Computation of magnetic shielding to simultaneously validate a crystal structure and assign a solid-state NMR spectrum
Computation of magnetic shielding to simultaneously validate a crystal structure and assign a solid-state NMR spectrum
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DOI：
10.1016/j.molstruc.2011.10.024
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发表时间：
2012-05-16
影响因子：
3.8
通讯作者：
Jochym, Dominik B.
中科院分区：
文献类型：
--
作者：
Apperley, David C.;Batsanov, Andrei S.;Jochym, Dominik B.
用C-13固体核磁共振结合屏蔽计算验证了剑桥晶体数据库(代码为ZIYXAG)中硫酸二特布他林二乙酸酯的结构的有效性，发现关于一个醋酸分子的几何构型是错误的。一项新的X射线衍射研究证实了错误的存在，并表明存在问题的分子中存在无序。核磁共振结晶学技术被用来进一步了解情况。二维(C-13，H-1)异核关联实验能够确定H-1的化学位移，包括氢键质子的化学位移。还用核磁共振监测了部分脱溶，并报道了一种新的溶剂--硫酸二特布他林单乙酸的C-13谱。对这种新化合物的异核相关实验可以测定它的大部分质子化学位移，并表明它有一个比在二醋酸溶剂中的氢键更强的氢键。(C)2011爱思唯尔B.V.保留所有权利。
The validity of the structure of diterbutaline sulphate diacetic acid solvate in the Cambridge Crystallographic Database (code ZIYXAG) was checked using C-13 solid-state NMR together with shielding computations and was found to be in error as far as the geometry of one acetic acid molecule is concerned. A new X-ray diffraction study confirmed the existence of an error and showed there was disorder in the molecule in question. Techniques of NMR crystallography were used to further understand the situation. Two-dimensional (C-13, H-1) heteronuclear correlation experiments enabled the H-1 chemical shifts to be determined, including those of the hydrogen-bonded protons. NMR was also used to monitor partial desolvation and the C-13 spectrum of a new solvate, diterbutaline sulphate monoacetic acid, is reported. Heteronuclear correlation experiments on this new compound allowed most of its proton chemical shifts to be determined and showed that it had one hydrogen bond stronger than any of those in the diacetic acid solvate. (C) 2011 Elsevier B.V. All rights reserved.