Abstract:The far infrared spectroelectrochemistry of linear M/Fe/S (M = Mo, W) complexes was investigated in methylene chloride and dichloroethane. With CsI as spectral windows, bands above 200 cm -1 can be observed in methylene chloride, except for a weak methylene chloride band at 450 cm -1 . Substitution of dichloroethane for methylene chloride, solvents of nearly identical electrochemical properties, allows one to observe solute bands in the 450 cm -1 region. The far-infrared spectroelectrochemistry of [MoFe2S4Cl4] 2-and its tungsten analogue was investigated. The disappearance of the oxidation bands and the appearance of bands due to the reduced product could be clearly observed. The origin of the vibrational bands could be clearly identified using 34 S substituted complexes. In addition NOT THE PUBLISHED VERSION; this is the author's final, peer-reviewed manuscript. The published version may be accessed by following the link in the citation at the bottom of the page.