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Data for 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) Data for Combining heteronuclear correlation NMR with spin-diffusion to detect relayed Cl–H–H and N–H–H proximities in molecular solids. [Dataset]
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Official URL: http://wrap.warwick.ac.uk/166510/
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.
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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 | ||||||||||||||||||||||||||||||||||||
Type of Data: | experimental data | ||||||||||||||||||||||||||||||||||||
Library of Congress Subject Headings (LCSH): | Nuclear magnetic resonance, Nuclear magnetic resonance spectroscopy, Crystallography, Solid state chemistry, Molecular crystals | ||||||||||||||||||||||||||||||||||||
Publisher: | University of Warwick, Department of Physics | ||||||||||||||||||||||||||||||||||||
Official Date: | 21 June 2022 | ||||||||||||||||||||||||||||||||||||
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Status: | Not Peer Reviewed | ||||||||||||||||||||||||||||||||||||
Publication Status: | Published | ||||||||||||||||||||||||||||||||||||
Media of Output (format): | .cif, .magres | ||||||||||||||||||||||||||||||||||||
Access rights to Published version: | Open Access (Creative Commons) | ||||||||||||||||||||||||||||||||||||
Copyright Holders: | University of Warwick | ||||||||||||||||||||||||||||||||||||
Description: | Dataset for following figures: |
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Date of first compliant deposit: | 21 June 2022 | ||||||||||||||||||||||||||||||||||||
Date of first compliant Open Access: | 21 June 2022 | ||||||||||||||||||||||||||||||||||||
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