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有机杂化锡硫化合物[Ni(tepa)]_2(μ_2-Sn_2S_6)的溶剂热合成及晶体结构

Solvothermal Synthesis and Crystal Structure of Organic-hybrid Thiostannate [Ni(tepa)]_2(μ_2-Sn_2S_6)
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摘要 利用溶剂热法合成了有机杂化锡硫化合物[Ni(tepa)]2(μ2-Sn2S6)(1,tepa=四乙烯五胺),其结构和光吸收特性经IR,元素分析和UV表征,晶体结构由X-射线单晶衍射仪测定。1属于四方晶系,空间群为I41/a,晶胞参数:a=0.909 0(17)nm,b=1.305 1(2)nm,c=1.299 2(2)nm,β=92.918(4)°,V=1.539 3(5)nm3,Z=4,Mr=462.89 g.mol-1,Dc=1.997 g.cm-3,μ=3.243 mm-1,F(000)=928,R1=0.070 2,wR2=0.151 2[I>2σ(I)],S=1.075。1中Ni2+离子与tepa配体的5个N原子和[Sn2S6]4-阴离子的一个端基S原子配位,形成了畸变八面体几何构型。[Sn2S6]4-阴离子作为桥连配体,通过端基S原子与[Ni(tepa)]2+配阳离子连接形成了中性的中心对称化合物[Ni(tepa)]2(μ2-Sn2S6)。 Thiostannate, [ Ni (tepa) ] 2 (μ2-Sn2S6 ) ( 1, tepa = tetraethylenepentamine ), was synthesized by solvothermal method. The structure of 1 was characterized by UV, IR and elemental analysis. The crystal structure of 1 was determined by single crystal X-ray diffraction. 1 belongs to the tetragonal system, space group I41/a witha=0.909 0(17)nm,b=1.305 1(2)nm,c=1.299 2(2)nm,β=92.918(4)°,V=1.539 3(5)nm^3,Z=4,Mr=462.89 g.mol^-1,Dc=1.997 g.cm^-3,μ=3.243 mm^-1,F(000)=928,R1=0.070 2,wR2=0.151 2[I〉2σ(I)],S=1.075. Ni^2+ ion is coordinated by five N atoms from a tepa ligand and one S atom of [ Sn2S6]4- anion, forming a slightly distorted octahedron. [ Sn2S6 ] 4- anion acts as a bidentate bridging ligand connecting two transition metal complex cations by trans terminal S atoms to form the neutral centrosymmetric [ Ni (tepa)] 2 (μ2-Sn2S6).
出处 《合成化学》 CAS CSCD 2007年第3期324-326,361,共4页 Chinese Journal of Synthetic Chemistry
基金 广西教育厅基金资助项目(200607216) 南京大学配位化学重点实验室开放基金资助项目
关键词 溶剂热法 锡硫化合物 晶体结构 合成 solvothermal method thiostannate crystal structure synthesis
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参考文献11

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