Single crystals of bismaleato lead(IV) [Pb2(C4H2O4)2] are grown by the controlled diffusion of lead ions in gelated hydrosilica matrix impregnated with maleate ions. The various functional groups present in the compound is identified using FTIR spectrum. The structure of the crystal was elucidated using single crystal XRD studies. It crystallizes in the monoclinic system with space group P21/c. The TG- DTA analysis was employed l to explore the thermal stability and decomposition the pattern. the dielectric measurements were made over wide frequency and temperature ranges. The optical band gap was determined using diffuse reflectance spectroscopy.