Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids.
Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids.
复制标题
利用粉末X射线衍射和固态NMR光谱的协同作用在有机分子固体的结构测定中。
DOI：
10.1021/jp4041106
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发表时间：
2013-06-13
期刊：
影响因子：
--
通讯作者：
Harris KD
中科院分区：
文献类型：
--
作者：
Dudenko DV;Williams PA;Hughes CE;Antzutkin ON;Velaga SP;Brown SP;Harris KD
我们报告了一种用于有机材料结构测定的策略，其中完整的固态核磁共振（NMR）光谱数据在粉末X射线衍射（XRD）数据的结构测定范围内被利用。根据粉末XRD数据确定晶体结构后，利用GIPAW方法中基于第一性原理密度泛函理论的技术计算结构的固态NMR数据，然后仔细检查与实验固态NMR数据的一致性。吲哚美辛和烟酰胺的1：1共晶的结构测定证明了这种方法的成功应用。从粉末XRD数据确定的晶体结构计算的1H和13 C化学位移与实验测量的那些非常一致，特别是包括直接键合的13 C-1H部分的1H和13 C化学位移的二维相关性。这种组合方法的关键特征是，根据实验粉末XRD数据和实验固态NMR数据来评估所确定的结构的质量，从而提供了对结构准确性的非常稳健的验证。
We report a strategy for structure determination of organic materials in which complete solid-state nuclear magnetic resonance (NMR) spectral data is utilized within the context of structure determination from powder X-ray diffraction (XRD) data. Following determination of the crystal structure from powder XRD data, first-principles density functional theory-based techniques within the GIPAW approach are exploited to calculate the solid-state NMR data for the structure, followed by careful scrutiny of the agreement with experimental solid-state NMR data. The successful application of this approach is demonstrated by structure determination of the 1:1 cocrystal of indomethacin and nicotinamide. The 1H and 13C chemical shifts calculated for the crystal structure determined from the powder XRD data are in excellent agreement with those measured experimentally, notably including the two-dimensional correlation of 1H and 13C chemical shifts for directly bonded 13C–1H moieties. The key feature of this combined approach is that the quality of the structure determined is assessed both against experimental powder XRD data and against experimental solid-state NMR data, thus providing a very robust validation of the veracity of the structure.
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