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  Heteronuclear cross-relaxation effect modulated by the dynamics of N-functional groups in the solid state under 15N DP-MAS DNP

Park, H., Uluca-Yazgi, B., Heumann, S., Schlögl, R., Granwehr, J., Heise, H., et al. (2020). Heteronuclear cross-relaxation effect modulated by the dynamics of N-functional groups in the solid state under 15N DP-MAS DNP. Journal of Magnetic Resonance, 312: 106688. doi:10.1016/j.jmr.2020.106688.

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Item Permalink: https://hdl.handle.net/21.11116/0000-0005-A33D-F Version Permalink: https://hdl.handle.net/21.11116/0000-0009-61A3-1
Genre: Journal Article

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 Creators:
Park, Heeyong1, 2, 3, Author
Uluca-Yazgi, Boran4, 5, Author
Heumann, Saskia1, Author
Schlögl, Robert1, 6, Author           
Granwehr, Josef2, 3, Author
Heise, Henrike4, 5, Author
Schleker, P. Philipp M.1, 2, Author
Affiliations:
1Max Planck Institute for Chemical Energy Conversion, Department of Heterogeneous Reactions, 45470 Mülheim an der Ruhr, Germany, ou_persistent22              
2Forschungszentrum Jülich, IEK-9, 52425 Jülich, Germany, ou_persistent22              
3RWTH Aachen University, Institute of Technical and Macromolecular Chemistry, 52074 Aachen, Germany, ou_persistent22              
4Forschungszentrum Jülich, IBI-7 and JuStruct, 52425 Jülich, Germany, ou_persistent22              
5Heinrich Heine Universität Düsseldorf, Institute of Physical Biology, 40225 Düsseldorf, Germany, ou_persistent22              
6Inorganic Chemistry, Fritz Haber Institute, Max Planck Society, ou_24023              

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 Abstract: In a typical magic-angle spinning (MAS) dynamic nuclear polarization (DNP) nuclear magnetic resonance (NMR) experiment, several mechanisms are simultaneously involved when transferring much larger polarization of electron spins to NMR active nuclei of interest. Recently, specific cross-relaxation enhancement by active motions under DNP (SCREAM-DNP) [Daube et al. JACS 2016] has been reported as one of these mechanisms. Thereby 13C enhancement with inverted sign was observed in a direct polarization (DP) MAS DNP experiment, caused by reorientation dynamics of methyl that was not frozen out at 100 K. Here, we report on the spontaneous polarization transfer from hyperpolarized 1H to both primary amine and ammonium nitrogens, resulting in an additional positive signal enhancement in the 15N NMR spectra during 15N DP-MAS DNP. The cross-relaxation induced signal enhancement (CRE) for 15N is of opposite sign compared to that observed for 13C due to the negative sign of the gyromagnetic ratio of 15N. The influence on CRE efficiency caused by variation of the radical solution composition and by temperature was also investigated.

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Language(s): eng - English
 Dates: 2020-01-122019-11-272020-01-142020-01-162020-03
 Publication Status: Issued
 Pages: 7
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 Table of Contents: -
 Rev. Type: Peer
 Identifiers: DOI: 10.1016/j.jmr.2020.106688
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Title: Journal of Magnetic Resonance
Source Genre: Journal
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Publ. Info: San Diego : Academic Press
Pages: 7 Volume / Issue: 312 Sequence Number: 106688 Start / End Page: - Identifier: ISSN: 0022-2364
CoNE: https://pure.mpg.de/cone/journals/resource/954922651175_1