羟化三苯基锡和(双三苄基锡)氧化物的合成及晶体结构研究  

Synthesis and Characterization of Ph_3SnOH and [(PhCH_2)_3Sn]_2O

作　　者：付彩霞[1] 张军红[2] 马春林[2] 张尊听[1] 

机构地区：[1]陕西师范大学化学与材料科学学院,陕西西安710062 [2]聊城大学化学系,山东聊城252059

出　　处：《合成化学》2003年第3期189-192,共4页Chinese Journal of Synthetic Chemistry

基　　金：国家自然科学基金资助项目 ( 2 0 2 710 2 5 ) ;教育部高等学校骨干教师资助计划项目 ( 2 0 5 0 )

摘　　要：在乙醇钠存在下三苯基氯化锡或三苄基氯化锡水解得羟化三苯基锡 (1)或 (双三苄基锡 )氧化物 (2 )。其结构经元素分析、IR和1HNMR表征 ,X 射线单晶衍射测定了其晶体结构。 1为正交晶系 ,空间群P2 1/n,a =0 .830 0 0 (19)nm ,b =1.0 36 5 (2 )nm ,c =1.80 2 6 (4 )nm ,β =95 .4 72 (7)°,Z =4 ,V =1.5 5 0 7(6 )nm3 ,Dc=1.5 72g·cm -3 ,μ=1.6 4 0mm -1,F(0 0 0 ) =72 8,R1=0 .0 30 9,WR2 =0 .0 70 6 ,中心锡原子为五配位的三角双锥构型 ,且通过配位氧原子连成无限链状。 2为正交菱面体晶系 ,空间群R3 ,a =b =c =0 .96 36 (3)nm ,α =β =γ =84 .0 85 (3)° ,Z =1,V =0 .8812 (4 )nm3 ,Dc=1.5 0 8g·cm -3 ,μ =1.4 4 8mm -1,F(0 0 0 ) =4 0 2 ,R1=0 .0 36 0 ,WR2 =0 .0 5 4 2 ,由两个中心锡原子组成一个结构单元的四配位线性聚合体。Two complexes Ph 3SnOH(1) or [(PhCH 2) 3Sn] 2O(2) were synthesized by the reaction of Ph 3SnCl or (PhCH 2) 3SnCl with sodium alkoxides in 1∶1 molar ratio. Their structures were characterized by element analysis, IR and 1H NMR. Their crystal structures were determined by X ray single crystal diffraction. The crystal 1 belongs to orthorhombic with space group P2 1/n ,a= 0.83000 (19)nm,b=1.0365(2)nm,c=1.8026(4)nm,β=95.472(7)°,Z=4,V=1.5507(6)nm 3,D c= 1.572 g·cm -3 ,μ=1.640mm -1 ,F(000)=728,R 1=0.0309,WR 2=0.0706. In the crystal of complex 1, the tin atom rendered five coordinate in a trigonal bipyramidal geometries. The crystal 2 belongs to rhombohedral with space group R 3,a=b=c=0.9636(3)nm,α=β=γ=84.085(3)°,Z=1,V= 0.8812(4) nm 3,D c=1.508g·cm -3 ,μ=1.448mm -1 ,F(000)=402,R 1=0.0360,WR 2= 0.0542. In the crystal of complex 2, two tin atoms formed a unit and tins were four coordinated.

关 键 词：三烃基锡 乙醇钠 合成 晶体结构 

分 类 号：O614.81[理学—无机化学]