X射线衍射单晶测试中晶体移位处理暨二亚胺衍生物结构解析研究

How to cope with the movement of crystals on the single-crystal X-ray diffraction and structure determination of the ethylenediamine derivative

X射线单晶衍射是测定晶体结构的有力手段。但是X射线单晶衍射测试对样品质量要求高,为达到足够的数据完整度测试时间长,期间容易出现意外情况如晶体发生移动或者变质,温度发生变化等。(2E,3E)-N^(2),N^(3)-二(4-甲基-2,6-二-((R)-1-苯乙基)苯基)丁烷-2,3-二亚胺晶体的X射线衍射测试被选取作为例子,详细阐述了X射线衍射测试过程中晶体意外移动的判断方法和应对手段,成功修正了数据并完成了结构精修,同时,第一次报道了该二亚胺衍生物晶体结构并上传剑桥晶体学数据库(CCDC索引号:2079144),并确认了产物R型绝对构型。

The single-crystal X-ray diffraction is a powerful method to determine the crystal structure.Meanwhile,the high quality of the crystal was required and several hours may be needed to achieve enough competence,which suffers from the accidental incidents such as crystal moving,decomposition or the instability of temperature control.In this work,the X-ray diffraction measurement and structure determination of(2E,3E)-N2,N3-bis(4-methyl-2,6-bis((R)-1-phenylethyl)phenyl)butane-2,3-diimine was practiced to elaborate the process of how to deal the crystal movement during the measurement.The structure of the ethylenediamine derivative was firstly reported and deposited to the Cambridge Crystal Database Centre(CCDC deposition number:2079144),and the absolute configuration R of the compound was confirmed.