二乙酰丙酮和2,2′-联吡啶的双核钯(Ⅱ)配合物的合成与结构表征

Synthesis and Structural Characterization of Binuclear Coordination Complex of Palladium(Ⅱ) with Bisacetylacetone and 2,2′-Bipyridine

以二氯化钯、联吡啶(bpy)、二乙酰丙酮合成了双核钯(Ⅱ)的新型固态三元配合物[{Pd(C10H8N2)}2(C10H12O4)][PF6]2,用元素分析、电导率、氢核磁共振谱、电喷雾质谱、红外光谱、电子光谱和荧光光谱对其进行了表征,确定了配合物的组成。利用热重-微分热重法(TG/DTG)讨论了配合物在氮气气氛中的热分解行为。结果表明:该配合物属于低自旋的平面正方形,配合物中离域π键和螯合环的形成使Pd-O和Pd-N键加强,配合物很稳定。

A new solid ternary coordination complex of [Pd（BiPy）]2·[BisAA]·[PF6]2 was synthesized by the reactions of PdC12 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 thermodeeomposition 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 rt bonds and of chelate ring, which made the coordination complex quite stable.