摘要
报道了 α－Ｋｅｇｇｉｎ型（ＮＨ４）４ＨＰＷ１０Ｖ２Ｏ４０·２．５Ｈ２Ｏ的水热合成方 法，采用Ｘ－ｒａｙ单晶衍射测定了晶体结构．结构分析表明：该晶体属于三斜晶 系，空间群为 Ｐ１－，晶胞参数： α＝ １． ３２２ ３（３）ｎｍ， ｂ＝１．３２４ ３（３）ｎｍ， ｃ＝ １． ３２５ ３ （３）ｎｍ，α＝７５．９８（３）°，β＝７５．９９（３）°，γ＝７６．０６（３）°，Ｚ＝２，Ｒ１（ｗＲ２）＝ ０．０８１２（０．１９８ ０）．杂多酸阴离子作为一个整体是有序 α—Ｋｅｇｇｉｎ结构，但由 于异构体存在，钨和钒原子在晶体学上无序分布在１２个配原子位置上，钒在每 个配原子位置上占有率并不相等，平均值为０．１６７，总占有率为２．００．元素分 析、热重分析、ＵＶ、 ＩＲ、３１Ｐ ＮＭＲ光谱支持单晶 Ｘ— ｒａｙ衍射结果．
It has been reported that the title compound was synthesized by a hydrothermal method and structurally characterized by single crystal x-ray diffraction. The crystal data were shown below: triclinic, space grouppP1- ,α= 1. 322 3 (3) nm, b = 1. 324 3 (3 )nm, c = 1. 325 3(3) nm, α= 75. 98(3)°, β= 75. 99(3)°, γ= 76. 06(3)°, Z = 2, R1 (wR2) = 0. 081 2(0. 1980). Although the heteropolyanion is ordered α-Keggin structure, W and V atonｓ are disorderly distributed in 12 addenda atomｓ crystallographically. The occupation probability of V on each addenda atom is unequal, the mean value is 0. 167 and the total probability on anion is 2. 00. The result was supported by elemental analysis, thermogravimetric analysis, UV-Vis, IR,31P NMR spectra.
出处
《分子科学学报》
CAS
CSCD
2000年第2期77-81,共5页
Journal of Molecular Science
基金
国家自然科学基金29471008
关键词
结构
水热合成
多金属氧酸盐
钨钒磷杂多酸盐
crystal structure
hydrothermal synthesis
polyoxometalate
tongstovan adophosphate
