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Combining heteronuclear correlation NMR with spin-diffusion to detect relayed Cl–H–H and N–H–H proximities in molecular solids
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Raval, Parth, Trébosc, Julien, Pawlak, Tomasz, Nishiyama, Yusuke, Brown, Steven P. and Reddy, G. N. Manjunatha (2022) Combining heteronuclear correlation NMR with spin-diffusion to detect relayed Cl–H–H and N–H–H proximities in molecular solids. Solid State Nuclear Magnetic Resonance, 120 . 101808. doi:10.1016/j.ssnmr.2022.101808 ISSN 0926-2040.
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Official URL: https://doi.org/10.1016/j.ssnmr.2022.101808
Abstract
Analysis of short-to-intermediate range intermolecular interactions offers a great way of characterizing the solid-state organization of small molecules and materials. This can be achieved by two-dimensional (2D) homo- and heteronuclear correlation NMR spectroscopy, for example, by carrying out experiments at high magnetic fields in conjunction with fast magic-angle spinning (MAS) techniques. But, detecting 2D peaks for the heteronuclear dipolar coupled spin pairs separated by greater than 3 Å is not always straightforward, particularly when low-gamma quadrupolar nuclei are involved. Here, we present a 2D correlation NMR experiment that combines the advantages of heteronuclear-multiple quantum coherence (HMQC) and proton-based spin-diffusion (SD) pulse sequences using radio-frequency-driven-recouping (RFDR) to probe inter and intramolecular 1H-X (X = 14N, 35Cl) interactions. This experiment can be used to acquire 2D 1H{X}-HMQC filtered 1H–1H correlation as well as 2D 1H-X HMQC spectra. Powder forms of dopamine·HCl and l-histidine·HCl·H2O are characterized at high fields (21.1 T and 18.8 T) with fast MAS (60 kHz) using the 2D HMQC-SD-RFDR approach. Solid-state NMR results are complemented with NMR crystallography analyses using the gauge-including projector augmented wave (GIPAW) approach. For histidine·HCl·H2O, 2D peaks associated with 14N–1H–1H and 35Cl–1H–1H distances of up to 4.4 and 3.9 Å have been detected. This is further corroborated by the observation of 2D peaks corresponding to 14N–1H–1H and 35Cl–1H–1H distances of up to 4.2 and 3.7 Å in dopamine·HCl, indicating the suitability of the HMQC-SD-RFDR experiments for detecting medium-range proximities in molecular solids.
Item Type: | Journal Article | |||||||||||||||||||||||||||||||||
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Subjects: | Q Science > QC Physics Q Science > QD Chemistry |
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Divisions: | Faculty of Science, Engineering and Medicine > Science > Physics | |||||||||||||||||||||||||||||||||
Library of Congress Subject Headings (LCSH): | Nuclear magnetic resonance , Nuclear magnetic resonance spectroscopy, Crystallography, Solid state chemistry, Molecular crystals | |||||||||||||||||||||||||||||||||
Journal or Publication Title: | Solid State Nuclear Magnetic Resonance | |||||||||||||||||||||||||||||||||
Publisher: | Elsevier | |||||||||||||||||||||||||||||||||
ISSN: | 0926-2040 | |||||||||||||||||||||||||||||||||
Official Date: | August 2022 | |||||||||||||||||||||||||||||||||
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Volume: | 120 | |||||||||||||||||||||||||||||||||
Article Number: | 101808 | |||||||||||||||||||||||||||||||||
DOI: | 10.1016/j.ssnmr.2022.101808 | |||||||||||||||||||||||||||||||||
Status: | Peer Reviewed | |||||||||||||||||||||||||||||||||
Publication Status: | Published | |||||||||||||||||||||||||||||||||
Access rights to Published version: | Restricted or Subscription Access | |||||||||||||||||||||||||||||||||
Date of first compliant deposit: | 22 June 2022 | |||||||||||||||||||||||||||||||||
Date of first compliant Open Access: | 3 August 2022 | |||||||||||||||||||||||||||||||||
RIOXX Funder/Project Grant: |
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