Synthetic methodologies and structures of metal-[c-60]fullerene complexes

A review of the chemistry of transition metal-[C-60] fullerene complexes is presented. The main focus is directed toward the different methodologies for obtaining both metal bound and ligand bound complexes of C-60, and the different types of structures which have been so far identified for metal-C-60 complexes

Mixed-chalcogenide, mixed-metal carbonyl clusters. Synthesis and characterization of Cp(2)Mo(2)Fe(2)(mu(4)-Te)(mu(3)-E')(CO)(6) (E,E'=Te; E=S,E'=Te; E,E'=S; E=S, E'=Se), Cp(2)Mo(2)Fe(2)(mu(3)-Te)(mu(3)-E)(CO)(7), and Cp(2)Mo(2)Fe(mu(3)-E)(CO)7 (E=S, TE)

Reflux of a benzene solution of Fe3STe(CO)(9) and Cp(2)Mo(2)(CO)(6) yielded the new cluster Cp(2)Mo(2)Fe(2)STe(CO)(7) (6) as the major product and the following clusters in smaller amounts: Cp(2)Mo(2)Fe(2)Te(3)(CO)(6) (1), Cp(2)Mo(2)Fe(2)STe(2)(CO)(6) (2), Cp(2)Mo(2)Fe(2)S(2)Te(CO)(6) (3), Cp(2)-Mo2FeTe(CO)(7) (4), Cp(2)Mo(2)FeS(CO)(7) (5), and Cp(2)Mo(2)Fe(2)Te(2)(CO)(7) (7). The new cluster 3 was formed in good yield when a benzene solution of 6 was refluxed with sulfur powder. Similarly, 2 was obtained when a benzene solution of 6 was refluxed with tellurium powder. A new cluster with three different chalcogen ligands, Cp(2)Mo(2)Fe(2)SSeTe(CO)(6) (8), was obtained when a benzene solution of 6 was refluxed in the presence of selenium powder. Structures of 1-4, 6, and 8 were established by crystallographic methods. The structures of 1-3 and 8 consist of Mo2Fe2 butterfly cores with a mu(4)-Te atom and two mu(3)-chalcogen atoms (1, Te and Te; 2, S and Te; 3, S and S; 8, S and Se) capping the two Mo2Fe faces. Each Mo atom has a Cp ligand, and each Fe atom has three terminally bonded carbonyl groups. The structure of 4 conists of a Mo2FeTe tetrahedron with each Mo possessing a Cp ligand and two terminally bonded carbonyl groups and the Fe atom having three terminal carbonyl groups attached to it. The structure of 6 consists of a Mo2Fe2 tetrahedron. One Mo2Fe face is capped by a mu(3)-S ligand and the other by a mu(3)-Te atom. The Fe-Fe bond is bridged by a carbonyl group; there are two terminally bonded carbonyl groups attached to each Fe atom. A semitriply bridging earbonyl group is attached to one Mo atom. The other Mo atom has one terminal carbonyl group. Each Mo atom has one Cp ligand attached to it

Synthesis and spectroscopic characterization of (CO)(6)Fe-2{mu-EC(H)=C(H)E'} (E not equal E'; E,E'=S, Se, Te) and (CO)(6)Fe-2{mu-TeC(H)=C(H)Te}. Structural characterization of (CO)(6)Fe-2{mu-SC(Ph)=C(H)Se} and (CO)(6)Fe-2{mu-SC(H)=C(Ph)Te}

When acetylene gas was bubbled through methanol solutions containing the mixed-chalcogenide compounds (CO)(6)Fe-2(mu-EE') (E not equal E'; E, E' = S, Se, Te), the acetylene adducts (Co)(6)Fe-2{mu-EC(H)=C(H)E'} (1, 52%, E, E' = S, Se; 2, 46%, Et E' = S, Te; 3, 38%, E, E' = Se, Te) were obtained, In addition, trace amounts of the homochalcogenide derivatives (CO)(6)Fe-2-{mu-EC(H)=C(H)E} (E = S, Se, Te) were also obtained. The Te-2 compound (CO)(6)Fe-2{mu-TeC-(H)=C(H)Te) (4) was obtained in 32% yield from the reaction of (CO)(6)Fe-2(mu-Te-2) with acetylene. Compounds 1-4 were characterized by IR and H-1, C-13, Se-77, and Te-125 NMR spectroscopy. Crystallographic analysis of the phenylacetylene adducts (CO)(6)Fe-2{mu-SC(Ph)=C(H)Se} (5) and (CO)(6)Fe-2(CO)(6)Fe-2{mu-SC(H)=C(Ph)Te) (6) were carried out. The structures of both 5 and 6 can be described as Fe(2)SE (E = Se, Te) tetrahedral butterfly cores containing the phenylacetylene as a bridge between the two wingtip chalcogen atoms, with three terminally bonded carbonyl groups on each Fe atom