Preparation and characterization of organometallic dysprosium complex embedded polyhedral silica nanofoam (PNE-SiO2) is reported. The nanoporous solid was obtained via a sol-gel process involving precipitation of polymer micelles, hydrolysis and condensation of silica by swelling of triblock copolymer template micelles of PEO-PPO-PEO at acidic pH using high oil concentration and fast stirring. Metal-complex incorporation was performed via wet impregnation (WI) at higher temperature, where the dysprosium complex is chemically bound to the silanol groups of the silica foam surface. Scanning electron microscopy (SEM), transmission electron microscopy (TEM) and small angle X-ray scattering (SAXS) revealed that the particles of the organometallic complex are evenly distributed on the walls of the polyhedral cells, while nitrogen adsorption/desorption measurements (BET) verified that the characteristic meso- and macrocell structure of PNE-SiO2 composed of polyhedral cells of silica joined at mesosized windows are preserved also after incorporation.