Triphosphamacrocycle complexes of rhodium(III), iron(II) and ruthenium(II); crystal structure of trichloro[1,5,9-tris(2-propyl)-1,5,9-triphosphacyclododecane]rhodium( III) 

Abstract

The free macrocyclic 1,5,9-tris(2-propyl)-1,5,9-triphosphacyclododecane (Prⁱ₃[12]aneP₃, L) has been used for the first time to prepare a range of metal complexes. Reaction of L with RhCl₃·3H₂O yields the six-co-ordinate fac-octahedral complex [RhCl₃(L)], which has been structurally characterised and is also used to prepare the analogous rhodium(III )–trihydrido and –triiodo complexes. The half-sandwich complex, [Fe(η⁵-C₅H₅)(L)]PF₆ was prepared from [Fe(η⁵-C₅H₅)(η⁶-C ₆H₅)]PF₆ and L. The ruthenium complexes [RuCl₂(dmso)(L)] (dmso = dimethyl sulfoxide) and [Ru₂(µ-Cl)₃(L)₂]Cl were also formed from the reaction of L with [RuCl₂(dmso)₄] and [RuCl₂(η⁶-C₆H₄Me-4-Pr ⁱ-1)]₂ respectively.

References

1. (a) E. P. Kyba, C. W. Hudson, M. J. McPhaul and A. M. John, J. Am. Chem. Soc., 1977, 99, 8053; E. P. Kyba, A. M. John, S. B. Brown, C. W. Hudson, M. J. McPhaul, A. Harding, K. Larsen, S. Niedzwiecki and R. E. Davis, J. Am. Chem. Soc., 1980, 102, 139; (b) E. P. Kyba and S.-S. P. Chou, J. Chem. Soc., Chem. Commun., 1980, 449; M. A. Fox, K. A. Campbell and E. P. Kyba, Inorg. Chem., 1981, 20, 4163.
2. E. P. Kyba, R. E. Davis, S. T. Liu, K. A. Hassett and S. B. Larsen, Inorg. Chem., 1985, 24, 4629.
3. B. N. Diel, P. F. Brandt, R. C. Haltiwanger and A. D. Norman, J. Am. Chem. Soc., 1982, 104, 4700; B. N. Diel, P. F. Brandt, R. C. Haltiwanger, M. J. L. Hackney and A. D. Norman, Inorg. Chem., 1989, 28, 2811.
4. (a) S. J. Coles, P. G. Edwards, J. S. Fleming and M. B. Hursthouse, J. Chem. Soc., Dalton Trans., 1995, 1139; (b) S. J. Coles, P. G. Edwards, J. S. Fleming, S. S. Liyanage and M. B. Hursthouse, J. Chem. Soc., Dalton Trans., 1996, 1801.
5. S. J. Coles, P. G. Edwards, J. S. Fleming and M. B. Hursthouse, J. Chem. Soc., Dalton Trans., 1995, 4091.
6. P. G. Edwards, J. S. Fleming and S. S. Liynanage, Inorg. Chem., 1996, 35, 4563.
7. T. J. Riedo and T. A. Kaden, Chimia, 1977, 31, 220; S. C. Rawle, G. A. Admans and S. R. Cooper, J. Chem. Soc., Dalton Trans., 1988, 93.
8. L. J. Zompa, Inorg. Chem., 1978, 17, 2531.
9. W. Rosen and D. H. Busch, Inorg. Chem., 1970, 9, 262; M. Nonoyama, Inorg. Chim. Acta, 1976, 20, 53; M. Nonoyama, J. Inorg. Nucl. Chem., 1977, 39, 550.
10. S. C. Rawle, T. J. Sewell and S. R. Cooper, Inorg. Chem., 1987, 26, 3769.
11. P. Chaudhuri and K. Wieghardt, Prog. Inorg. Chem., 1987, 35, 329.
12. A. J. Blake and M. Schröder, Adv. Inorg. Chem., 1990, 35, 1.
13. (a) J. Chatt, N. P. Johnson and B. L. Shaw, J. Chem. Soc., 1964, 2508; (b) R. B. King, P. N. Kapour and R. N. Kaffer, Inorg. Chem., 1971, 10, 1841.
