Synthesis, structures, and reactivity of four-electron-donor η2-organonitrile, carbonyl oxo, and carbonyl thio complexes of Tungsten

Organometallics

Volumn 15, Issue 10, 1996, Pages 2428-2430

  Thomas, Simon ^a   Tiekink, Edward R T ^b   Young, Charles G ^a  

^a UNIVERSITY OF MELBOURNE   (Australia)

^b UNIVERSITY OF ADELAIDE   (Australia)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 0001266784     PISSN: 02767333     EISSN: None     Source Type: Journal    
DOI: 10.1021/om960083l     Document Type: Article

References (38)

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12. x are also accessible: Thomas, S.; Eagle, A. A.; Gable, R. W.; Young, C. G. Unpublished results.
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15. 2 (1.23 g, 1.56 mmol) in tetrahydrofuran (30 mL) was cooled to 0°C, and pyridine N-oxide (0.30 g, 3.15 mmol) was added. The reaction mixture was stirred for 1 h and the solvent evaporated. The residue was chromatographed on silica using dichloromethane/hexane (3/1) to yield a pink-brown fraction. The product was recrystallized from dichloromethane/methanol as pink crystals, which were filtered, washed with methanol, and dried in vacuo. Yield: 0.76 g, 63%.
16. w = 0.035). In all structural figures, the numbering of the pyrazole rings parallels that shown for the ring containing N(11).
17. Orpen, A. G.; Brammer, L.; Allen, F. H.; Kennard, O.; Watson, D. G.; Taylor, R. J. Chem. Soc., Dalton Trans. 1989, S1.
18. 2-RCN)(CO) (R = Et, Ph) complexes can be prepared but are relatively unstable in solution.
19. 2] as white crystals.
20. 2] (0.75 g, 1.77 mmol) in acetonitrile (25 mL) was heated to 80°C for 30 min and then cooled to room temperature. The solvent was evaporated and the residue chromatographed on silica-dichloromethane to yield a green fraction. The product was recrystallized from dichloromethane/hexane as green crystals, which were filtered, washed with hexane and dried in vacuo. Yield: 0.82 g, 50%.
21. 2-MeCN (one site) > CO.
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31. The elaboration of bound nitriles has been highlighted in the recent work of Templeton et al.: (a) Feng, S. G.; Templeton, J. L. J. Am. Chem. Soc. 1989, 111, 6477. (b) Feng, S. G.; Templeton, J. L. Organometallics 1992, 11, 1295. (c) Feng, S. G.; White, P. S.; Templeton, J. L. Organometallics 1993, 12, 1765. (d) Young, C. G.; Philipp, C. C.; White. P. S.; Templeton, J. L. Inorg. Chem. 1995, 34, 6412.
32. The elaboration of bound nitriles has been highlighted in the recent work of Templeton et al.: (a) Feng, S. G.; Templeton, J. L. J. Am. Chem. Soc. 1989, 111, 6477. (b) Feng, S. G.; Templeton, J. L. Organometallics 1992, 11, 1295. (c) Feng, S. G.; White, P. S.; Templeton, J. L. Organometallics 1993, 12, 1765. (d) Young, C. G.; Philipp, C. C.; White. P. S.; Templeton, J. L. Inorg. Chem. 1995, 34, 6412.
33. The elaboration of bound nitriles has been highlighted in the recent work of Templeton et al.: (a) Feng, S. G.; Templeton, J. L. J. Am. Chem. Soc. 1989, 111, 6477. (b) Feng, S. G.; Templeton, J. L. Organometallics 1992, 11, 1295. (c) Feng, S. G.; White, P. S.; Templeton, J. L. Organometallics 1993, 12, 1765. (d) Young, C. G.; Philipp, C. C.; White. P. S.; Templeton, J. L. Inorg. Chem. 1995, 34, 6412.
34. The elaboration of bound nitriles has been highlighted in the recent work of Templeton et al.: (a) Feng, S. G.; Templeton, J. L. J. Am. Chem. Soc. 1989, 111, 6477. (b) Feng, S. G.; Templeton, J. L. Organometallics 1992, 11, 1295. (c) Feng, S. G.; White, P. S.; Templeton, J. L. Organometallics 1993, 12, 1765. (d) Young, C. G.; Philipp, C. C.; White. P. S.; Templeton, J. L. Inorg. Chem. 1995, 34, 6412.
35. WC = 171 Hz, CO). Further characterization of this material is underway.
36. 2-MeCN)(CO) (0.80 g, 1.00 mmol) in 1:1 acetonitrile/THF (30 mL) was heated to 75°C, and propylene sulfide (0.20 mL, 2.55 mmol) was added. The reaction mixture was heated for 30 min and then cooled to room temperature. The solvent was evaporated and the residue chromatographed on silica-dichloromethane/hexane (2/1) to yield a green fraction. The product was recrystallized from dichloromethane/methanol as green crystals, which were filtered, washed with methanol, and dried in vacuo. Yield: 0.45 g, 57%.
37. w = 0.042). The chloroform molecule of solvation is disordered about a crystallographic 2-fold axis, and the absolute structure was determined on the basis of differences in Friedel pairs included in the data set.
38. Thomas, S.; Eagle, A. A.; Tiekink, E. R. T.; Young, C. G. Unpublished results.