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机构地区:[1]河南大学化学化工学院,河南省多酸化学重点实验室,河南开封475004
出 处:《化学研究》2014年第1期1-7,共7页Chemical Research
基 金:Supported by the Natural Science Foundation of China(21101055,21301049,U1304208);the Natural Science Foundation of Henan Province(122300410106);the Foundation of Education Department of Henan Province(2010B150006);the Students Innovative Pilot Plan of Henan University(2012,2013)
摘 要:在常温水溶液条件下,合成了一种二维四核铁取代夹心型锑钨酸盐NdNa3[Fe4(H2O)10][β-B-SbW9O33]2·36H2O(1),并通过IR光谱和单晶X射线衍射对其进行了表征.化合物1属于三斜晶系,P-1空间群,晶胞参数:a=1.264 8(3)nm,b=1.270 1(3)nm,c=1.616 0(4)nm,α=74.467(4)°,β=77.592(4)°,γ=83.658(4)°,V=2.438 9(9)nm3,Z=1,Dc=4.000g/cm3,GOOF=1.047,R1=0.065 6,wR2=0.162 2.X射线单晶结构分析表明,化合物1的多阴离子由两个相同的三缺位Keggin[β-B-SbW9O33]9-单元通过四个八面体配位的铁离子连接而成.四个FeO6八面体没有直接相连,四个FeIII离子可以分为两组:内部的FeIII离子带有两个水配体,而外部的FeIII离子连有三个水配体.邻近二聚多阴离子通过无序的钠/钕桥配离子构筑了二维层结构.A 2-D tetra-FeIII substituted sandwich-type antimonotungstate NdNa3[Fe4(H2O)10][β-SbW9O33]2·36H2O(1) was prepared under the conventional aqueous solution condition and characterized by IR spectrum and single-crystal X-ray diffraction. I crystallizes in the triclinic space group P-1 with a = 1.264 8(3) nm, b = 1.270 1(3) rim, c = 1.616 0(4) nm, α=74.467(4)°,β=77.592(4)°,γ=83.658(4)°,V=2.4389(9)nm3,Z=1,Dc=4.000g/cm3,G00F-1.047,R1=0.0656,wR2=0.1622. X-ray structure analysis reveals that 1 contains a dimeric polyoxoanion constructed from two identical trivacant Keggin [β-B-SbW9O38]9- units linked via four octahedral FeIII cations. There is no direct connection among four FeO6 octahedra. Four FeIII cations can be divided into two inequivalent pairs: the inner Fem cations have two terminal water ligands while the outer FenI cations own three terminal water ligands. Adjacent dimeric polyoxoanions are connected together through disordered Na/Nd bridges giving rise to a 2-D sheet structure.
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