14. R. L. Geerts, J. C. Hoffman and K. G. Caulton, Inorg. Chem., 1986, 25, 590; C. Bianchini, C. Meath, A. Meli and M. Sabat, J. Chem. Soc., Chem. Commun., 1986, 777; C. Bianchini, F. Lascki, D. Masi, C. Meath, A. Meli, F. M. Chainani, D. M. Proserpio, M. Sabat and P. Zanello, Inorg. Chem., 1989, 28, 2552.
15. A. Albinati, F. Denartin, P. Janner, L. F. Rhodes and L. M. Venanzi, J. Am. Chem. Soc., 1989, 111, 2115; J. Ott, L. M. Venanzi, C. A. Ghiardi, S. Madollini and A. Orlandini, J. Organomet. Chem., 1985, 291, 89.
16. S. G. Davies, H. Felkin and O. Watts, J. Chem. Soc., Chem. Commun., 1980, 159.
17. A. J. Blake, R. D. Crofts, G. Reid and M. Schröder, J. Organomet. Chem., 1989, 259, 371.
18. (a) L. F. Rhodes, C. Sorato, L. M. Venanzi and F. Backechi, Inorg. Chem., 1988, 27, 604; A. Albinati, Q. Jiang, H. Ruegger and L. M. Venanzi, Inorg. Chem., 1988, 32, 4945; (b) S. G. Davies, S. J. Simpson, H. Felkin and T. Fillebeen-Khan, Organometallics, 1983, 2, 539; (c) J. B. Letts, T. J. Mazanec and D. W. Meek, Organometallics, 1983, 2, 695; G. Jia, A. L. Rheingold, B. S. Haggerty and D. W. Meek, Inorg. Chem., 1992, 31, 900; (d) L. Dahlenburg, S. Kerstan and D. Werner, J. Organomet. Chem., 1991, 411, 457.
19. S. C. Rawle and S. R. Cooper, J. Chem. Soc., Chem. Commun., 1987, 308; S. C. Rawle, T. J. Sewell and S. R. Cooper, Inorg. Chem., 1987, 26, 3769; M. N. Bell, A. J. Blake, M. Schröder and T. A. Simpson, J. Chem. Soc., Chem. Commun., 1986, 471; M. N. Bell, A. J. Blake, M. Schröder, H.-J. Küppers and K. Wieghardt, Angew. Chem., Int. Ed. Engl., 1987, 26, 250; M. N. Bell, A. J. Blake, R. O. Gould, S. Parsons, C. Radek and M. Schröder, Transition Met. Chem., 1995, 20, 600.
20. F. A. Cotton, K. A. Dunbar, C. T. Bagle, L. R. Favello, S.-J. Kang, A. C. Price and M. G. Verbruggen, Inorg. Chim. Acta, 1991, 184, 35.
21. A. C. Skapski and F. A. Stephens, J. Chem. Soc., Dalton Trans., 1973, 1789.
22. F. H. Allen, G. Chang, K. K. Cheung, T. F. Lai, L. M. Lee and A. Pidcock, Chem. Commun., 1970, 1297.
23. R. B. King, Organometallic Syntheses, eds. R. B. King and J. J. Eisch, Academic Press, New York, 1965, vol. 1, p. 139.
24. M. A. Bennett and A. K. Smith, J. Chem. Soc., Dalton Trans., 1974, 223.
25. I. P. Evans, A. Spencer and G. Wilkinson, J. Chem. Soc., Dalton Trans., 1973, 204.
26. J. W. Pflugrath and A. Messerschmidt, MADNES, Version 11, Delft Instruments, Delft, 1989.
27. N. P. C. Walker and D. Stuart, Acta Crystallogr., Sect. A, 1983, 39, 158; adapted for FAST geometry by A. Karaulov, University of Wales, Cardiff, 1991.
28. G. M. Sheldrick, Acta Crystallogr., Sect. A, 1990, 46, 467.
29. G. M. Sheldrick, University of Göttingen, 1993.
30. K. Davies and K. C. Prout, University of Oxford, 1993.