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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 international edition
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 5.831
H-Index - 550
eISSN - 1521-3773
pISSN - 1433-7851
DOI - 10.1002/anie.201501172
Subject(s) - crystal structure , solid state nuclear magnetic resonance , density functional theory , nuclear magnetic resonance spectroscopy , polarization (electrochemistry) , spectroscopy , chemistry , carbon 13 nmr , single crystal , two dimensional nuclear magnetic resonance spectroscopy , materials science , crystal structure prediction , analytical chemistry (journal) , crystallography , computational chemistry , 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.