In this work, we studied the Nickel electrodeposition to determine its potential of reduction. Then. We studied the complexation of this compound dithiolic selected with Nickel in a mixed medium (DMF/H2O) by an electrochemical method. We have noticed that the addition of an increasing quantity of Nickel ions involves the modification of the intensity of the cathodic current of this compound without modifying its potential of reduction. In addition, there is a displacement of the potential of oxidation, which involves an electrochemical signature, which proves the complexation.