Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids

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• 作者：Dmytro V. Dudenko ; P. Andrew Williams ; Colan E. Hughes ; Oleg N. Antzutkin ; Sitaram P. Velaga ; Steven P. Brown ; Kenneth D. M. Harris
• 刊名：The Journal of Physical Chemistry C
• 出版年：2013
• 出版时间：June 13, 2013
• 年：2013
• 卷：117
• 期：23
• 页码：12258-12265
• 全文大小：377K
• 年卷期：v.117,no.23(June 13, 2013)
• ISSN：1932-7455

文摘

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 p>1p>H and p>13p>C 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 p>1p>H and p>13p>C chemical shifts for directly bonded p>13p>C鈥?sup>1p>H 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.