三(邻甲苯基)氢化锡与1-乙炔基环戊醇和1-乙炔基环己醇的加成物的合成及晶体结构

Synthesis and Crystal Structures of Additive Product of Tri-o-tolyltin Hydride and 1-Ethynylcyclopentanol and 1-Ethynylcyclohexanol

通过三 (邻甲苯基 )氢化锡与 1 乙炔基环己醇和 1 乙炔基环戊醇发生加成反应 ,得到两个加成物 :(Z) 1 [2 (三 -邻甲苯基锡基 )乙烯基 ]环戊醇 ( 1)和 (Z) 1 [2 (三 -邻甲苯基锡基 )乙烯基 ]环己醇 ( 2 ) .通过元素分析、红外光谱和核磁共振氢谱等手段对其结构进行了表征 .用X射线单晶衍射测定了加成物 1和 2的晶体结构 .二者均为具有分子内O→Sn弱配位的扭曲四面体结构 .1属于单斜晶系 ,P2 1 /n空间群 ,晶胞参数 :a =1 0 496( 2 )nm ,b =1 765 8( 4 )nm ,c =1 3 193 ( 3 )nm ,β =90 60 ( 3 )° ,V =2 44 5 1( 8)nm3 ,Z =4,R =0 0 3 17,wR =0 0 82 0 .2属于三斜晶系 ,空间群P1,晶胞参数 :a =0 85 5 92 ( 17)nm ,b =0 93 0 16( 19)nm ,c =1 63 68( 3 )nm ;α =83 76( 3 )° ,β =82 69( 3 )° ,γ =78 0 5 ( 3 )° ;V =12 60 0 ( 4 )nm3 ,Z =2 ,R =0 0 3 77,wR =0 10 3 0 .

Z ) 1 [2 (Tri o tolylstannyl)vinyl]cyclopentanol (1) and ( Z ) 1 [2 (tri o tolylstannyl)vinyl] cyclohexanol (2) were synthesized by additive reaction of the corresponding tri o tolyltin hydride to the triple bond of 1 ethynylcyclopentanol and 1 ethynylcyclohexanol, respectively. All compounds were characterized by elemental analysis, IR and 1H NMR spectra. The crystal and molecular structures of 1 and 2 have been determined by single crystal X ray diffraction analysis. The Sn atoms in 1 and 2 adopt a tetrahedral geometry distorted towards trigonal bipyramid duo to a weak intramolecular interaction between Sn and hydroxyl O atoms [the distances of Sn—O are 0 2771(4) nm for 1 and 0 2764(5) nm for 2]. Compound 1 belongs to monoclinic system with space group P 2 1/ n , a =1 0496(2) nm, b =1 7658(4) nm, c =1 3193(3) nm, β =90 60(3)°, V =2 4451(8) nm 3, Z =4, R = 0 0317, wR =0 0820. Compound 2 belongs to triclinic system with space group P 1, a =0 85592(17) nm, b =0 93016(19) nm, c =1 6368(3) nm, α =83 76(3)°, β =82 69(3)°, γ =78 05(3)°, V =1 2600(4) nm 3, Z = 2, R =0 0377, wR =0 1030.