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Chapter 2

High-resolution 1H 2D Magic-angle Spinning Techniques for Organic Solids

This practical guide outlines how 1H MAS NMR experiments are applied in our laboratory for the analysis of solid-state structures adopted by small and moderately sized organic solids at natural isotopic abundance. The power of such MAS NMR experiments for probing intermolecular interactions, such as hydrogen bonding, ππ and CH–π interactions, is demonstrated, for example for pharmaceuticals and in supramolecular self-assembly. The focus is on two-dimensional homonuclear [1H double-quantum (DQ) and spin diffusion (NOESY) experiments] and heteronuclear (dipolar-based 1H–13C CP HETCOR and 14N–1H HMQC and J-based 1H–13C refocused INEPT) experiments. The alternative approaches for obtaining 1H high resolution by either brute-force fast MAS or homonuclear 1H decoupling under moderate MAS are presented. Recoupling techniques that reintroduce homonuclear or heteronuclear dipolar couplings are described. The advantage of combining the different MAS NMR experiments with insight from complementary experimental techniques, notably powder X-ray diffraction, as well as the calculation of NMR parameters using the GIPAW method is emphasised.

Print publication date: 09 Apr 2018
Copyright year: 2018
Print ISBN: 978-1-78262-854-5
PDF eISBN: 978-1-78801-046-7
ePub eISBN: 978-1-78801-419-9
From the book series:
New Developments in NMR