收稿日期: 2008-10-07
修回日期: 2008-12-22
网络出版日期: 2009-05-15
基金资助
supported by National Natural Science Foundation of China (20571053)
Synthesis and characterization of fluorinated indium phosphate
Received date: 2008-10-07
Revised date: 2008-12-22
Online published: 2009-05-15
Supported by
supported by National Natural Science Foundation of China (20571053)
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InF2 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.
李兴亮 , 苏哲 , 李首建 . 氟化磷酸铟的合成与表征[J]. 中国科学院大学学报, 2009 , 26(3) : 310 -318 . DOI: 10.7523/j.issn.2095-6134.2009.3.004
A fluorinated indiumphosphate, InF2 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.
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