Abstract: The present invention relates to methods for preparing polymetallic precursors and for preparing improved nanocomposites formed from such precursors which are useful in fuel cell catalyst compositions. The nanocomposites include a support and a plurality of polymetallic nanoparticles with a selected metal atomic ratio. The metals in the polymetallic precursors have a stoichiometric ratio which is approximately equal to the selected atomic ratio of metals in the nanoparticles such that stoichiometric control is provided for the resulting nanocomposite catalyst. Crystalline intermetallic or metal alloy nanoparticles form when a polymetallic precursor having a particular metal stoichiometry is contacted with a conductive support, and the precursor is thermally degraded on the support leading to retention of the metal core of the precursor on the support.