Single crystals of Cadmium oxalate have been grown in silica gel. The optimum conditions were established by varying the concentration of gel solution and reactants, gel setting time and so forth. Prismatic transparent ring i.e. crystal were obtained. Obtained crystals exhibits triclinic structure with unit cell dimension a =4•3551A°, b = 6•8898A°, c =3•2175A°, α= 90•013A°,ß=97•337A°, , γ= 101•963A° calculated from x-ray diffractogram. The grown crystals werefurther characterized with the help of FT-IR studies. Thermal behavior and stability of the grown cadmium oxalate crystals were investigated in the temperature range of 30-1000°c.