Journal
ISRAEL JOURNAL OF CHEMISTRY
Volume 54, Issue 1-2, Pages 207-221Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/ijch.201300126
Keywords
Dynamic nuclear polarization (DNP); Natural products; NMR spectroscopy; Radicals; Structureactivity relationships
Categories
Funding
- National Institutes of Health [EB002804, EB003151, EB002026, EB001960, EB001035, EB001965, EB004866]
- National Institutes of Health (NIGMS) [GM095843]
- Ente Cassa di Risparmio di Firenze
- MIUR PRIN [2009FAKHZT_001]
- European Commission [261863]
- Instruct, EU ESFRI
- Natural Science and Engineering Research Council of Canada
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We report our recent efforts directed at improving high-field dynamic nuclear polarization (DNP) experiments. We investigated a series of thiourea nitroxide radicals and the associated DNP enhancements ranging from epsilon=25 to 82, which demonstrate the impact of molecular structure on performance. We directly polarized low-gamma nuclei, including C-13, H-2, and O-17, by the cross effect mechanism using trityl radicals as a polarization agent. We discuss a variety of sample preparation techniques for DNP with emphasis on the benefits of methods that do not use a glass-forming cryoprotecting matrix. Lastly, we describe a corrugated waveguide for use in a 700MHz/460GHz DNP system that improves microwave delivery and increases enhancements up to 50%.
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