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A fast magic-angle spinning three-dimensional NMR experiment for simultaneously probing H-H and N-H proximities in solids
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Reddy, G. N. Manjunatha, Malon, Michal, Marsh, Andrew, Nishiyama, Yusuke and Brown, Steven P. (2016) A fast magic-angle spinning three-dimensional NMR experiment for simultaneously probing H-H and N-H proximities in solids. Analytical Chemistry, 88 (23). pp. 11412-11419. doi:10.1021/acs.analchem.6b01869
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Official URL: http://dx.doi.org/10.1021/acs.analchem.6b01869
Abstract
A fast magic-angle spinning (MAS) solid-state NMR experiment is presented that combines 1H Double-Quantum (DQ) and 14N-1H HMQC (Heteronuclear Multiple-Quantum Coherence) pulse-sequence elements, so as to simultaneously probe H-H and N-H proximities in molecular solids. The proposed experiment can be employed in both two-dimensional (2D) and three-dimensional (3D) versions: firstly, a 2D 14N HMQC-filtered 1H-DQ experiment provides specific DQ-SQ correlation peaks for proton pairs that are in close proximities to the nitrogen sites, thereby achieving spectral filtration. Secondly, a proton-detected three-dimensional (3D) 1H(DQ)-14N(SQ)-1H(SQ) experiment correlates 1H(SQ)-1H(DQ) chemical shifts with 14N shifts such that longer range N…H-H correlations are observed between protons and nitrogen atoms with internuclear NH distances exceeding 3 Å. Both 2D and 3D versions of the proposed experiment are demonstrated for an amino acid hydrochloride salt, L-histidine.HCl.H2O, and a DNA nucleoside, guanosine.2H2O. In the latter case, the achieved spectral filtration ensures that DQ cross peaks are only observed for guanine NH and CH8 1H resonances and not ribose and water 1H resonances, thus providing insight into the changes in the solid-state structure of this hydrate that occur over time – significant changes are observed in the NH and NH2 1H chemical shifts as compared to the freshly recrystallized sample previously studied by Reddy et al, Cryst. Growth Des. 15, 5945, 2015.
| Item Type: | Journal Article | ||||||||||||||||||
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| Subjects: | Q Science > QD Chemistry | ||||||||||||||||||
| Divisions: | Faculty of Science > Chemistry Faculty of Science > Physics |
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| Library of Congress Subject Headings (LCSH): | Nuclear magnetic resonance spectroscopy, Self-assembly (Chemistry) | ||||||||||||||||||
| Journal or Publication Title: | Analytical Chemistry | ||||||||||||||||||
| Publisher: | American Chemical Society | ||||||||||||||||||
| ISSN: | 0003-2700 | ||||||||||||||||||
| Official Date: | 31 October 2016 | ||||||||||||||||||
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| Date of first compliant deposit: | 2 November 2016 | ||||||||||||||||||
| Volume: | 88 | ||||||||||||||||||
| Number: | 23 | ||||||||||||||||||
| Page Range: | pp. 11412-11419 | ||||||||||||||||||
| DOI: | 10.1021/acs.analchem.6b01869 | ||||||||||||||||||
| Status: | Peer Reviewed | ||||||||||||||||||
| Publication Status: | Published | ||||||||||||||||||
| Access rights to Published version: | Open Access | ||||||||||||||||||
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