The complexes of nickel(II) and palladium(II) with dipivaloylmethane (DPM: 2,2,6,6- tetramethyl-3,5-heptandion) were synthesized. The experimental results showed that the formula of the complex of nickel(II) with DPM formed in diethylether - ethanol(EtOH) solvent was Ni(DPM). This complex was converted into Ni(DPM)2 complex by heating at 80o C. The formula of Pd(II) - DPM complex was Pd(DPM)2. Both of Pd(DPM)2 and Ni(DPM)2 were good volatile complexes.