Abstract: The cxidalion-rcduclion characteristic of the ternary clathratc compound {Mo[S₂CN(C₂H₅)₂]₄}⁺{FcCl₄}^-{(C₆H₅CH₂S)₂ was studied by electrochemical measurment in combinaticn with quantum-chemical calculations. The cyclic voltam-mogram of this ternary clathrate compound in 0.1 M KClO₄-DMFwith a platinum electrode was seen to have 2 pairs of oxidation-reduction peaks. Both the electrochemical parameters derived from the voltammogram and the results of EHMOcalculalions indicate that the pair of oxidation-reduction peak at relatively positive potentials corresponds to the oxidation-reduction reaction of Fc(Ⅲ)/Fe(Ⅱ) which is irreversible in nature, while the pair of oxidalion-reducticn peak at more negative potentials corresponds to the oxidation-reduction reaction of Mo(Ⅴ)/Mo(Ⅳ), which is scmircvcrsible. the calculations from experimental measurements are fairly in agremcnt with the theoretical calculalions.