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(14) N solid-state NMR spectroscopy of amino acids

Veinberg, Stanislav L., Friedl, Zachary W., Lindquist, Austin W., Kispal, Brianna, Harris, Kristopher J., O'Dell, Luke A. and Schurko, Robert W. 2016, (14) N solid-state NMR spectroscopy of amino acids, Chemphyschem, vol. 17, no. 23, pp. 4011-4027, doi: 10.1002/cphc.201600873.

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Title (14) N solid-state NMR spectroscopy of amino acids
Author(s) Veinberg, Stanislav L.
Friedl, Zachary W.
Lindquist, Austin W.
Kispal, Brianna
Harris, Kristopher J.
O'Dell, Luke A.ORCID iD for O'Dell, Luke A. orcid.org/0000-0002-7760-5417
Schurko, Robert W.
Journal name Chemphyschem
Volume number 17
Issue number 23
Start page 4011
End page 4027
Total pages 17
Publisher Wiley-VCH Verlag
Place of publication Weinheim, Germany
Publication date 2016-12-05
ISSN 1439-7641
Keyword(s) NMR spectroscopy
amino acids
hydrogen bonding
nitrogen
polymorphism
Science & Technology
Physical Sciences
Chemistry, Physical
Physics, Atomic, Molecular & Chemical
Chemistry
Physics
NUCLEAR-QUADRUPOLE RESONANCE
PROTON MAGNETIC-RELAXATION
ELECTRIC-FIELD GRADIENT
ANGLE-SPINNING NMR
X-RAY-DIFFRACTION
MOLECULAR-MOTION
120 K
CROSS-POLARIZATION
CRYSTAL-STRUCTURES
ADIABATIC PULSES
Summary (14) N ultra-wideline solid-state NMR (SSNMR) spectra were obtained for 16 naturally occurring amino acids and four related derivatives by using the WURST-CPMG (wideband, uniform rate, and smooth truncation Carr-Purcell-Meiboom-Gill) pulse sequence and frequency-stepped techniques. The (14) N quadrupolar parameters were measured for the sp(3) nitrogen moieties (quadrupolar coupling constant, CQ , values ranged from 0.8 to 1.5 MHz). With the aid of plane-wave DFT calculations of the (14) N electric-field gradient tensor parameters and orientations, the moieties were grouped into three categories according to the values of the quadrupolar asymmetry parameter, ηQ : low (≤0.3), intermediate (0.31-0.7), and high (≥0.71). For RNH3(+) moieties, greater variation in N-H bond lengths was observed for systems with intermediate ηQ values than for those with low ηQ values (this variation arose from different intermolecular hydrogen-bonding arrangements). Strategies for increasing the efficiency of (14) N SSNMR spectroscopy experiments were discussed, including the use of sample deuteration, high-power (1) H decoupling, processing strategies, high magnetic fields, and broadband cross-polarization (BRAIN-CP). The temperature-dependent rotations of the NH3 groups and their influence on (14) N transverse relaxation rates were examined. Finally, (14) N SSNMR spectroscopy was used to differentiate two polymorphs of l-histidine through their quadrupolar parameters and transverse relaxation time constants. The strategies outlined herein permitted the rapid acquisition of directly detected (14) N SSNMR spectra that to date was not matched by other proposed methods.
Language eng
DOI 10.1002/cphc.201600873
Field of Research 020401 Condensed Matter Characterisation Technique Development
030301 Chemical Characterisation of Materials
0306 Physical Chemistry (Incl. Structural)
0202 Atomic, Molecular, Nuclear, Particle And Plasma Physics
0307 Theoretical And Computational Chemistry
Socio Economic Objective 970103 Expanding Knowledge in the Chemical Sciences
HERDC Research category C1 Refereed article in a scholarly journal
ERA Research output type C Journal article
Copyright notice ©2016, Wiley-VCH Verlag
Persistent URL http://hdl.handle.net/10536/DRO/DU:30087905

Document type: Journal Article
Collection: Institute for Frontier Materials
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