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Pulsed EPR dipolar spectroscopy at Q- and G-band on a trityl biradical

Pulsed EPR dipolar spectroscopy at Q- and G-band on a trityl biradical

Title: Pulsed EPR dipolar spectroscopy at Q- and G-band on a trityl biradical
Author: Akhmetzyanov, D.
Schöps, P.
Marko, A.
Kunjir, N. C.
Sigurdsson, Snorri   orcid.org/0000-0003-2492-1456
Prisner, Thomas F.
Date: 2015
Language: English
Scope: 24446-24451
University/Institute: Háskóli Íslands
University of Iceland
School: Verkfræði- og náttúruvísindasvið (HÍ)
School of Engineering and Natural Sciences (UI)
Department: Raunvísindadeild (HÍ)
Faculty of Physical Sciences (UI)
Raunvísindastofnun (HÍ)
Science Institute (UI)
Series: Physical Chemistry Chemical Physics;17(37)
ISSN: 1463-9076
1463-9084 (eISSN)
DOI: 10.1039/c5cp03671b
Subject: Dynamic nuclear polarization; Electron double resonance; Spin labels; Distance measurements; Radicals; Echo; GHZ; ESR; Algorithm; Litrófsgreining; Efnagreining; Rafeindir
URI: https://hdl.handle.net/20.500.11815/1958

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Akhmetzyanov, D., Schöps, P., Marko, A., Kunjir, N. C., Sigurdsson, S. T., & Prisner, T. F. (2015). Pulsed EPR dipolar spectroscopy at Q- and G-band on a trityl biradical. Physical Chemistry Chemical Physics, 17(37), 24446-24451 doi:10.1039/c5cp03671b


Pulsed electron paramagnetic resonance (EPR) spectroscopy is a valuable technique for the precise determination of distances between paramagnetic spin labels that are covalently attached to macromolecules. Nitroxides have commonly been utilised as paramagnetic tags for biomolecules, but trityl radicals have recently been developed as alternative spin labels. Trityls exhibit longer electron spin relaxation times and higher stability than nitroxides under in vivo conditions. So far, trityl radicals have only been used in pulsed EPR dipolar spectroscopy (PDS) at X-band (9.5 GHz), K-u-band (17.2 GHz) and Q-band (34 GHz) frequencies. In this study we investigated a trityl biradical by PDS at Q-band (34 GHz) and G-band (180 GHz) frequencies. Due to the small spectral width of the trityl (30 MHz) at Q-band frequencies, single frequency PDS techniques, like double-quantum coherence (DQC) and single frequency technique for refocusing dipolar couplings (SIFTER), work very efficiently. Hence, Q-band DQC and SIFTER experiments were performed and the results were compared; yielding a signal to noise ratio for SIFTER four times higher than that for DQC. At G-band frequencies the resolved axially symmetric g-tensor anisotropy of the trityl exhibited a spectral width of 130 MHz. Thus, pulsed electron electron double resonance (PELDOR/DEER) obtained at different pump-probe positions across the spectrum was used to reveal distances. Such a multi-frequency approach should also be applicable to determine structural information on biological macromolecules tagged with trityl spin labels.


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