A procedure for creating nano-sized chromium clusters (10-100 A) in a porous amorphous hybrid xerogel is described. The xerogel, a poly(1,4-phenylene) bridged silsesquioxane, is a hybrid organic-inorganic network material prepared by sol-gel processing of 1,4-bis(triethoxysilyl)benzene (M-1) and chromium tricarbonyl (triethoxysilyl)benzene (M-2). Chromium(0) metal clusters were produced by an internal doping procedure. Following drying, the hybrid xerogel, when heated to 120 degrees C under high vacuum, results in the formation of irregularly shaped, nano-sized chromium clusters. TEM images were used to establish the size of the metal particles. EDAX and electron diffraction techniques were used to verify the elemental composition and morphology of the metal clusters. Only a slight decrease in surface area and an increase in pore diameter were observed following chromium metal deposition. Intimately mixed nanophases consisting of CdS and chromium metal were also prepared by a combination of external and internal doping procedures.