摘要
合成并测定了十钒酸盐Ｎａ_６Ｖ_（１０）Ｏ_（２８）·１２Ｈ_２Ｏ的单晶结构。晶体属单斜晶系，Ｐ２_１／ｎ群空间，ａ＝１２．０１９（２），ｂ＝１７．１５４（２），ｃ＝１８．１７８（６），β＝１０６．２９（２）°，Ｖ＝３５７９（１），Ｍ_ｒ＝１２８７．５，Ｆ（０００）＝２５６０，μ＝２５，４４ｃｍ￣（－１），Ｚ＝４，Ｄ_ｃ＝２．３８ｇ·ｃｍ（－３）。结构由重原子法解出，全矩阵最小二乘法修正至Ｒ＝０．０６４，Ｒ_ｗ＝０．０８３。Ｖ_（１０）簇阴离子可以看成由１０个ＶＯ_６变形八面体形成，其中氧原子有４种类型：端氧、二桥氧、三桥氧和六桥氧。结果表明，阳离子相同但结晶水的数目不同时，十钒酸盐的晶系和空间群不同。
The title compound was synthesized from the system of NaOH-H_2MoO_4-HCl-V_2O_5.The crystals are monoclinic with space group P2_1/n and have a unit cell with a=12.019 (2) ,b=17.154(2),c= 18.178(6),β=106. 29(2)°,V=3579(1), M_r=1287.5,F(000) =2560,μ=25.44 cm￣(-1),Z=4,D_c= 2. 38 g·cm￣(-3). The structure was solved by heavy atomic method and refined by full-matrix least-squares method to R= 0. 064,R_w=0.083. The cluster anion is formed by 10 distorted VO_6 octahedra and there are four types of oxygen atoms: apical oxygen and three kinds of bridge oxygen atoms which are coordinated to two,three and six vanadium atoms respectively.
基金
国家自然科学基金委员会和结构化学国家重点实验室资助
