Novel synthetic route to soluble polyanions: synthesis and crystal structure of [K(18-crown-6)]₄[Pb₉]·en·tol †

Abstract

[K(18-crown-6)]₄[Pb₉] was obtained by a novel synthetic procedure, which allows the generation of polyanions by direct reduction of the elements in molten crown ethers at temperatures slightly above 40 °C; the crystal structure refinement shows the coordination of three K atoms to the nonaplumbide anion.

References

1. A. Joannis, C.R. Hebd. Seances Acad. Sci., 1891, 113, 795.
2. E. Zintl, J. Goubenau and W. Dullenkopf, Z. Phys. Chem., Abt. A, 1931, 154, 1.
3. C. A. Kraus, J. Am. Chem. Soc., 1907, 29, 1557.
4. C. J. Warren, R. C. Haushalter and A. B. Bocarsly, J. Alloys Compd., 1995, 229, 175.
5. J.-M. Lehn, Struct. Bonding (Berlin), 1973, 16, 1.
6. D. G. Adolphson, J. D. Corbett and D. J. Merryman, J. Am. Chem. Soc., 1976, 98, 7234.
7. J. D. Corbett, Chem. Rev., 1985, 85, 383.
8. J. D. Corbett, Struct. Bonding (Berlin), 1997, 87, 157.
9. T. F. Fässler, in Metal Clusters in Chemistry, eds. P. Braunstein, L. A. Oro and P. R. Raithby, Wiley-VCH Verlag, Weinheim, 1999.
10. P. A. Edwards and J. D. Corbett, Inorg. Chem., 1977, 16, 903.
11. T. F. Fässler and M. Hunziker, Inorg. Chem., 1994, 33, 5380.
12. T. F. Fässler and M. Hunziker, Z. Anorg. Allg. Chem., 1996, 622, 837.
13. J. Campbell, D. A. Dixon, H. P. A. Mercier and G. J. Schrobilgen, Inorg. Chem., 1995, 34, 5798.
14. B. W. Eichhorn and R. C. Haushalter, J. Chem. Soc., Chem. Commun., 1990, 937.
15. R. G. Teller, L. J. Krause and R. C. Haushalter, Inorg. Chem., 1983, 22, 1809.
16. T. F. Fässler and R. Hoffmann, Chimia, 1998, 52, 158.
17. T. F. Fässler and R. Hoffmann, Angew. Chem., 1999, 111, 526; Angew. Chem., Int. Ed., 1999, 38, 543.
18. B. W. Eichhorn and R. C. Haushalter, J. Am. Chem. Soc., 1988, 110, 870.
19. V. Quéneau and S. C. Sevov, Inorg. Chem., 1998, 37, 1358.
20. E. Todorov and S. C. Sevov, Inorg. Chem., 1998, 37, 3889.