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Quantitative Structural Constraints for Organic Powders at Natural Isotopic Abundance Using Dynamic Nuclear Polarization Solid‐State NMR Spectroscopy
Author(s) -
Mollica Giulia,
Dekhil Myriam,
Ziarelli Fabio,
Thureau Pierre,
Viel Stéphane
Publication year - 2015
Publication title -
angewandte chemie
Language(s) - English
Resource type - Journals
eISSN - 1521-3757
pISSN - 0044-8249
DOI - 10.1002/ange.201501172
Subject(s) - nuclear magnetic resonance spectroscopy , crystal structure , solid state nuclear magnetic resonance , density functional theory , spectroscopy , chemistry , polarization (electrochemistry) , carbon 13 nmr , two dimensional nuclear magnetic resonance spectroscopy , single crystal , crystal structure prediction , carbon 13 nmr satellite , materials science , analytical chemistry (journal) , crystallography , computational chemistry , fluorine 19 nmr , nuclear magnetic resonance , organic chemistry , stereochemistry , physics , quantum mechanics
A straightforward method is reported to quantitatively relate structural constraints based on 13 C– 13 C double‐quantum build‐up curves obtained by dynamic nuclear polarization (DNP) solid‐state NMR to the crystal structure of organic powders at natural isotopic abundance. This method relies on the significant gain in NMR sensitivity provided by DNP (approximately 50‐fold, lowering the experimental time from a few years to a few days), and is sensitive to the molecular conformation and crystal packing of the studied powder sample (in this case theophylline). This method allows trial crystal structures to be rapidly and effectively discriminated, and paves the way to three‐dimensional structure elucidation of powders through combination with powder X‐ray diffraction, crystal‐structure prediction, and density functional theory computation of NMR chemical shifts.