Lead-cobalt mixed levo tartrate crystals for different compositions of lead and cobalt were grown by using single diffusion gel growth method in silica hydro gel medium. Long and dendrite type white crystals as well as spherulitic crystals were obtained. The metallic composition in the crystals was estimated by EDAX. It was found that the metallic composition in the crystals did not vary as per the composition of supernatant solution, i.e., lead content was found more than cobalt content. The powder XRD suggested the orthorhombic nature for all crystals. The grown crystals were characterized by FTIR spectroscopy and thermal studies. The FTIR spectra revealed the presence of water molecules, O-H, C-H, C-O and C=O functional groups. The thermo-grams suggested that the crystals were thermally unstable and decomposed into oxide through carbonate stage.