Pd(0) nanoclusters were dispersed by using the metal vapour synthesis technique in organometallic polymers of chemical structure [-M(PBu3)(2)-C&3bond; C-C6H4-C6H4-C&3bond; C-](n) (M = Pd, Pt), namely Pd-DEBP and Pt-DEBP. The hybrids were characterized by means of solid state C-13 and 31 P nuclear magnetic resonance, which highlighted the chain organization and the plasticizing effect of the nanoparticles on the polymers. Scanning electron microscopy images of the pristine organometallic polymers, and of their hybrids containing Pd(0), exhibited a growth of nanosized fibrils on glass substrates. High resolution transmission electron microscopy measurements showed a narrow distribution of Pd(0) nanoparticles which have dimensions in the range 1.0-5.0 nm in the case of Pd/Pd-DEBP hybrids and 0.5-2.0 nm in the case of Pd/Pt-DEBP hybrids.