Abstract Reactions of [Me 2 SSMe] BF 4 with metal thiolate complexes have been used to prepare new complexes with coordinated organic disulfide ligands. Complexes prepared include [CpFe (CO)(L)(PhSSMe)] BF 4 (L, PPh 3, PPh 2 Me, PPh 2 OMe, P (OPh) 3),[CpFe (CO) 2 (MeSSMe)] BF 4 and [CpW (CO) 3 (MeSSMe)[BF 4. A molybdenum analogue of the last compound and [Mn (CO) 5 (MeSSMe)] BF 4 were identified in solution as products of ...