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TOTAPOL: A Biradical Polarizing Agent for Dynamic Nuclear Polarization Experiments in Aqueous Media
Abstract
In a previous publication, we described the use of biradicals, in that case two TEMPO molecules tethered by an ethylene glycol chain of variable length, as polarizing agents for microwave driven dynamic nuclear polarization (DNP) experiments. The use of biradicals in place of monomeric paramagnetic centers such as TEMPO yields enhancements that are a factor of approximately 4 larger (epsilon approximately 175 at 5 T and 90 K) and concurrently the concentration of the polarizing agent is a factor of 4 smaller (10 mM electron spins), reducing the residual electron nuclear dipole broadening. In this paper we describe the synthesis and characterization by EPR and DNP/NMR of an improved polarizing agent 1-(TEMPO-4-oxy)-3-(TEMPO-4-amino)propan-2-ol (TOTAPOL). Under the same experimental conditions and using 2.5 mm magic angle rotors, this new biradical yields larger enhancements (epsilon approximately 290) at lower concentrations (6 mM electron spins) and has the additional important property that it is compatible with experiments in aqueous media, including salt solutions commonly used in the study of proteins and nucleic acids.
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Dynamic nuclear polarization for sensitivity enhancement in modern solid-state NMR
Lilly Thankamony, A. S., Wittmann, J. J., Kaushik, M., & Corzilius, B. (2017) · Progress in Nuclear Magnetic Resonance Spectroscopy · doi:10.1016/j.pnmrs.2017.06.002 · Cited by 544
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Sauvée, C., Rosay, M., Casano, G., Aussenac, F., Weber, R. T., Ouari, O., & Tordo, P. (2013) · Angewandte Chemie International Edition · doi:10.1002/anie.201304657 · Cited by 503
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Metadata
- Authors
- Song, C., Hu, K.-N., Joo, C.-G., Swager, T. M., & Griffin, R. G.
- Venue
- Journal of the American Chemical Society
- Publisher
- American Chemical Society (ACS)
- Published
- 2006-08-16
- Volume
- 128
- Issue
- 35
- Pages
- 11385-11390
- ISSN
- 0002-7863 (ISSN-L)
- 1520-5126
- OpenAlex
- W2065265087
- Cited by
- 550
- References
- 0
- FWCI
- 4.73
- Type
- journal article
- Language
- en
- Open access
- closed
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