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Volume 64 
Part 11 
Page i73  
November 2008  

Received 15 July 2008
Accepted 21 September 2008
Online 15 October 2008

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Key indicators
Single-crystal X-ray study
T = 120 K
Mean [sigma](S-O) = 0.002 Å
R = 0.017
wR = 0.042
Data-to-parameter ratio = 14.4
Details
Open access

catena-Poly[tetrasodium [[cis-dioxido-trans-bis(sulfato-[kappa]O)molybdate(VI)]-[mu]-sulfato-[kappa]2O:O']]

Susan J. Cline Schäffera* and Rolf W. Bergb

aTårnby Gymnasium & HF, Tejn Allé 5, DK-2770 Kastrup, Denmark, and bThe Technical University of Denmark, The Department of Chemistry, Building 207, DK-2800 Lyngby, Denmark
Correspondence e-mail: su@tgy.dk

Single crystals of the title compound, {Na4[MoVIO2(SO4)3]}n, were grown from a melt of MoO3 and Na2SO4 in Na2S2O7. In contrast to the structure of the isoformular K compound, K4[MoVIO2(SO4)3], with its monomeric anion, this sodium analogue contains a polymeric anion of the type {[MoVIO2(SO4)2-[mu]-(SO4)]4-}n. The MoVI cations, surrounded by two tightly bonded O atoms and four O atoms of one bridging and two terminal sulfato ligands, form zigzag chains parallel to [100]. All four Na+ cations are situated between the anionic chains and have distorted octahedral coordination spheres.

Related literature

The structure of the title isoformular potassium compound, K4[MoVIO2(SO4)3], was determined by Schäffer & Berg (2008[Schäffer, S. J. C. & Berg, R. W. (2008). Acta Cryst. E64, i20.]). For related Mo-containing compounds, see Salles et al. (1996[Salles, L., Robert, F., Semmer, V., Jeannin, Y. & Bregeault, J. (1996). Bull. Soc. Chim. Fr. 133, 319-328.]) and Nørbygaard et al. (1998[Nørbygaard, T., Berg, R. W. & Nielsen, K. (1998). Molten Salts XI, Proceedings of the Electrochemical Society 98-11, pp. 553-565. Pennington, NJ: Electrochemical Society.]). Related compounds with Mo replaced by W were discussed by Schäffer & Berg (2005[Schäffer, S. J. C. & Berg, R. W. (2005). Acta Cryst. E61, i49-i51.]) and Berg et al. (2006[Berg, R. W., Ferré, I. M. & Schäffer, S. J. C. (2006). Vib. Spectrosc. 42, 346-352.]). Other sulfato complexes coordinated to late transition metal centers were reported by Berg & Thorup (2005[Berg, R. W. & Thorup, N. (2005). Inorg. Chem. 44, 3485-3493.]), Borup et al. (1990[Borup, F., Berg, R. W. & Nielsen, K. (1990). Acta Chem. Scand. 44, 328-331.]), Nielsen et al. (1993[Nielsen, K., Fehrmann, R. & Eriksen, K. M. (1993). Inorg. Chem. 32, 4825-4828.]) and Rasmussen et al. (2003[Rasmussen, S. B., Rasmussen, R. M., Fehrmann, R. & Nielsen, K. (2003). Inorg. Chem. 42, 7123-7128.]).

[Scheme 1]

Experimental

Crystal data

  • Na4[MoO2(SO4)3]

  • Mr = 508.08

  • Orthorhombic, P 21 21 21

  • a = 8.4739 (6) Å

  • b = 9.2892 (7) Å

  • c = 15.1046 (11) Å

  • V = 1188.97 (15) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.85 mm-1

  • T = 120 (2) K

  • 0.24 × 0.18 × 0.02 mm
Data collection

  • Bruker SMART APEX CCD diffractometer

  • Absorption correction: gaussian (SHELXTL; Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) Tmin = 0.665, Tmax = 0.964

  • 14125 measured reflections

  • 2861 independent reflections

  • 2817 reflections with I > 2[sigma](I)

  • Rint = 0.031
Refinement

  • R[F2 > 2[sigma](F2)] = 0.017

  • wR(F2) = 0.042

  • S = 1.10

  • 2861 reflections

  • 199 parameters

  • [Delta][rho]max = 0.51 e Å-3

  • [Delta][rho]min = -0.26 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 1205 Friedel pairs

  • Flack parameter: 0.01 (2)

Table 1
Selected bond lengths (Å)

Mo1-O2 1.6905 (16)
Mo1-O1 1.7108 (16)
Mo1-O5 1.9925 (16)
Mo1-O4 2.0102 (16)
Mo1-O6i 2.1661 (15)
Mo1-O3 2.1907 (15)
Symmetry code: (i) [x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+1].

Data collection: SMART (Bruker, 2002[Bruker (2002). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2002[Bruker (2002). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2186 ).

Acknowledgements

The authors thank Astrid Schøneberg and Bodil Holten for their help and advice.

References

Berg, R. W., Ferré, I. M. & Schäffer, S. J. C. (2006). Vib. Spectrosc. 42, 346-352.  [CrossRef] [ChemPort]
Berg, R. W. & Thorup, N. (2005). Inorg. Chem. 44, 3485-3493.  [CrossRef] [PubMed] [ChemPort]
Borup, F., Berg, R. W. & Nielsen, K. (1990). Acta Chem. Scand. 44, 328-331.  [CrossRef] [ChemPort]
Bruker (2002). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Nielsen, K., Fehrmann, R. & Eriksen, K. M. (1993). Inorg. Chem. 32, 4825-4828.  [CrossRef] [ChemPort]
Nørbygaard, T., Berg, R. W. & Nielsen, K. (1998). Molten Salts XI, Proceedings of the Electrochemical Society 98-11, pp. 553-565. Pennington, NJ: Electrochemical Society.
Rasmussen, S. B., Rasmussen, R. M., Fehrmann, R. & Nielsen, K. (2003). Inorg. Chem. 42, 7123-7128.  [CrossRef] [PubMed] [ChemPort]
Salles, L., Robert, F., Semmer, V., Jeannin, Y. & Bregeault, J. (1996). Bull. Soc. Chim. Fr. 133, 319-328.  [ChemPort]
Schäffer, S. J. C. & Berg, R. W. (2005). Acta Cryst. E61, i49-i51.  [CrossRef] [details]
Schäffer, S. J. C. & Berg, R. W. (2008). Acta Cryst. E64, i20.  [CrossRef] [details]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]

Acta Cryst (2008). E64, i73  [ doi:10.1107/S1600536808030328 ]

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