The complex, oxoisothiocyanatobis(pyrrolidinyldithiocarbamato)molybdenum(V), MoO(NCS) (pyrroldtc)2 was prepared. The IR spectra of the complex suggest that the thiocyanate group is attached through nitrogen and the presence of MoO3+ moiety. The voltammograms of the complex in acetonitrile exhibited a pronounced cathodic wave at -0.23 V vs S.C.E. which was attributed to Mo(V)/Mo(IV) couple. The magnetic, epr and electrochemical studies indicate that the compound is mononuclear and molybdenum is in +5 oxidation state. © 1984.