High-throughput and in situ EDXRD investigation on the formation of two new metal aminoethylphosphonates - Ca(O₃PC₂H₄NH₂) and Ca(OH)(O₃PC₂H₄NH₃)路2H₂O

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• 作者：Corinna Schmidt^a ; Mark Feyand^a ; André ; Rothkirch^b ; Norbert Stock^a ; ^{stock@ac.uni-kiel.de}
• 关键词：Crystal growth ; In situ EDXRD ; Solvothermal ; High-throughput ; Crystal structure
• 刊名：Journal of Solid State Chemistry
• 出版年：2012
• 期刊代码：130_00224596
• 类别：ch
• 出版时间：April, 2012
• 卷：188
• 期：Complete
• 页码：44-49
• 文件大小：844 K

摘要

The system Ca²⁺/2-aminoethylphosphonic acid/H₂O/NaOH was systematically investigated using high-throughput methods. The experiments led to one new compound Ca(O₃PC₂ H₄NH₂) (1) and the crystal structure was determined using in house X-ray powder diffraction data (monoclinic, P2₁/c, a=9.7753(3), b=6.4931(2), c=8.4473(2) 脜, 尾=106.46(2)掳, V=514.20(2) 脜³, Z=4). The formation of 1 was investigated by in situ energy dispersive X-ray diffraction measurements (EDXRD) at beamline F3 at HASYLAB (light source DORIS III), DESY, Hamburg. An intermediate, Ca(OH)(O₃PC₂H₄NH₃)路2H₂O (2), was observed and could be isolated from the reaction mixture at ambient temperatures by quenching the reaction. The crystal structure of 2 was determined from XRPD data using synchrotron radiation (monoclinic, P2₁/m, a=11.2193(7), b=7.1488(3), c=5.0635(2) 脜, 尾=100.13(4)掳, V=399.78(3) 脜³, Z=2).