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Volume 64 
Part 3 
Page i20  
March 2008  

Received 2 January 2008
Accepted 5 February 2008
Online 13 February 2008


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Key indicators
Single-crystal X-ray study
T = 120 K
Mean [sigma](Mo-O) = 0.002 Å
R = 0.017
wR = 0.042
Data-to-parameter ratio = 15.4
Details

Tetrapotassium cis-dioxido-trans-bis(sulfato-[kappa]O)sulfato([kappa]2O,O')molybdate(VI)

Susan J. Cline Schäffera+ and Rolf W. Berga*

aThe Technical University of Denmark, Department of Chemistry, Building 207, DK-2800 Lyngby, Denmark
Correspondence e-mail: su@tgy.dk

The title compound, K4[MoVIO2(SO4)3], was precipitated from a melt of molybdenum(VI) oxide and potassium sulfate in potassium disulfate. The compound contains monomeric [MoVIO2(SO4)3]4- anions, with the MoVI atom, both oxide ligands, and the S atom and both ligating O atoms of the bidentate sulfate group lying on a crystallographic mirror plane. One of the potassium cations is nine-coordinate, while the other is eight-coordinate.

Related literature

For related literature, see: Topsøe & Nielsen (1947[Topsøe, H. F. A. & Nielsen, A. (1947). Trans. Dan. Akad. Technol. Sci. 1, 18-24.]); 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.]); Nørbygaard et al. (1998[Nørbygaard, T., Berg, R. W. & Nielsen, K. (1998). Molten Salts XI Electrochem. Soc. Proc. 98-11, 553-565.]); Nielsen et al. (1993[Nielsen, K., Fehrmann, R. & Eriksen, K. M. (1993). Inorg. Chem. 32, 4825-4828.]); Rasmussen et al. (2003[Rasmussen, S. B., Rasmussen, R. M., Fehrmann, R. & Nielsen, K. (2003). Inorg. Chem. 42, 7123-7128.]); Salles et al. (1996[Salles, L., Robert, F., Semmer, V., Jeannin, Y. & Bregeault, J. (1996). Bull. Soc. Chim. Fr. 133, 319-328.]); Schäffer & Berg (2005[Schäffer, S. J. C. & Berg, R. W. (2005). Acta Cryst. E61, i49-i51.]); Tamasi & Cini (2003[Tamasi, G. & Cini, R. (2003). Dalton Trans. pp. 2928-2936.]).

[Scheme 1]

Experimental

Crystal data

  • K4[MoO2(SO4)3]

  • Mr = 572.52

  • Orthorhombic, P n m a

  • a = 7.5931 (5) Å

  • b = 17.1276 (11) Å

  • c = 10.5132 (7) Å

  • V = 1367.26 (16) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 2.71 mm-1

  • T = 120 (2) K

  • 0.28 × 0.18 × 0.07 mm
Data collection

  • Bruker SMART APEX CCD diffractometer

  • Absorption correction: Gaussian (XPREP; Bruker, 2002[Bruker (2002). SMART, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.512, Tmax = 0.684

  • 16179 measured reflections

  • 1693 independent reflections

  • 1681 reflections with I > 2[sigma](I)

  • Rint = 0.018
Refinement

  • R[F2 > 2[sigma](F2)] = 0.016

  • wR(F2) = 0.041

  • S = 1.11

  • 1693 reflections

  • 110 parameters

  • [Delta][rho]max = 0.59 e Å-3

  • [Delta][rho]min = -0.46 e Å-3

Table 1
Selected geometric parameters (Å, °)

Mo1-O1 1.6889 (18)
Mo1-O2 1.6883 (18)
Mo1-O3 2.2665 (17)
Mo1-O4 2.1837 (16)
Mo1-O6 2.0365 (12)
K1-O5i 2.6408 (12)
K1-O8ii 3.2305 (14)
K2-O8iii 2.7005 (14)
K2-O6iv 3.0239 (13)
O2-Mo1-O1 105.77 (10)
O2-Mo1-O6 98.04 (4)
O1-Mo1-O6 94.84 (4)
O6-Mo1-O6v 158.22 (7)
O2-Mo1-O4 155.71 (8)
O1-Mo1-O4 98.52 (8)
O6-Mo1-O4 79.65 (3)
O2-Mo1-O3 92.29 (8)
O1-Mo1-O3 161.94 (8)
O6-Mo1-O3 82.38 (3)
O4-Mo1-O3 63.43 (6)
Symmetry codes: (i) [x-{\script{1\over 2}}, y, -z-{\script{1\over 2}}]; (ii) [-x+{\script{1\over 2}}, -y, z-{\script{1\over 2}}]; (iii) [x+{\script{1\over 2}}, y, -z+{\script{1\over 2}}]; (iv) [x-{\script{1\over 2}}, y, -z+{\script{1\over 2}}]; (v) [x, -y+{\script{1\over 2}}, z].

Data collection: SMART (Bruker, 2002[Bruker (2002). SMART, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2002[Bruker (2002). SMART, SAINT and XPREP. 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: BI2277 ).

Acknowledgements

The authors thank Astrid Schønberg and Bodil Holten for help and advice.

References

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.  [ChemPort]
Bruker (2002). SMART, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.
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 Electrochem. Soc. Proc. 98-11, 553-565.
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]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Tamasi, G. & Cini, R. (2003). Dalton Trans. pp. 2928-2936.  [CrossRef]
Topsøe, H. F. A. & Nielsen, A. (1947). Trans. Dan. Akad. Technol. Sci. 1, 18-24.

Acta Cryst (2008). E64, i20  [ doi:10.1107/S1600536808003851 ]

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