The hydrolysis-condensation pathways of Ni-Sb-ethoxides in different toluene-ethanol solvents have been studied. The hydrolysis was performed by slow addition of controlled amounts of water, diluted in toluene-ethanol solvents. Characterization of the hydrolysis products was performed with single crystal X-ray determinations, IR-spectroscopy, UV-Vis spectroscopy and TGA. In this way, a number of different Ni-Sb-(oxo)-ethoxides have been isolated and characterized. It was thereby shown that the Ni:Sb ratio of the hetero bimetallic oxo-alkoxides varied much depending on the degree of hydrolysis and that the species formed vary with the solvent used and the speed at which the water is added.