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DOI: 10.1039/A808760A (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1999, 1651-1654

First 12-tungstovanadate Keggin compound: synthesis and crystal structure of [Me4N]7[VW12O40]·15H2O

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M. Ishaque Khan, Sabri Cevik and Randy Hayashi

Abstract

The hydrothermal reaction of Na2WO4·2H2O with finely powdered vanadium metal and tetramethylammonium chloride at 160 °C gave an orange solution which yielded the 12-tungstovanadate Keggin compound [Me4N]7[VW12O40]·15H2O 1. This novel compound has been characterized by the IR, UV-VIS and EPR spectroscopic methods, manganometric titration, and single crystal structure analysis. The crystal structure consists of discrete tetramethylammonium cations, lattice water molecules, and anions of the mixed-valence species [VW12O40]7–. The anion cluster contains tungsten addenda atoms and a {VIVO4} group at its center which is responsible for the overall tetrahedral symmetry of the near spherical polyanion.

References

  1. (a) M. T. Pope, Heteropoty and Isopoly Oxometalates, Springer, Berlin, 1983 Search PubMed; (b) M. T. Pope and A. Müller, Angew. Chem., Int. Ed. Engl., 1991, 30, 34 CrossRef; (c) Polyoxometalates: From Platonic Solids To Anti-Retroviral Activity, eds. M. T. Pope and A. Müller, Kluwer, Dordrecht, 1994 Search PubMed; (d) V. W. Day and W. G. Klemperer, Science (Washington, DC), 1985, 228, 4699 Search PubMed; (e) C. L. Hill, Chem. Rev., 1998, 98, 1 CrossRef CAS.
  2. J. Berzelius, Pogg. Ann., 1826, 6, 369 Search PubMed.
  3. J. F. Keggin, Nature (London), 1933, 131, 908 CrossRef CAS; Proc. R. Soc. London, Ser. A, 1934, 144, 75 Search PubMed.
  4. J. W. Linett, J. Chem. Soc., 1961, 3796 RSC; J. Fuchs, Z. Naturforsch., Teil B, 1973, 28, 389 Search PubMed; H. T. Evans and M. T. Pope, Inorg. Chem., 1984, 23, 501 CrossRef CAS.
  5. (a) L. C. W. Baker, V. S. Baker, K. Eriks, M. T. Pope, M. Shibata, O. W. Rollins, J. H. Fang and L. L. Koh, J. Am. Chem. Soc., 1966, 88, 2329 CrossRef CAS; (b) T. J. R. Weakley and S. A. Malik, J. Inorg. Nucl. Chem., 1967, 29, 2935 CAS and refs. therein; (c) C. M. Tourne, G. F. Tourne, S. A. Malik and T. J. R. Weakley, J. Inorg. Nucl. Chem., 1967, 29, 2935 CAS and refs. therein; (d) F. Zonnevijlle and M. T. Pope, J. Am. Chem. Soc., 1979, 101, 2731 CrossRef CAS; (e) W. H. Knoth, J. Am. Chem. Soc., 1979, 101, 759 CrossRef CAS; (f) X.-Y. Zhang, C. J. O'Connor, G. B. Jameson and M. T. Pope, Inorg. Chem., 1996, 35, 30 CrossRef CAS and refs. therein; (g) D. E. Katsoulis and M. T. Pope, Inorg. Chem., 1984, 106, 2737 CAS; (h) N. Casan-Pastor and L. C. W. Baker, J. Am. Chem. Soc., 1992, 114, 10384 CrossRef and refs. therein; (i) N. Casan-Pastor, P. Gomez-Romero, G. B. Jameson and L. C. W. Baker, J. Am. Chem. Soc., 1991, 113, 5658 CrossRef CAS and refs. therein; (j) J. Rhule, C. L. Hill, D. Judd and R. Schinazi, Chem. Rev., 1998, 98, 327 CrossRef CAS; (k) W. P. Griffith, Transition Met. Chem., 1991, 16, 548 CAS; (l) J. Niu, X. You, C. Duan, H. Fun and Z. Zhou, Inorg. Chem., 1996, 35, 4211 CrossRef CAS; (m) C. Rong and M. T. Pope, J. Am. Chem. Soc., 1992, 114, 2932 CrossRef CAS.
  6. (a) R. Klevtsova, L. Glinskaya, E. Yurchenko and T. Gutsul, J. Struct. Chem., 1991, 32, 687 CrossRef; (b) K. Nomiya and M. Miwa, Polyhedron, 1985, 4, 1407 CrossRef CAS; (c) C. M. Flynn and M. T. Pope, Inorg. Chem., 1971, 10, 2745 CrossRef CAS; (d) E. Radkov and R. Beer, Polyhedron, 1995, 14, 2139 CrossRef CAS; (e) L. Pettersson, I. Andersson and O. W. Howarth, Inorg. Chem., 1992, 31, 4032 CrossRef CAS; D. Hou, K. S. Hagen and C. Hill, J. Chem. Soc., Chem. Commun., 1993, 426 RSC; A. Müller, R. Sessoli, E. Krickemeyer, H. Bögge, J. Meyer, D. Gatteschi, L. Pardi, J. Westphal, K. Hovemeier, R. Rohlfing, J. Döring, F. Hellweg, C. Beugholt and M. Schmidtmann, Inorg. Chem., 1997, 36, 5239 CrossRef; L. Suber, M. Bonamico and V. Fares, Inorg. Chem., 1997, 36, 2030 CrossRef CAS.
  7. G. M. Sheldrick, SADABS, Program for Empirical Absorption Correction of Area Detector Data, University of Göttingen, 1996.
  8. SMART Software Reference Manual, Siemens Analytical X-Ray Instruments, Madison, WI, 1994 Search PubMed.
  9. SAINT Version 4 Software Reference Manual, Siemens Analytical X-Ray Instruments, Madison, WI, 1995 Search PubMed.
  10. G. M. Sheldrick, SHELXTL Version 5 Reference Manual, Siemens Analytical X-Ray Instruments, Madison, WI, 1994 Search PubMed.
  11. International Tables for Crystallography, Kluwer, Boston, 1995, Vol. C, Tables 6.1.1.4, 4.2.6.8 and 4.2.4.2 Search PubMed.
  12. M. I. Khan, E. Yohannes and D. Powell, Inorg. Chem., 1999, 38, 212 CrossRef CAS.
  13. (a) L. Seguin, B. Grand and G. Nowogrocki, Eur. J. Solid State Inorg. Chem., 1995, 32, 181 CAS; (b) M. Asami, H. Ichida and Y. Sasaki, Acta Crystallogr., Sect. C, 1984, 40, 35 CrossRef.
  14. I. D. Brown, in Structure and Bonding in Crystals, eds. M. O'Keefe and A. Navrotsky, Academic Press, New York, 1981, Vol. II, p. 1 Search PubMed.
  15. G. M. Varga, Jr., E. Papaconstantinou and M. T. Pope, Inorg. Chem., 1970, 9, 662 CrossRef; R. A. Prados and M. T. Pope, Inorg. Chem., 1976, 15, 2547 CrossRef CAS.
  16. M. Che, M. Fournier and J. P. Launay, J. Chem. Phys., 1979, 71, 1954 CrossRef CAS.
  17. M. I. Khan, S. Cevik, R. J. Doedens, Q. Chen, S. Li and C. J. O'Connor, Inorg. Chim. Acta, 1998, 277, 69 CrossRef CAS.
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