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  1H high field electron-nuclear double resonance spectroscopy at 263 GHz/9.4 T.

Tkach, I., Bejenke, I., Hecker, F., Kehl, A., Kasanmascheff, M., Gromov, I., et al. (2019). 1H high field electron-nuclear double resonance spectroscopy at 263 GHz/9.4 T. Journal of Magnetic Resonance, 303, 17-27. doi:10.1016/j.jmr.2019.04.001.

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Item Permalink: http://hdl.handle.net/21.11116/0000-0003-6E61-5 Version Permalink: http://hdl.handle.net/21.11116/0000-0003-8978-C
Genre: Journal Article

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 Creators:
Tkach, I.1, Author              
Bejenke, I.1, Author              
Hecker, F.1, Author              
Kehl, A.1, Author              
Kasanmascheff, M.1, Author              
Gromov, I., Author
Prisecaru, I., Author
Höfer, P., Author
Hiller, M.1, Author              
Bennati, M.1, Author              
Affiliations:
1Research Group of Electron Paramagnetic Resonance, MPI for Biophysical Chemistry, Max Planck Society, ou_578606              

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Free keywords: 263 GHz ENDOR resonator, high frequency; 263 GHz ENDOR setup; High field ENDOR and EPR; Hyperfine spectroscopy; Nuclear spins; Tyrosyl radicals
 Abstract: We present and discuss the performance of 1H electron-nuclear double resonance (ENDOR) at 263 GHz/9.4 T by employing a prototype, commercial quasi optical spectrometer. Basic instrumental features of the setup are described alongside a comprehensive characterization of the new ENDOR probe head design. The performance of three different ENDOR pulse sequences (Davies, Mims and CP-ENDOR) is evaluated using the 1H BDPA radical. A key feature of 263 GHz spectroscopy - the increase in orientation selectivity in comparison with 94 GHz experiments - is discussed in detail. For this purpose, the resolution of 1H ENDOR spectra at 263 GHz is verified using a representative protein sample containing approximately 15 picomoles of a tyrosyl radical. Davies ENDOR spectra recorded at 5 K reveal previously obscured spectral features, which are interpreted by spectral simulations aided by DFT calculations. Our analysis shows that seven internal proton couplings are detectable for this specific radical if sufficient orientation selectivity is achieved. The results prove the fidelity of 263 GHz experiments in reporting orientation-selected 1H ENDOR spectra and demonstrate that new significant information can be uncovered in complex molecular systems, owing to the enhanced resolution combined with high absolute sensitivity and no compromise in acquisition time.

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Language(s): eng - English
 Dates: 2019-04-032019-06
 Publication Status: Published in print
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 Rev. Method: Peer
 Identifiers: DOI: 10.1016/j.jmr.2019.04.001
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Title: Journal of Magnetic Resonance
Source Genre: Journal
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Pages: - Volume / Issue: 303 Sequence Number: - Start / End Page: 17 - 27 Identifier: -