氟化磷酸铟的合成与表征

以尿素与氯化胆碱的低共熔点液体同时兼做溶剂和模板传递剂,在离子热体系下合成了InF_{2 2}(NH₄)₃.采用同样的低共熔点液体在水热条件下不能得到相同的产物.产物晶体参数如下:C2/c(No.15)空间群,a=13.799(3) ,b=5.091(2) ,c=16.094(3) , β=112.942(16)°,V=1041.2(5) ³ and Z=4; R₁=0.0582,wR₂=0.1589. 在产物结构中,In八面体与P四面体形成四员环,顶角相连形成链状结构.客体铵分子填充于链与链间的空穴中,通过氢键与骨架中的F原子,P—OH和 P O 基团作用,链与链间靠范德华力吸引进而形成层状结构.产物进一步通过粉末XR, EDX, IR, XPS和TG/DTA进行表征.

Synthesis and characterization of fluorinated indium phosphate

A fluorinated indiumphosphate, InF_{2 2}(NH₄)₃, has been prepared under ionothermal condition using deep-eutectic solvents of choline chloride and urea as solvent and template-delivery agents. The same material can not be observed with the presence of the same deep-eutectic mixture under normal hydrothermal process. The compound crystallized in the monoclinic system, space group C2/c (No.15) with cell parameters a=13.799(3) , b=5.091(2) , c=16.094(3) , β=112.942(16)°, V=1041.2(5) ³ and Z=4; the final residual factors were R₁=0.0582 and wR 2=0.1589. The structure is built from an infinite chain composed of interconnected 4-member ring with formula of InF₂ ^3-₂. The guest ammonium are hydrogen bonded to the F atoms located in two outmost vertexes of indium octahedral and terminal P—OH and P O groups in the chain respectively. The integrated framework is formed by van der Waals forces holding the chains together as extensive H bond array exists in the compound. The further characterizations of the compound have been performed by X-ray powder diffraction, EDX, IR, XPS and TG/DTA analyses.