TY - DATA T1 - Exploiting the Synergy of Powder X‑ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids PY - 2015/12/16 AU - Dmytro V. Dudenko AU - P. Andrew Williams AU - Colan E. Hughes AU - Oleg N. Antzutkin AU - Sitaram P. Velaga AU - Steven P. Brown AU - Kenneth D. M. Harris UR - https://acs.figshare.com/articles/dataset/Exploiting_the_Synergy_of_Powder_X_ray_Diffraction_and_Solid_State_NMR_Spectroscopy_in_Structure_Determination_of_Organic_Molecular_Solids/2024055 DO - 10.1021/jp4041106.s002 L4 - https://ndownloader.figshare.com/files/3595350 KW - 13 C chemical shifts KW - crystal structure KW - Organic Molecular SolidsWe report KW - approach KW - GIPAW KW - powder XRD data KW - NMR data KW - 1 H KW - structure determination N2 - 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. ER -