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Temperature Controlling Polymorphism and Polymorphic Interconversion in Sublimation Crystallization of 5-Methoxy-salicylaldhyde Azine

机译:温度控制多态性和5-甲氧基 - 水杨醛吡啶胺升华结晶的多态性和多态性互连

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摘要

Traditional growth of organic crystals is mostly based on solution processing techniques, but facile crystal preparation of compounds with poor solubility or polymorphic characters remains a challenge. Here, we demonstrate an in-air sublimation method for strategical preparation of 5-methoxy-salicylaldhyde azine (compound 1) in two polymorphic crystal forms by controlling sublimation temperature. The kinetically stable form was offered under 180 degrees C with the opposite orientation of methoxy group with respect to the longest chain in the molecule (termed 1-anti), while the thermodynamically stable one was offered above 200 degrees C with that in same orientation (termed 1-syn). Moreover, the overall dynamic forming and interconversion between 1-anti and 1-syn crystals in the sublimation process were well-studied by powder X-ray diffraction, IR, emission spectra, and DFT calculations. All the results revealed that this sublimation crystallization technique should be helpful for detection and even selective preparation of pure organic crystals with polymorphic characters.
机译:有机晶体的传统生长主要是基于溶液加工技术,但溶解度差或多晶特性的化合物的容易晶体制备仍然是一个挑战。这里,我们通过控制升华温度,证明了一种以两种多态性晶体形式的5-甲氧基 - 水杨醛氮(化合物1)的拓展方法。在180℃下提供动力学稳定的形式,相对于分子中最长链(称为1-抗)的甲氧基相对取向,而热力学稳定的同时以相同的取向(称为1-SYN)。此外,通过粉末X射线衍射,红外线,发射光谱和DFT计算研究了升华过程中的1-抗和1-SYN晶体之间的总体动态形成和相互互连。所有结果表明,这种升华结晶技术应该有助于检测甚至用多态特征选择纯有机晶体的选择性制备。

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  • 来源
    《Crystal growth & design》 |2019年第1期|共8页
  • 作者单位

    Nanchang Univ Inst Adv Study Nanchang 330031 Jiangxi Peoples R China;

    Nanchang Univ Inst Adv Study Nanchang 330031 Jiangxi Peoples R China;

    Nanchang Univ Inst Adv Study Nanchang 330031 Jiangxi Peoples R China;

    Nanchang Univ Inst Adv Study Nanchang 330031 Jiangxi Peoples R China;

    Nanchang Univ Inst Adv Study Nanchang 330031 Jiangxi Peoples R China;

    Nanchang Univ Inst Adv Study Nanchang 330031 Jiangxi Peoples R China;

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  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 晶体学;
  • 关键词

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