摘要
甲醇和水混合溶剂中,邻羟基苯乙酮缩氨基硫脲(L=C9H11N3OS)和乙酰丙酮氧钒VO(acac)2,在醋酸钠存在下反应,得到一种新颖的二维层状超分子配合物[VO(acac)2(H2O)].(C9H11 N3OS).通过红外光谱和X-射线单晶衍射对其进行结构表征.该晶体属三斜晶系,P1-空间群,晶胞参数为:a=0.780 87(9)nm,b=1.232 82(13)nm,c=1.337 4(2)nm,α=108.708(8)°,β=91.299(8)°,γ=107.652(6)°,V=1.151 7(3)nm3,Z=2,Dc=1.420 g.cm-3,μ=0.565 mm-1,F(000)=514,R1=0.051 6,ωR2=1.102 2.其中钒中心为六配位的近乎理想的八面体构型.通过氢键和π-π相互作用形成独特的二维层状超分子结构.同时研究了该配合物的荧光性质和热稳定性.CCDC:764394.
A novel 2D supramolecular complex ·(C9H11N3OS) was synthesized by the reaction of 2-hydroxyacetophenone thiosemicarbazone,vanadyl acetylacetonate,sodium acetate,in a mixed of methanol and water.The crystal structure of title compound was reported by X-ray diffraction.The crystal is of triclinic,space group P1-with unit cell parameters:a=0.780 87(9)nm,b=1.232 82(13)nm,c=1.337 4(2)nm,α=108.708(8)°,β=91.299(8)°,γ=107.652(6)°,V=1.151 7(3) nm3,Z=2,Dc=1.420 g·cm-3,μ=0.565 mm-1,F(000)=514,R1=0.0516,ωR2=1.1022.The coordination geometry of the V(Ⅳ) atom was a ideal octahedral configuration.The complex are assembled by hydrogen bonds and π-π interactions into a 2D layer supramolecular structure.The luminescent and TGA properties of the complex have been further studied and discussed.CCDC:764394.
出处
《首都师范大学学报(自然科学版)》
2011年第6期32-36,共5页
Journal of Capital Normal University:Natural Science Edition
基金
北京市教育委员会科技发展计划面上项目(No.KM200910028011)
关键词
钒(Ⅳ)配合物
缩氨基硫脲
超分子
晶体结构
vanadium(Ⅳ) complex
thiosemicarbazone
supermolecular
crystal structural