A Tungsten 0 -Fullerene-60 Derivative

Pasquali, P. Leoni, P. Sabatino, and D. Braga, Gazx- Chim. Ital. 122, 275 (1992). 

Submitted by JANICE M. HALL, JOSHUA H. HOYNE, and JOHN R. SHAPLEY  

Since the first report of a complex involving a direct metal-to-Ceo bond, (Ph3P)2 Pt( 7 -C6o)/ numerous studies have established that the fullerene Ceo acts as a moderately electronegative alkene in coordinating to electron-rich metal centers. In many cases the Ceo ligand is subject to relatively facile displacement when the complex is in solution however, the zerovalent, octahedral complexes M(CO)3(dppe)(Cgo) [M = Mo, W dppe = l,2-bis(diphenylphosphino)ethane] display outstanding stability even under severe conditions. The overall time needed to prepare these complexes from commercially available M(CO)g is dramatically reduced by adopting a biphasic procedure for the synthesis of the precursor M(CO)4(dppe), which was first described for the preparation of Mo(CO)4 (dppe). Here details are presented for the biphasic synthesis of W(CO)4(dppe) and for its use in the preparation of W(CO)3(dppe)(Cgo)- 

W(CO)e (Strem), dppe (Arapahoe), and [n-Bu4N]Br (Aldrich) are reagent-grade and used as received. Cgo (98%) is available from Southern Chemical Group. Other solvents and reagents are reagent-grade and used as received. 

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