Simple metal acetates react to give bimetallic heterocubanes of the type [${{{\rm {\rm M}}{{1\hfill \atop 4- y\hfill}}}}$${{{\rm {\rm M}}{{2\hfill \atop y\hfill}}}}$O4] (see structure, M1,2=Mn, Co, Ni, Zn), which in turn are precursors for the selective formation of bimetallic oxide nanoparticles with a controlled composition. The size of the particles can be controlled by adjusting the thermolysis temperature.