Present work reports the dielectric, FTIR and thermal studies of Ni2+:MHMH single crystals. The influence of addition of transition metal ions on the dielectric properties, like dielectric constant, loss tangent and a.c. conductivity of these crystals were discussed. FTIR studies confirm the presence of carboxylate ions. The melting point of the sample and final product after decomposition were studied using TG/DTA.