Abstract: A new solid ternary coordination complex of Pd(BiPy)2·BisAA·PF62 was synthesized by the reactions of PdCl2 with 2,2′-bipyridine and with bisacetylacetone in succession,and its molecular structure and composition were characterized by element analysis,conductometry,1H NMR,ESI-MS IR-spectrometry,electron spectroscopy,and fluorescence spectrometry.Its behavior of thermodecomposition in nitrogen atmosphere was studied by TG/DTG.It was found that the complex is of planary square structure with low spin.The bonds between Pd and O,and between Pd and N were strengthened through the formation of conjugated π bonds and of chelate ring,which made the coordination complex quite stable.