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新型环形聚阴离子[{WO（H₂O）}₃(AsW₈O₃₁)3]^21-的结构及表征

A Novel Cyclic Heteropolyanion [{WO（H₂O）}₃(AsW₈O₃₁)3]²¹-

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【Author】 LIU, Bin a XUE, Gang-Lin ,a,c WANG, Ji-Wu b ZHAO , Jian-She a HE, Shui-Yang a SHI, Qi-Zhen a ( a Shaanxi Key Laboratory of Physico-Inorganic Chemistry, Department of C hemistry, Northwest University, Xi′an 710069) ( b Department of Chemistry and Chemical Engineering, Yan′an University, Y an′an 716000) ( c State Key Laboratory of Coordination Chemistry, Nanjing University, Nan jing 210093)

【机构】西北大学化学系陕西省物理无机化学重点实验室；延安大学化学化工学院陕西省化学反应工程重点实验室；西北大学化学系陕西省物理无机化学重点实验室西安710069；西安710069；南京大学化学系国家配位化学重点实验室南京210093；延安716000；西安710069；

【摘要】在pH =3 0的水溶液中 ,Na2 WO4·2H2 O与NaAsO2 ·6H2 O和NH4Cl反应 ,得到了新的杂多钨酸盐 (NH4) 19Na2 [{WO (H2 O) } 3(AsW8O3 1) 3]·45H2 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 =3 1165(11)nm ,b=1 73 88(7)nm ,c =2 2 789(9)nm ,β =97 3 4 2 (6)°,V =12 2 48(8)nm3,Z =4,R1=0 0 571,wR2 =0 0 741[I>2σ(I) ] .环型聚阴离子 [{WO(H2 O) } 3(AsW8O3 1) 3] 2 1- 是由三个 {WO(H2 O) }桥连三个新发现的 {AsW8O3 1}单元构成的 ,环聚离子 [{WO(H2 O) } 3(AsW8O3 1) 3] 2 1- 具有近似D3h对称性 .对该化合物还进行了183 WNMR ,IR和TG表征更多还原

【Abstract】 A novel heteropolyoxometalate (NH 4) 19 Na 2[{WO(H 2O)} 3(AsW 8O 31 ) 3]·45H 2O was synthesized by the reaction of Na 2WO 4·2H 2O with N aAsO 2·6H 2O and NH 4Cl 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 ) nm, β=97 342(6)°, V=12 248(8) nm 3, Z=4, R 1=0 0571, wR 2=0 0741 [I>2σ(I)]. The polyanion [{WO(H 2O)} 3(AsW 8O 3 1 ) 3] 21- consists of three new {AsW 8O 31 } subunits related thro ugh a C 3 axis and joined up by three extra {WO(H 2O)} group. Each {WO(H 2O)} joints two AsW 8O 31 subunits by sharing two cis oxygen atoms wit h each other, the polyanion [{WO(H 2O)} 3(AsW 8O 31 ) 3] 21- has approximately D 3h symmetry. The compound was also characterized by 183 W NMR, IR and TG.更多还原