Natural-abundance solid-state H-2 NMR spectroscopy at high magnetic field

Aliev, Abil E., Mann, Sam E., Iuga, Dinu, Hughes, Colan Evan and Harris, Kenneth David Maclean ORCID: https://orcid.org/0000-0001-7855-8598 2011. Natural-abundance solid-state H-2 NMR spectroscopy at high magnetic field. Journal of Physical Chemistry A 115 (22) , pp. 5568-5578. 10.1021/jp202810k

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Abstract

High-resolution solid-state 2H NMR spectroscopy provides a method for measuring 1H NMR chemical shifts in solids and is advantageous over the direct measurement of high-resolution solid-state 1H NMR spectra, as it requires only the application of routine magic angle sample spinning (MAS) and routine 1H decoupling methods, in contrast to the requirement for complex pulse sequences for homonuclear 1H decoupling and ultrafast MAS in the case of high-resolution solid-state 1H NMR. However, a significant obstacle to the routine application of high-resolution solid-state 2H NMR is the very low natural abundance of 2H, with the consequent problem of inherently low sensitivity. Here, we explore the feasibility of measuring 2H MAS NMR spectra of various solids with natural isotopic abundances at high magnetic field (850 MHz), focusing on samples of amino acids, peptides, collagen, and various organic solids. The results show that high-resolution solid-state 2H NMR can be used successfully to measure isotropic 1H chemical shifts in favorable cases, particularly for mobile functional groups, such as methyl and −N+H3 groups, and in some cases phenyl groups. Furthermore, we demonstrate that routine 2H MAS NMR measurements can be exploited for assessing the relative dynamics of different functional groups in a molecule and for assessing whole-molecule motions in the solid state. The magnitude and field-dependence of second-order shifts due to the 2H quadrupole interaction are also investigated, on the basis of analysis of simulated and experimental 1H and 2H MAS NMR spectra of fully deuterated and selectively deuterated samples of the α polymorph of glycine at two different magnetic field strengths.

Item Type:	Article
Status:	Published
Schools:	Chemistry
Subjects:	Q Science > QD Chemistry
Publisher:	ACS
ISSN:	1089-5639
Last Modified:	18 Oct 2022 13:11
URI:	https://orca.cardiff.ac.uk/id/eprint/12829

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