jp4041106_si_002.cif (13.19 kB)
Exploiting the Synergy of Powder X‑ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids
dataset
posted on 2015-12-16, 23:00 authored by Dmytro V. Dudenko, P. Andrew Williams, Colan E. Hughes, Oleg N. Antzutkin, Sitaram
P. Velaga, Steven P. Brown, Kenneth D. M. HarrisWe 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.