摘要
在p H≈6.5及稀土盐的存在下,用Na_(2)WO_(4)·2 H_(2)O与Na As O_(2)及Co(NO_(3))_(2)·6 H_(2)O反应,得到了夹层型杂多钨酸盐Na9[Na_(3){Co(H_(2)O)}_(3)(As W_(9)O_(33))_(2)]·44H_(2)O单晶,用X射线单晶衍射法及元素分析确定了其结构,晶胞参数为:a=1.4083(6)nm,b=2.3241(6)nm,c=3.2197(10)nm,α=90°,β=98.995(6)°,γ=90°,V=10.408(6)nm^(3),Z=4,空间群C2/c,R_(1)=0.0604,w R_(2)=0.0792(I>2σ).[Na_(3){Co(H_(2)O)}_(3)(As W_(9)O_(33))_(2)]^(9-)具有近似D3 h对称性,Co^(2+)的配位数均为5.对题示化合物进行了IR,UV-Vis表征。
The novel sandwich heteropolytungstate Na 9[Na 3{Co(H 2O)}3(AsW 9O 33)2]·44H 2O is obtained by the reaction of Na 2WO 4·2H 2O with NaAsO 2 and Co(NO 3)2·6H 2O under pH≈6.5 and in the existence of rare-earth salt.Its structure is determined by X-ray diffraction analysis and element analysis.The cell parameters are as follows:a=1.4083(6)nm,b=2.3241(6)nm,c=3.2197(10)nm,α=90°,β=98995(6)°,γ=90°,V=10.408(6)nm 3,Z=4;space group:C 2/c,R1=0.0604,wR2=0.0792(I>2σ).X-ray diffraction analysis determined all non-hydrogen atomic coordinates.The structure of[Na 3{Co(H 2O)}3(AsW 9O 33)2]9-reveals a sandwich-like arrangement of two{α-β-AsW 9}moieties enclosing three Na+and three Co(H 2O)2+[Na 3{Co(H 2O)}3(AsW 9O 33]29-has an approximate D 3h symmetry.The coordination numbers of all CO 2+ions in the sandwich anion are five.
出处
《西安石油学院学报(自然科学版)》
2002年第4期66-69,共4页
Journal of Xi'an Petroleum Institute(Natural Science Edition)
基金
陕西省化学反应工程重点实验室开放基金
陕西省教委专项基金资助项目(99JK305)
关键词
杂多钨酸盐
晶体结构
钴
砷
钨
heteropolytungstate
crystal structure
cobalt
arsenic
tungsten