双齿膦参与的非均三脚架配位银化合物的合成、结构与表征  

Synthesis, Structure and Characterization of an Ag Complex of a Hetero-armed Tripodal Ligand with Diphosphine Participation

作　　者：张利[1] 刘俊[1] 邓良容[1] 张华新[1] 蔡跃鹏[1] 刘汉钦[1] 康北笙[1,2] 

机构地区：[1]中山大学化学与化学工程学院 [2]中国科学院上海有机化学研究所金属有机国家重点实验室上海200032

出　　处：《化学学报》2002年第4期566-568,共3页Acta Chimica Sinica

基　　金：国家自然科学基金 (No.2 99730 5 9) ;广东省自然科学基金 (No .0 0 12 32 );中山大学化学与化学工程学院综合化学实验创新研究基金资助项目

摘　　要：Complex [Ag 2(DPYBIM)(dppm)](BF 4) 2·CH 3OH was obtained from the reaction of AgBF 4 and the hetero-armed tripodal ligand DPYBIM [N,N-bis(2-pyridylmethyl)-N-(2-benzimidazolylmethyl)amine] with the participation of dppm [bis(diphenylphosphino)- methane]. Single crystal X-ray diffraction analysis showed that the crystal belongs to the triclinic space group P1-. The cell parameters are: M r=1135.17, a=1.0619(2) nm, b=1.4246(3) nm, c=1.6767(3) nm, α=91.08(3)°, β=104.04(3)°, γ=101.77(3)°, V=2.4027(8) nm 3, D c=1.569 Mg/m 3, Z=2, F(000)=1140, μ=9.53 cm -1, R=0.057, wR=0.145. In the complex, one of the Ag atoms is linearly coordinated by PN from dppm and the benzimidazolyl group of the tripodal ligand, respectively, while the other is tetrahedrally coordinated by PN 3 where two of the N atoms are from the pyridine arms and one is the amino-N. Two types of intermolecular π...π interactions lead to the 1D infinite "Z"-shaped chain. The complex was characterized by elemental analysis, IR and MS. 31P NMR showed characteristic AA′XX′pattern of two symmetrical multiplets centered at δ=10.07.Complex [Ag-2 (DPYBIM) (dppm)] (BF4)(2).CH3OH was obtained from the reaction of AgBF4 and the hetero-armed tripodal ligand DPYBIM [N, N-bis (2-pyridylmethyl)-N-(2-benzimidazolylmethyl) amine] with the participation of dppm [bis ( diphenylphosphino) - methane]. Single crystal X-ray diffraction analysis showed that the crystal belongs to the triclinic space group P (1) over bar. The cell parameters are: M-r = 1135.17, a 1.0619 (2) nm, b = 1.4246 (3) rim, c = 1.6767 (3) run, a = 91.08 (3)degrees, beta = 104.04(3)degrees, gamma = 101.77 (3)degrees, V = 2.4027 (8) nm(3), D-c = 1.569 Mg/m(3) Z = 2, F (000) = 1140, mu = 9. 53 cm(-1), R = 0.057, wR = 0.145. In the complex, one of the Ag atoms is linearly coordinated by PN from dppm and the benzimidazolyl group of the tripodal ligand, respectively, while the other is tetrahedrally coordinated by PN3 where two of the N atoms are from the pyridine am-is and one is the amino-N. Two types of intermolecular pi...pi interactions lead to the ID infinite 'Z'-shaped chain. The complex was characterized by elemental analysis, IR and MS. P-31 NMR showed characteristic AA'XX'pattern of two symmetrical multiplets centered at delta = 10.07.

关 键 词：双齿膦 合成 结构 表征 银配合物 非均三脚架配体 双齿膦配体 ^31P核磁谱 

分 类 号：O641.4[理学—物理化学]