De Novo Determination of the Crystal Structure of a Large Drug Molecule by Crystal Structure Prediction-Based Powder NMR Crystallography
De Novo Determination of the Crystal Structure of a Large Drug Molecule by Crystal Structure Prediction-Based Powder NMR Crystallography
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DOI：
10.1021/ja4088874
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发表时间：
2013-11-20
影响因子：
15
通讯作者：
Emsley, Lyndon
中科院分区：
文献类型：
--
作者：
Baias, Maria;Dumez, Jean-Nicolas;Emsley, Lyndon
药物4-[4-（2-金刚烷基氨基甲酰基）-5-叔丁基-吡唑-1-基]苯甲酸的晶型4的晶体结构使用NMR粉末晶体学在天然同位素丰度下的方案结合固态H-1 NMR光谱、晶体结构预测和密度泛函理论化学位移计算来确定。这是对以前未知结构的分子化合物进行NMR晶体结构测定的第一个例子，并且在422 g/mol下，这是迄今为止应用该方法的最大化合物。
The crystal structure of form 4 of the drug 4-[4-(2-adamantylcarbamoyl)-5-tert-butyl-pyrazol-1-yl]benzoic acid is determined using a protocol for NMR powder crystallography at natural isotopic abundance combining solid-state H-1 NMR spectroscopy, crystal structure prediction, and density functional theory chemical shift calculations. This is the first example of NMR crystal structure determination for a molecular compound of previously unknown structure, and at 422 g/mol this is the largest compound to which this method has been applied so far.