鼓形有机锡氧杂环羧酸簇合物[PhCH2Sn(O)(O2CC4H3S)]6·2CH2Cl2 和 [PhCH2Sn(O)(O2CC3H2NO)]6·2CH2Cl2的合成和晶体结构

利用三苄基氧化锡与2-噻吩甲酸和2-唑甲酸反应,合成了六聚体苄基锡氧2-噻吩甲酸酯(1)和六聚体苄基锡氧2-唑甲酸酯(2)鼓形簇合物.通过元素分析、红外光谱和X射线单晶衍射对其结构进行了表征.测试结果表明:化合物1属三斜晶系,空间群p1,a=1.2760(3)nm,b=1.3056(3)nm,c=1.3343(3)nm,α=105.65(3)°,β=96.27(3)°,γ=97.20(3)°,Z=1,V=2.0997(7)nm3,Dc=1.809g/cm3,μ=2.097mm-1,F(000)=1116,R=0.0651,wR=0.1292.化合物2属三斜晶系,空间群p1,a=1.2240(4)nm,b=1.3673(4)nm,c=1.3744(4)nm,α=107.760(4)°,β=98.069(5)°,γ=91.480(5)°,Z=2,V=2.1631(12)nm3,Dc=3.373g/cm3,μ=3.799mm-1,F(000)=2136,R=0.0382,wR=0.079.它们均为鼓形簇状结构,锡原子呈畸变的八面体构型.化合物1通过分子间S…S近距离作用,形成一维链状结构.

Synthesis and Crystal Structure of Drum Organooxotin Clusters from Hetero-aromatic Carboxylic Acid [PhCH2Sn(O)(O2CC4H3S)]6·2CH2Cl2 and [PhCH2Sn(O)(O2CC3H2NO)]6·2CH2Cl2

Two novel drum organooxotin clusters PhCH2Sn(O)(O2CC4H3S)]6·2CH2Cl2(1) and PhCH2Sn(O)(O2CC3H2NO)]6·2CH2Cl2(2) were synthesized by the reaction of (PhCH2)3Sn]2O with 2-thiophenecarboxylic acid and 2-oxazoliylcarboxylcarboxylic acid in 1;2 molar ratio. Their crystal structures were determined by X-ray single crystal diffraction. Crystal 1 belongs to triclinic system with space group p1, a=1.276 0(3) nm, b=1.305 6(3) nm, c=1.334 3(3) nm, α= 105.65(3)°, β=96.27(3)°, γ=97.20(3)°, Z=1, V=2.099 7(7) nm3, Dc=1.809 g/cm3, μ=2.097mm-1, F(000)=1 116, R=0.065 1, wR=0.129 2. Crystal 2 belongs to triclinic system with space group p1, a=1.224 0(4) nm,b=1.367 3(4) nm, c=1.374 4(4) nm, α=107.760(4)°, β=98.069(5)°, γ=91.480(5)°, Z=2, V=2.163 1(12) nm3, Dc=3.373 g/cm3, μ=3.799mm-1, F(000)=2 136, R=0.038 2, wR= 0.079. Their structures show a distorted octahedron configuration with six-coordination for the central tin atoms. In crystal 1, the molecules are packed in the unit celLIn one-dimensional chain structure through weak interaction between the sulfur atom and one of the sulfur of an adjacent molecule.