The electrochemical behavior of bis-(2,6-diisopropylphenyl)diazobutadiene- 1,4 and its nickel dibromide complex on dropping mercury and glassy carbon electrodes in an aprotic solvent was studied by AC polarography and cyclic voltammetry. Both the ligand and the nickel ion complex were shown to undergo electroreduction. The electrochemical reduction of nickel bis-(2,6- diisopropylphenyl)diazobutadiene-1,4 dibromide occurred stepwise and formed intermediate nickel(I) species.