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
摘 要
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.
双核钯配合物
二氯化钯
2,2′-联吡啶
二乙酰丙酮
Characterization
Binuclear coordination
Palladium(Ⅱ)
2,2′-Bipyridine
Bisacetylacetone
Abstract
A new solid ternary coordination complex of [Pd(BiPy)]2·[BisAA]·[PF6]2 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.
中图分类号 O657.3
所属栏目 工作简报
基金项目 江西省自然科学基金项目(2008GZH0063),江西省教育厅科技项目(GJJ07429,GJJ09355)
收稿日期 2008/3/4
修改稿日期
网络出版日期
作者单位点击查看
备注梅光泉(1965-),男,江西高安市人,教授,博士,研究方向为应用化学、配位化学.
引用该论文: MEI Guang-quan,HUANG Ke-long. Synthesis and Structural Characterization of Binuclear Coordination Complex of Palladium(Ⅱ) with Bisacetylacetone and 2,2′-Bipyridine[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(4): 458～462
梅光泉,黄可龙. 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[J]. 理化检验－化学分册, 2009, 45(4): 458～462
共有人对该论文发表了看法，其中：
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】HUANG Hai-ping,LI Sheng-hui,YU Shu-yan,et al.Novel pyrazolate-bridged dinuclear Pd(Ⅱ) diimine complexes that bind inorganic anions[J].Inorg Chem Commun,2005,8:656-660．
【2】俞开潮,YOUSEF H,程银华,等.催化增强化学蒸气沉积法在聚酰亚胺上沉积钯-铂合金薄层[J].无机化学学报,2006,22(5):789-794．
【3】KRUGER P E,MOUBARAKI B,FALLON G D,et al.Tetranuclear copper(Ⅱ) complexes incorporating short and long metal-metal separations:synthesis,structure and magnetism[J].J Chem Soc,Dalton Trans,2000(5):713-718．
【4】GEARY W J.Use of conductivity mesurements in organic solvents for the characterization of coordination compounds[J].Coordination Chemistry Reviews,1971,7(1):81-122．
【5】NEWKOME G R,PUCKETT W E,KIEFER G E,et al.Chemistry of heterocyclic compounds series.94.Square-planar cis- and trans-C-palladium(Ⅱ) complexes of N electron-deficient heteroaromatic ligands.Ligand synthesis,complexation,and spectral analyses and complex interaction with phage PM2 DNA[J].Inorg Chem,1985,24(6):8l1-826．
【6】赵永亮,赵风英.铕镧苯甲酸α,α′-联吡啶配合物的合成及性质研究[J].光谱学与光谱分析,2002,22(6):987-990．
【7】中本一雄.无机和配位化合物的红外和拉曼光谱[M].4版.北京:化学工业出版社,1991:288-290．
【8】梁广,刘伟平,普绍平,等.乙酰丙酮钯(Ⅱ)的合成及其结构表征[J].贵金属,2004,25(4):12-16．
【9】SINGHAL A,MISHRA R,KULSHRESHTHA S K.Dimeric allylpalladium(Ⅱ) complexes with pyrazolate bridges:synthesis,characterization,structure and thermal behaviour[J].J Organometal Chem,2006,691:1402-1410．
【2】俞开潮,YOUSEF H,程银华,等.催化增强化学蒸气沉积法在聚酰亚胺上沉积钯-铂合金薄层[J].无机化学学报,2006,22(5):789-794．
【3】KRUGER P E,MOUBARAKI B,FALLON G D,et al.Tetranuclear copper(Ⅱ) complexes incorporating short and long metal-metal separations:synthesis,structure and magnetism[J].J Chem Soc,Dalton Trans,2000(5):713-718．
【4】GEARY W J.Use of conductivity mesurements in organic solvents for the characterization of coordination compounds[J].Coordination Chemistry Reviews,1971,7(1):81-122．
【5】NEWKOME G R,PUCKETT W E,KIEFER G E,et al.Chemistry of heterocyclic compounds series.94.Square-planar cis- and trans-C-palladium(Ⅱ) complexes of N electron-deficient heteroaromatic ligands.Ligand synthesis,complexation,and spectral analyses and complex interaction with phage PM2 DNA[J].Inorg Chem,1985,24(6):8l1-826．
【6】赵永亮,赵风英.铕镧苯甲酸α,α′-联吡啶配合物的合成及性质研究[J].光谱学与光谱分析,2002,22(6):987-990．
【7】中本一雄.无机和配位化合物的红外和拉曼光谱[M].4版.北京:化学工业出版社,1991:288-290．
【8】梁广,刘伟平,普绍平,等.乙酰丙酮钯(Ⅱ)的合成及其结构表征[J].贵金属,2004,25(4):12-16．
【9】SINGHAL A,MISHRA R,KULSHRESHTHA S K.Dimeric allylpalladium(Ⅱ) complexes with pyrazolate bridges:synthesis,characterization,structure and thermal behaviour[J].J Organometal Chem,2006,691:1402-1410．
相关信息
