The preparation of catalysts from molecular precursors is the long term goal of our research. The predetermination of metal composition in molecular precursors is an advantage of this method over others (e.g. co-precipitation). The main objective of this project is the production of Pd/Co-nanoparticles from Pd2Co(Me2Brpz)4Cl4 and Co 2Pd(Me2Brpz)4Cl4 precursors (Me 2BrpzH = 3,5-dimethyl-4-BrpzH. These heterobimetallic compounds have been characterized by X-ray crystallographic analysis and standard spectroscopic techniques. The precursors were thermally reduced to remove the inorganic and organic ligands, producing the desired alloys. The particles obtained from thermal reduction have been analyzed by X-rays fluorescence (XRF). Spheres and agglomerates of nanoparticles are observed on the surface of carbon / copper grids.