三苄基锡哌啶氨荒酸酯和二苄基锡双哌啶氨荒酸酯合成及晶体结构

Synthesis and Crystal Structure of Tribenzyltin Dithiopiperidylcarbamate and Dibenzyltin Bisdithiopiperidylcarbamate

利用三苄基氯化锡 ,二苄基二氯化锡和哌啶氨荒酸钠反应 ,合成了三苄基锡哌啶氨荒酸酯 (1)和二苄基锡双哌啶氨荒酸酯 (2 ) .通过元素分析、红外光谱、核磁共振氢谱和质谱对其结构进行了表征 .用X 射线单晶衍射测定了这两个化合物的晶体结构 .化合物 1为三斜晶系 ,空间群P 1,a =1.0 2 71(2 )nm ,b =1.1131(2 )nm ,c =1.2 0 96 (2 )nm ,α =76 .5 6 (3)° ,β=81.0 9(3)° ,γ =89.81(3)° ,Z =2 .化合物 2为单斜晶系 ,空间群P2 1/c ,a =0 .9710 (3) ,b =2 .436 (1) ,c=1.2 393(3)nm ,β =90 .2 8(2 )° ,Z =4.在 1的晶体中 ,锡原子呈五配位畸变三角双锥构型 ;

Tribenzyltin dithiopiperidylcarbamate (1) and dibenzyltin bisdithiopiperidylcarbamate (2) were synthesized by the reaction of tribenzyltin chloride or dibenzyltin dichloride with dithiopiperidylcarbamate. Their structures were established by elemental analyses, IR, H-1 NMR and MS spectra, and the crystal structures were determined by X-ray single crystal diffraction. Crystal 1 belongs to triclinic with space group P-1, a = 1.071(2) m, b = 1.1131(2) nm, c = 1.2096(2) nm, alpha = 76.56(3)degrees, beta = 81.09(3)degrees, gamma = 89.81(3)degrees, Z = 2. Crystal 2 belongs to monoclinic with space group P2(1)/c, a = 0.9710(3) nm, b = 2.436(1) nm, c = 1.2393(3) nm, alpha = 76.56(3)degrees, beta = 81.09(3)degrees, gamma = 89.81(3)degrees, Z = 4. In crystal 1 the tin atoms are five-coordinated adopting a distorted trigonal bipyramidal structure. In crystal 2, the structure consists of discrete molecules containing six-coordinate tin atoms in a distorted octahedron configuration.