The redox properties of the hydrotalcite-intercalated bis(2-mercapto-2,2-diphenyl-ethanoate) dioxomolybdate(VI) complex are investigated by cyclic voltammetry by using modified carbon paste electrodes and clay-modified electrodes. The electrochemical data provide evidence that boundary-associated species involving the VI, V and TV oxidation states of molybdenum are responsible for the electroactivity.