4-Methacryloxybenzaldehyde was prepared and subjected to suspension polymerization with divinylbenzene as a cross-linking agent. The resulting network polymer was ligated with benzoyl hydrazone. The functional polymer was treated with transition metal ions (Cu(II), Ni(II)). The polymer-metal complexes were characterized by elemental analysis, IR, 1 H-NMR, solid state 13 C cross-polarization magic-angle spinning (CP/MAS) NMR, electron paramagnetic resonance (EPR), thermogravimetric and scanning electron microscopy (SEM) studies.