Synthesis and crystal structures of low-valent binuclear vanadium complexes using the tethering ligand m-xylylenebis(acetylacetonate) (m-xba^2–)

Abstract

An intriguing structural type new to low-valent vanadium chemistry and the binucleating ligand m-H₂xba is exhibited by the reported V^III dimers and the first structurally characterized bis(acetylacetonate) ligated complex of V^II.

References

1. (a) L. Gelmini and W. H. Armstrong, J. Chem. Soc., Chem. Commun., 1989, 1904; (b) M. J. Scott, W. C. A. Wilisch and W. H. Armstrong, J. Am. Chem. Soc., 1990, 112, 2429; (c) W. C. A. Wilisch, M. J. Scott and W. H. Armstrong, Inorg. Chem., 1988, 27, 4333Our interest in low-valent vanadium syntheses reactivity appears elsewhere: (d) C. R. Randall and W. H. Armstrong, J. Chem. Soc., Chem. Commun., 1988, 986; (e) D. B. Sable and W. H. Armstrong, Inorg. Chem., 1992, 31, 161; (f) H. H. Murray, S. G. Novick, W. H. Armstrong and C. S. Day, J. Cluster Sci., 1993, 4, 439; (g) J. A. Davis, C. P. Davie, D. P. Sable and W. H. Armstrong, Chem. Commun., 1998, in press.
2. Y. Hayasi and J. Schwartz, Inorg. Chem., 1981, 20, 3473.
3. M. E. Vol'pin, M. A. Ilatovskaya, E. I. Larikov, M. L. Khidekel', Y. A. Shvetsov and V. B. Shur, Dokl. Akad. Nauk SSSR, 1965, 164, 331.
4. (a) M. Doring, H. Gorls, E. Uhlig, K. Brodersen, L. Dahlenburg and A. Wolski, Z. Anorg. Allg. Chem., 1992, 614, 65; (b) P. Knopp, K. Wieghardt, B. Nuber, J. Weiss and W. S. Sheldrick, Inorg. Chem., 1990, 29, 363; (c) S. Lee, K. Nakanishi, M. Y. Chiang, R. B. Frankel and K. Spartalian, J. Chem. Soc., Chem. Commun., 1988, 785; (d) V. I. Lisoivan and S. A. Gromilov, Zh. Neorg. Khim., 1986, 31, 2539; (e) E. Solari, S. De Angelis, C. Floriani, A. Chiesi-Villa and C. Guastini, Inorg. Chem., 1992, 31, 141 Also reported, [(thf)₃V(µ-acac)(µ-Cl)ZnCl₂], a dimeric structure of acetylacetonate bonded to V^II and Zn^IIvia one of its bridging oxygen atoms; (f) V. A. Grillo, E. J. Seddon, C. M. Grant, G. Aromi, J. C. Bollinger, K. Folting and G. Christou, Chem. Commun., 1997, 1561.
5. J. M. Crabtree, D. W. Marsh, J. C. Tomkinson, R. J. P. Williams and W. C. Fernelius, Proc. Chem. Soc., 1961, 336; W. P. Schaefer, Inorg. Chem., 1965, 4, 642; Y. Torii, H. Iwaki and Y. Inamura, Bull. Chem. Soc. Jpn., 1967, 40, 1550; V. A. Alekseevskii and T. A. Grabovskaya, Russ. J. Inorg. Chem., 1985, 30, 1739.
6. A. W. Maverick and F. E. Klavetter, Inorg. Chem., 1984, 23, 4129.
7. J. P. Collman, J. E. Hutchison, M. A. Lopez, R. Guilard and R. R. Reed, J. Am. Chem. Soc., 1991, 113, 2794; J. P. Collman, J. E. Hutchison, M. A. Lopez and R. Guilard, J. Am. Chem. Soc., 1992, 114, 8066; J. P. Collman, J. E. Hutchison, M. S. Ennis, M. A. Lopez and R. Guilard, J. Am. Chem. Soc., 1992, 114, 8074; J. P. Collman, J. E. Hutchison and P. S. Wagenknecht, Angew. Chem., Int. Ed. Engl., 1994, 33, 1537; R. Guilard, S. Brandes, C. Tardieux, A. Tabard, M. L'Her, C. Miry, P. Gouerec, Y. Knop and J. P. Collman, J. Am. Chem. Soc., 1995, 117, 11 721; J. P. Collman, M. S. Ennis, D. A. Oxford, L. L. Chng and J. H. Griffin, Inorg. Chem., 1996, 35, 1751.
8. L. E. Manzer, Inorg. Synth., 1982, 21, 135 . The bromide derivative was prepared similarly and purified by Soxhlet extraction using thf.
9. The synthesis of m-H₂xba has been described previously: A. W. Maverick, D. P. Martone, J. R. Bradbury and J. E. Nelson, Poyhedron, 1989, 8, 1549.
10. F. L. Bowden and D. Ferguson, Inorg. Chim. Acta, 1978, 26, 251.
11. J. J. H. Edema, W. Stauthamer, S. Gambarotta, F. van Bolhuis, W. J. J. Smeets and A. L. Spek, Inorg. Chem., 1990, 29, 1302.