摘要
在pH=30的水溶液中,Na_(2)WO_(4)·2H_(2)O与NaAsO_(2)·6H_(2)O和NH_(4)Cl反应,得到了新的杂多钨酸盐(NH_(4))_(19)Na_(2)[{WO(H_(2)O)}_(3)(AsW_(8)O_(31))_(3)]·45H_(2)O单晶,用X射线单晶衍射法及元素分析确定了其结构,晶体属单斜晶系,空间群C2/c,晶胞参数为:a=31165(11)nm,b=17388(7)nm,c=22789(9)nm,β=97342(6)°,V=12248(8)nm^(3),Z=4,R1=00571,wR_(2)=00741[I>2σ(I)].环型聚阴离子[{WO(H_(2)O)}_(3)(AsW_(8)O_(31))_(3)]^(21-)是由三个{WO(H_(2)O)}桥连三个新发现的{AsW_(8)O_(31)}单元构成的,环聚离子[{WO(H_(2)O)}_(3)(AsW_(8)O_(31))_(3)]^(21-)具有近似D3h对称性.对该化合物还进行了^(183)WNMR,IR和TG表征。
A novel heteropolyoxometalate(NH_(4))_(19)Na_(2)[{WO(H_(2)O)}_(3)(AsW_(8)O_(31))_(3)].45H_(2)O was synthesized by the reaction of Na_(2)WO_(4).2H_(2)O with NaAsO_(2).6H_(2)O and NH_(4)Cl in pH=3.0 aqueous solution.The single crystal X-ray diffraction study shows that the crystal belongs to monoclinic system,space group C2/c,with a 3.1165(11)nm,b=1.7388(7)nm,c=2.2789(9)mn,beta=97.342(6)degrees,V=12.248(8)nm^(3),Z=4,R,0.0571,wR_(2)=0.0741[I>2sigma(1)].The polyanion[{WO(H_(2)O)}_(3)(AsW_(8)O_(31))_(3)]^(21-)consists of three new{AsW_(8)O_(31)}subunits related through a C-3 axis and joined up by three extra{WO(H_(2)O)}group.Each{WO(H_(2)O)}joints two AsW_(8)O_(31) subunits by sharing two cis oxygen atoms with each other,the polyanion[{WO(H_(2)O)}_(3)(AsW_(8)O_(31))_(3)](21-)has approximately D-3h symmetry.The compound was also characterized by ^(183)W NMR,IR and TG.
作者
刘斌
薛岗林
王继武
赵建设
何水样
史启祯
LIU Bin;XUE Gang-Lin;WANG Ji-Wu;ZHAO Jian-She;HE Shui-Yang;SHI Qi-Zhen(Shaanzi Key Laboratory of Physico-Inorganic Chemistry,Department of Chemistry,Northwest University,Xi'an 710069;Department of Chemistry and Chemical Engineering,Yan'an University,Yan'an 716000;State Key Laboratory of Coordination Chemistry,Nanjing Univeersity,Nanjing 210093)
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
2003年第10期1608-1611,共4页
Acta Chimica Sinica
基金
高等学校重点实验室访问学者基金
陕西省化学反应工程重点实验室开放基金资助项目
关键词
杂多钨酸盐
晶体结构
钨
砷
heteropolytungstate
crystal structure
tungsten
arsenic
