Poly[(methacrylato)aluminum(III)] was prepared by applying gamma-radiation to the corresponding aluminum(Ill) methacrylate monomer. Scanning electron microscopy images show pellets of similar to 500 nm for the aluminum(III) methacrylate monomer, and submicrometric fibers-made granules for the aluminum-containing polymers. X-ray photoelectron spectroscopy measurements reveal two peaks in the Al 2p core-level spectra of the monomer and of the poly[(methacrylato)aluminum(III)], which means that two different coordination modes for the Al(III) ions might be present in these compounds. Infrared and Raman spectroscopy studies confirmed that the structure for this novel coordination polymer consists of hexa-coordinated Al(III) ions linked by the carboxylate groups of methacrylate ligands, along with hydroxyl groups and coordinated water, in a combination of monodentate and bridging bidentate coordination modes. Hence, combination of spectroscopic methods is a helpful tool to get valuable information on the structure of nonmacrocrystalline coordination polymers. (c) 2006 Wiley Periodicals, Inc.