  • 69065 measured reflections

  • 12827 independent reflections

  • 10059 reflections with I > 2[sigma](I)

  • Rint = 0.063
Refinement

  • R[F2 > 2[sigma](F2)] = 0.060

  • wR(F2) = 0.159

  • S = 1.04

  • 12827 reflections

  • 680 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 2.47 e Å-3

  • [Delta][rho]min = -1.81 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C2-H2B...O13i 0.96 2.32 3.030 (14) 130
C6-H6B...O2ii 0.96 2.41 3.291 (18) 153
C11-H11A...O10 0.96 2.50 3.437 (15) 166
C14-H14A...O5iii 0.96 2.46 3.386 (19) 163
C14-H14B...O20iv 0.96 2.36 3.255 (17) 154
C16-H16C...O14iii 0.96 2.53 3.420 (17) 154
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) x-1, y-1, z; (iii) x, y-1, z; (iv) -x+1, -y+1, -z.

Data collection: COLLECT (Nonius, 2002[Nonius (2002). COLLECT. Nonius BV, Delft, The Netherlands.]); cell refinement: HKL-DENZO/SCALEPACK (Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, part A, edited by C.W. Carter Jr. & R. M. Sweet, pp. 307-326. New York: Academic Press.]); data reduction: HKL-DENZO/SCALEPACK; program(s) used to solve structure: SIR2004 (Burla et al., 2005[Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381-388.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 (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: PV2546 ).

Acknowledgements

The authors gratefully acknowledge financial support from the Ministry of Higher Education and Scientific Research of Tunisia.

References

Blessing, R. H. (1995). Acta Cryst. A51, 33-38.  [CrossRef] [details]
Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381-388.  [ISI] [CrossRef] [ChemPort] [details]
Dolbecq, A., Dumas, E., Mayer, C. R. & Mialane, P. (2010). Chem. Rev. 110, 6009-6048.  [ISI] [CrossRef] [ChemPort] [PubMed]
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  [CrossRef] [details]
Hur, N. H., Klemperer, W. G. & Wang, R.-C. (1990). Inorg. Synth. 27, 77-78.
Koo, B. & Lee, U. (2006). Inorg. Chim. Acta. 359, 2067-2071.  [ISI] [CrossRef] [ChemPort]
Nonius (2002). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, part A, edited by C.W. Carter Jr. & R. M. Sweet, pp. 307-326. New York: Academic Press.
Qiu, Y., Xu, L., Gao, G., Wang, W. & Li, F. (2006). Inorg. Chim. Acta. 359, 451-458.  [ISI] [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Spek, A. L. (2009). Acta Cryst. D65, 148-155.  [ISI] [CrossRef] [details]
Wang, X., Guo, Y., Li, Y., Wang, E., Hu, C. & Hu, N. (2003). Inorg. Chem. 42, 4135-4140.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]

Acta Cryst (2012). E68, m938-m939   [ doi:10.1107/S1600536812025949 ]

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