摘要
以NH4VO3,H3PMo12O40·x H2O,Cu(NO3)2和哌嗪为主要原料,采用水热方法,合成了一个新的钼钒二聚体簇合物——(H2NC4H8NH2)6[MoVI16VV12P2O84]·5H2O(1),其结构和性能经UV-Vis,IR,X-射线衍射、光电子能谱及热重分析表征。1属单斜晶系,P2(1)/c空间群,晶胞参数a=20.450(4),b=24.989(5),c=20.450(4),β=93.89°,V=10 427(4)3,Fw=4 159.18,Dc=2.650 g·cm-3,μ=3.018 mm-1,F(000)=7 952,Gof=1.029。晶体结构解析表明:1由两个单元Keggin型簇核[PMo8V6O42]7-聚合而成一个二聚体簇[P2Mol6V12O84]14-,该二聚体簇核和有机配体哌嗪之间通过复杂的氢键相互作用,展示三维超分子网络结构。
The novel polyoxometalate,( H2NC4H8NH2)6[MoVI16VV12P2O84]·5H2O( 1),was hydrothermally synthesized using NH4VO3,H3PMo12O40·x H2 O,Cu( NO3)2and piperazine as the starting materials. The structure and properties were characterized by UV-Vis,IR,XRD,XPS spectra and TG analysis. 1 belongs to monoclinic system,space group P2( 1) / c with a = 20. 450( 4) ,b = 24. 989( 5) ,c = 20. 450( 4) ,β = 93. 89 °,V = 10 427( 4) 3,Fw = 4 159. 18,Dc = 2. 650 g·cm- 3,μ = 3. 018 mm- 1,F( 000) = 7 952,Gof = 1. 029. The results showed that the polyanion [P2Mol6V12O84]14-was a dipolymer formed by two [PMo8V6O42]7-units. 1 exhibited a novel 3-D supramolecular arrays constructed from dipolymer anions and organic ligands via hydrogen bonds.
出处
《合成化学》
CAS
CSCD
2016年第1期51-54,62,共5页
Chinese Journal of Synthetic Chemistry
基金
吉林省科技厅项目(20130101033JC)
关键词
水热合成
金属氧簇
钼钒二聚体
晶体结构
性能
hydrothermal synthesis
polyoxometalate
Mo-V dipolymer
crystal structure
property
