摘要
通过三苯基氢化锡与1-乙炔基茚满醇的加成反应,得到加成物(Z)-1-[2-(三苯基锡基)乙烯基]-1-茚满醇(Ⅰ).将加成物Ⅰ与相等物质的量的溴反应后,得到一溴代物(Z)-1-[2-(一溴二苯基锡基)乙烯基]-1-茚满醇(Ⅱ).通过元素分析、1HNMR和IR等手段对两个新型有机锡化合物进行了结构表征.用X射线单晶衍射测定了一溴代物Ⅱ的晶体结构.一溴代物Ⅱ具有分子内O→Sn[0.2370(2)nm]配位键,构成以Sn为中心的扭曲三角双锥构型.一溴代物Ⅱ属于单斜晶系:空间群为P2(1)/n;晶胞参数a=1.1891(2)nm,b=1.3586(3)nm,c=1.6403(3)nm,β=104.20(3)°,V=2.5689(9)nm-3,Z=4,Dc=1.505mg/m3,μ(MoKα)=2.567mm-1,F(000)=1168,最终可靠因子R1=0.0331,wR2=0.0719.
<Abstrcat>1-Ethynylindanol reacted with a triphenylltin hydride Ph3 SnH and generated the corresponding (Z)-1-[2-(triphenylstannyl)vinyl]-1-indanol (Ⅰ).The product obtained reacts with one equivalent of bromine to form the associated (Z)-1-[2-(bromodiphenylstannyl)- vinyl]-1-indanol (Ⅱ).The compounds were characterization by elemental analysis, 1 H NMR and FT-IR spectroscopy.The (solid-state) structures of compounds Ⅱ have been determined by X-ray diffraction analysis.A trigonal bipyramidal geometry is found in Ⅱ where the oxygen atom, which forms significant O→Sn interaction of (0.237 0(12) )nm, is in an apical position as is the bromine atom.Compound Ⅱ belongs monoclinic to with space group P2(1)/n,a=1.189 1(2)nm,b= 1.358 6(3)nm, c=1.640 3(3)nm, β=104.20(3)°,V= (2.568 9)(9)nm(-3), Z =4,Dc=1.505 mg/m3, μ(Mo Kα) = 2.567 mm(-1), F(000) = 1 168, R1=(0.033 1), wR2=0.071 9.
出处
《东北师大学报（自然科学版）》
CAS
CSCD
北大核心
2005年第2期63-66,共4页
Journal of Northeast Normal University(Natural Science Edition)
基金
国家自然科学基金资助项目(29734143
29672013)
关键词
有机锡
三苯基氢化锡
合成
晶体结构
organotin
phenyltin hydride
synthesis
crystal structure
