Protonation of [{(mu-SCH2)(2)N(C6H4-p-NO2)}{Fe(CO)(2)(PMe3)}(2)] in the presence of 4 equiv. of HOTf afforded two species, a mu-hydride diiron complex, the molecular structure of which was crystallographically characterized, and a p-S-protonated species, which was readily deprotonated in the presence of pyridine.