The reactions of activated CpFeMn(CO)(7) la and Cp*FeMn(CO)(7) 1b, CP = C5Me5 with thiirane yielded the new dimeric mixed metal disulfido complexes: [CpFeMn(CO)(5)(mu(3)-S-2)](2) (2) and [Cp*FeMn(CO)(5)(mu(3)-S-2)](2) (3). Compounds 2 and 3 both contain two triply bridging disulfido ligands. When heated at 40 degreesC, compound 2 was transformed into a trimeric compound Cp3Fe3Mn3(CO)(15)(mu(3)-S-2)(mu(4)-S-2)(2), 4. Compound 4 contains three disulfido ligands. each of which has a different bridging coordination mode in the six atom metal cluster. There are three inequivalent CpFe(CO)(2) groupings linked to a central Mn-3(S-2)(3) core by the disulfido ligands. In Solution. Compound 4 exhibits a dynamical intramolecular exchange process that interconverts two of the three CpFe(CO), groups on the NMR timescale. (C) 2004 Elsevier B.V. All rights reserved.