一维链状3-吡啶甲酸三苄基锡的合成和晶体结构

利用三苄基氯化锡和3-吡啶甲酸在三乙胺存在下以1:1摩尔比反应,合成了一维链状的有机锡配合物3-吡啶甲酸三苄基锡{(C7H7)3Sn(PyCO2H)2Sn(C7H7)3}。通过元素分析、红外光谱、核磁共振氢谱和X-射线单晶衍射对其结构进行了表征。测试结果表明:该配合物(C27H25- NO2Sn, Mr = 514.17)为单斜晶系,空间群P21/c, a = 10.618(6), b = 14.683(8), c = 16.050(9) ?β= 106.488(9)? Z = 4, V = 2399(2) ?, Dc = 1.423 g/cm3, ?= 1.087 mm-1, F(000) = 1040, R = 0.0266, wR = 0.0629。通过3-吡啶甲酸配体的氮原子桥联, 形成五配位三角双锥构型的链状结构。

Synthesis and Crystal Structure of the Organotin Complex Tribenzyltin 3-Picolinate

The title complex tribenzyltin 3-picolinate C27H25NO2Sn (Mr = 514.17) was synthesized by the reaction of 3-pyridinecarboxylic acid with the tribenzyltin chloride in benzene with Et3N, and characterized by elemental analysis, IR and 1H NMR. The crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/c with a = 10.618(6), b = 14.683(8), c = 16.050(9) ? ?=106.488(9)o, Z = 4, V = 2399(2) ?, Dc = 1.423 g/cm3, ?= 1.087 mm-1, F(000) = 1040, R = 0.0266 and wR = 0.0629. In this crystal, the tin atom is five-coordinated in a trigonal bipyramidal structure by bridging the pyridine N atom, resulting the chain organotin complex.