Jähnig, Fabian, Aaron Himmler, Grzegorz Kwiatkowski, Alexander Däpp, Andreas Hunkeler, Sebastian Kozerke, and Matthias Ernst. “A Spin-Thermodynamic Approach to Characterize Spin Dynamics in TEMPO-Based Samples for Dissolution DNP at 7 T Field.” Journal of Magnetic Resonance 303 (June 1, 2019): 91–104
The spin dynamics of dissolution DNP samples consisting of 4.5 M [13C]urea in a mixture of (1/1)Vol glycerol/water using 4-Oxo-TEMPO as a radical was investigated. We analyzed the DNP dynamics as function of radical concentration at 7 T and 3.4 T static magnetic field as well as function of deuteration of the solvent matrix at the high field. The spin dynamics could be reproduced in all cases, at least qualitatively, by a thermodynamic model based on spin temperatures of the nuclear Zeeman baths and an electron non-Zeeman (dipolar) bath. We find, however, that at high field (7 T) and low radical concentrations (25 mM) the nuclear spins do not reach the same spin temperature indicating a weak coupling of the two baths. At higher radical concentrations, as well as for all radical concentrations at low field (3.4 T), the two nuclear Zeeman baths reach the same spin temperature within experimental errors. Additionally, the spin system was prepared with different initial conditions. For these cases, the thermodynamic model was able to predict the time evolution of the system well. While the DNP profiles do not give clear indications to a specific polarization transfer mechanism, at high field (7 T) increased coupling is seen. The EPR line shapes cannot clarify this in absence of ELDOR type experiments, nevertheless DNP profiles and dynamics under frequency-modulated microwave irradiation illustrate the expected increase in coupling between electrons with increasing radical concentration.
Electron spin resonance studies on deuterated nitroxyl spin probes used in Overhauser-enhanced magnetic resonance imaging #DNPNMR #ODNP
From The DNP-NMR Blog:
Electron spin resonance studies on deuterated nitroxyl spin probes used in Overhauser-enhanced magnetic resonance imaging #DNPNMR #ODNP
Jebaraj, D. David, Hideo Utsumi, and A. Milton Franklin Benial. “Electron Spin Resonance Studies on Deuterated Nitroxyl Spin Probes Used in Overhauser-Enhanced Magnetic Resonance Imaging.” Magnetic Resonance in Chemistry 55, no. 8 (2017): 700–705.
https://doi.org/10.1002/mrc.4576.
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06-23-2018 12:47 AM
Communication: Dissolution DNP reveals a long-lived deuterium spin state imbalance in methyl groups #DNPNMR
From The DNP-NMR Blog:
Communication: Dissolution DNP reveals a long-lived deuterium spin state imbalance in methyl groups #DNPNMR
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Jhajharia, A., et al., Communication: Dissolution DNP reveals a long-lived deuterium spin state imbalance in methyl groups. J Chem Phys, 2017. 146(4): p. 041101.
https://www.ncbi.nlm.nih.gov/pubmed/28147551
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08-31-2017 12:14 AM
Measuring absolute spin polarization in dissolution-DNP by Spin PolarimetrY Magnetic Resonance (SPY-MR)
From The DNP-NMR Blog:
Measuring absolute spin polarization in dissolution-DNP by Spin PolarimetrY Magnetic Resonance (SPY-MR)
Vuichoud, B., et al., Measuring absolute spin polarization in dissolution-DNP by Spin PolarimetrY Magnetic Resonance (SPY-MR). J. Magn. Reson., 2015. 260: p. 127-135.
http://www.sciencedirect.com/science/article/pii/S1090780715002074
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01-27-2016 09:09 PM
[NMR paper] Electron Spin Density on the Axial His Ligand of High-Spin and Low-Spin Nitrophorin 2 Probed by Heteronuclear NMR Spectroscopy.
Electron Spin Density on the Axial His Ligand of High-Spin and Low-Spin Nitrophorin 2 Probed by Heteronuclear NMR Spectroscopy.
http://www.ncbi.nlm.nih.gov/corehtml/query/egifs/http:--pubs.acs.org-images-pubmed-acspubs.jpg Related Articles Electron Spin Density on the Axial His Ligand of High-Spin and Low-Spin Nitrophorin 2 Probed by Heteronuclear NMR Spectroscopy.
Inorg Chem. 2013 Jan 17;
Authors: Abriata LA, Zaballa ME, Berry RE, Yang F, Zhang H, Walker FA, Vila AJ
Abstract
The electronic structure of heme proteins is exquisitely tuned...
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02-03-2013 10:19 AM
Computational Study andMolecular Orbital Analysisof NMR Shielding, Spin–Spin Coupling, and Electric Field Gradientsof Azido Platinum Complexes
Computational Study andMolecular Orbital Analysisof NMR Shielding, Spin–Spin Coupling, and Electric Field Gradientsof Azido Platinum Complexes
Kiplangat Sutter and Jochen Autschbach
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja3040762/aop/images/medium/ja-2012-040762_0008.gif
Journal of the American Chemical Society
DOI: 10.1021/ja3040762
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA
http://feeds.feedburner.com/~r/acs/jacsat/~4/XTeiJ4ddvO4
[NMR paper] Spin labels as a tool to identify and characterize protein-ligand interactions by NMR
Spin labels as a tool to identify and characterize protein-ligand interactions by NMR spectroscopy.
Related Articles Spin labels as a tool to identify and characterize protein-ligand interactions by NMR spectroscopy.
Chembiochem. 2002 Mar 1;3(2-3):167-73
Authors: Jahnke W
NMR spectroscopy based discovery and optimization of lead compounds for a given molecular target requires the development of methods with maximum sensitivity and robustness. It is shown here that organic nitroxide radicals ("spin labels") can be used to boost the sensitivity...
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11-24-2010 08:49 PM
[NMR paper] Thermodynamic insights into proteins from NMR spin relaxation studies.
Thermodynamic insights into proteins from NMR spin relaxation studies.
Related Articles Thermodynamic insights into proteins from NMR spin relaxation studies.
Curr Opin Struct Biol. 2001 Oct;11(5):555-9
Authors: Spyracopoulos L, Sykes BD
NMR spin relaxation measurements of picosecond to nanosecond timescale backbone and sidechain fluctuations of protein molecules, and subsequent entropic interpretation yield interesting, but sometimes counterintuitive, insights into proteins. The stabilities of proteins and protein interactions are achieved...
A spin-thermodynamic approach to characterize spin dynamics in TEMPO-based samples for dissolution DNP at 7 T field #DNPNMR
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