具有四配位铁中心的微孔磷酸铁晶体的溶剂热合成与表征

Solvothermal Synthesis and Characterization of A 3 D Iron Phosphate with Excluxively Four Coordinated Iron

在有机溶剂乙二醇中合成了具有三维骨架结构的磷酸铁晶体 ,对其进行了单晶结构解析 ,热重分析 ,穆斯堡尔谱以及红外光谱测试 ,证实晶体组成为 [NH3CH2 CH2 NH3]0 .5[FePO4 ],晶体结构属正交晶系 ,空间群Pc cn ,晶胞参数a =10 .36 1(6 ) ,b =10 .390 (5) ,c=9.135(7) ,V =983.3(11) 3,Z =8,Dc=2 .4 57Mg·m- 3,F(0 0 0 ) =72 8,R =0 .0 52 8,wR =0 .1194。在其结构中 ,磷氧四面体和铁氧四面体严格交替共用顶点在 [0 0 1]方向上形成八员环 ,双质子化的乙二胺分子占据八员环空隙。

A 3 D open framework iron phosphate [NH 3CH 2CH 2NH 3] 0.5 [FePO 4], which contains organic ethylenediammonium dication in the framework voids, has been synthesized under solvothermal conditions and has been characterized by single crystal diffraction, IR spectrum, Mssbauer spectroscopy and thermogravimetric analysis. The compound crystallizes in the orthorhombic space group with a =10.361(6)?, b =10.390(5)?, c =9.135(7)?, V =983.3(11)? 3,Z=8.The structure consists of corner sharing FeO 4 and PO 4 tetrahedra to form an open framework structure with eight membered ring channels along [001] direction. This new material was obtained by use of iron power as iron source in ethylene glycol solvent. The most important feather of the compound is that it contains four coordinated iron atoms which is very rare in iron phosphates.