Compounds of methacrylic acid with cobalt(II), nickel(II), and copper(II) have been prepared in aqueous solution. The compounds have stoichiometries Co(C4H5O2)2H2O; Ni(C4H5O2)(2)1.5H2O and Cu(C4H5O2)(OH) and polymeric octahedral structures. Thermal decomposition studies show that the hydrated compounds lose water followed by the organic ligands to give the metal oxides. The copper compound decomposes with loss of the organic ligand and the OH group to give the metal oxide.