The synthesis and characterization of a group of new dendrimers-namely, nanoparticle-cored dendrimers (NCDs)-are described. These materials were obtained by the reduction of hydrogen tetrachloroaurate phase-transferred into toluene in the presence of Frechet-type polyaryl ether dendritic disulfide wedges of generation 1-5. These materials, possessing nanometer-sized gold clusters at the core and dendritic wedges radially connected to the core by Au-S bonds, were analyzed by TEM and TGA, and by UV, IR, and NMR spectroscopies. The number of branching units connected to the core decreased with the generation of the dendritic wedge, and this number changed from 2.18/nm(2) for Au-G-2 to 0.27/nm(2) for Au-G-5. This result suggests that, in the higher-generation NCDs, a large fraction of the surface area of the metal cluster is not passivated and is therefore available for catalytic activity.