Articles | Volume 1, issue 2
https://doi.org/10.5194/mr-1-285-2020
© Author(s) 2020. This work is distributed under
the Creative Commons Attribution 4.0 License.
the Creative Commons Attribution 4.0 License.
https://doi.org/10.5194/mr-1-285-2020
© Author(s) 2020. This work is distributed under
the Creative Commons Attribution 4.0 License.
the Creative Commons Attribution 4.0 License.
Strategies to identify and suppress crosstalk signals in double electron–electron resonance (DEER) experiments with gadoliniumIII and nitroxide spin-labeled compounds
Markus Teucher
Faculty of Chemistry and Biochemistry, Ruhr University Bochum, Universitätsstraße 150, 44801 Bochum, Germany
Mian Qi
Faculty of Chemistry and Center for Molecular Materials (CM), Bielefeld University, Universitätsstraße 25, 33615 Bielefeld, Germany
Ninive Cati
Faculty of Chemistry and Center for Molecular Materials (CM), Bielefeld University, Universitätsstraße 25, 33615 Bielefeld, Germany
Henrik Hintz
Faculty of Chemistry and Center for Molecular Materials (CM), Bielefeld University, Universitätsstraße 25, 33615 Bielefeld, Germany
Adelheid Godt
Faculty of Chemistry and Center for Molecular Materials (CM), Bielefeld University, Universitätsstraße 25, 33615 Bielefeld, Germany
Enrica Bordignon
CORRESPONDING AUTHOR
Faculty of Chemistry and Biochemistry, Ruhr University Bochum, Universitätsstraße 150, 44801 Bochum, Germany
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Magn. Reson. Discuss., https://doi.org/10.5194/mr-2024-19, https://doi.org/10.5194/mr-2024-19, 2024
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Quantification of heterogeneous systems such as unstructured or semi-structured (bio)macromolecules is an important but challenging task. Pulse EPR methods can contribute by characterizing the local nuclear environment of a spin centre. Here, we provide a detailed assessment of a pulse EPR technique derived from a RIDME experiment. We review the theoretical principles, discuss the data analysis and demonstrate an application to a spin-labeled macromolecule supported by in silico modelling.
Gunnar Jeschke, Nino Wili, Yufei Wu, Sergei Kuzin, Hugo Karas, Henrik Hintz, and Adelheid Godt
Magn. Reson. Discuss., https://doi.org/10.5194/mr-2024-17, https://doi.org/10.5194/mr-2024-17, 2024
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Electron spins sense their environment via magnetic interactions. An important contribution stems from nuclear spins in their vicinity. They cause loss of coherence and thus reduce resolution of spectra obtained by experiments on electron spins and the efficiency of transferring electron-spin magentization to other nuclear spins. Here we study how protons in trityl radicals contribute to coherence loss. Such coherence loss is slower in the presence of a strong microwave field.
Agathe Vanas, Janne Soetbeer, Frauke Diana Breitgoff, Henrik Hintz, Muhammad Sajid, Yevhen Polyhach, Adelheid Godt, Gunnar Jeschke, Maxim Yulikov, and Daniel Klose
Magn. Reson., 4, 1–18, https://doi.org/10.5194/mr-4-1-2023, https://doi.org/10.5194/mr-4-1-2023, 2023
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Nanometre distance measurements between spin labels by pulse EPR techniques yield structural information on the molecular level. Here, backed by experimental data, we derive a description for the total signal of the single-frequency technique for refocusing dipolar couplings (SIFTER), showing how the different spin–spin interactions give rise to dipolar signal and background – the latter has thus far been unknown.
Hassane EL Mkami, Robert I. Hunter, Paul A. S. Cruickshank, Michael J. Taylor, Janet E. Lovett, Akiva Feintuch, Mian Qi, Adelheid Godt, and Graham M. Smith
Magn. Reson., 1, 301–313, https://doi.org/10.5194/mr-1-301-2020, https://doi.org/10.5194/mr-1-301-2020, 2020
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Through a series of DEER measurements on two Gd rulers, with Gd–Gd distances of 2.1 and 6.0 nm, we show that artefacts commonly observed when measuring short distances can be eliminated by avoiding excitation of the central transition by both the pump and observer pulses. By using a wideband induction mode sample holder at 94 GHz, we demonstrate that high-quality DEER measurements will become possible using Gd spin labels at sub-µM concentrations, with implications for in-cell DEER measurements.
Nino Wili, Henrik Hintz, Agathe Vanas, Adelheid Godt, and Gunnar Jeschke
Magn. Reson., 1, 75–87, https://doi.org/10.5194/mr-1-75-2020, https://doi.org/10.5194/mr-1-75-2020, 2020
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Measuring distances between unpaired electron spins is an important application of electron paramagnetic resonance. The longest distance that is accessible is limited by the phase memory time of the electron spins. Here we show that strong continuous microwave irradiation can significantly slow down relaxation. Additionally, we introduce a phase-modulation scheme that allows measurement of the distance during the irradiation. Our approach could thus significantly extend the accessible distances.
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Atmos. Chem. Phys., 18, 15841–15857, https://doi.org/10.5194/acp-18-15841-2018, https://doi.org/10.5194/acp-18-15841-2018, 2018
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We synthesized a compound, a tetraol, which is an atmospheric oxidation product in isoprene-derived secondary organic aerosols, and studied whether the tetraol is liquid or solid depending upon temperature and relative humidity, both in pure form and in mixtures with other compounds. Our results imply a liquid state of
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Related subject area
Field: EPR | Topic: Pulse-sequence development
The decay of the refocused Hahn echo in double electron–electron resonance (DEER) experiments
Distance measurement between trityl radicals by pulse dressed electron paramagnetic resonance with phase modulation
Optimising broadband pulses for DEER depends on concentration and distance range of interest
Thorsten Bahrenberg, Samuel M. Jahn, Akiva Feintuch, Stefan Stoll, and Daniella Goldfarb
Magn. Reson., 2, 161–173, https://doi.org/10.5194/mr-2-161-2021, https://doi.org/10.5194/mr-2-161-2021, 2021
Short summary
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Double electron–electron resonance (DEER) provides information on the structure of proteins by attaching two spin labels to the protein at a well-defined location and measuring the distance between them. The sensitivity of the method in terms of the amount of the protein that is needed for the experiment depends strongly on the relaxation properties of the spin label and the composition of the solvent. We show how to set up the experiment for best sensitivity when the solvent is water (H2O).
Nino Wili, Henrik Hintz, Agathe Vanas, Adelheid Godt, and Gunnar Jeschke
Magn. Reson., 1, 75–87, https://doi.org/10.5194/mr-1-75-2020, https://doi.org/10.5194/mr-1-75-2020, 2020
Short summary
Short summary
Measuring distances between unpaired electron spins is an important application of electron paramagnetic resonance. The longest distance that is accessible is limited by the phase memory time of the electron spins. Here we show that strong continuous microwave irradiation can significantly slow down relaxation. Additionally, we introduce a phase-modulation scheme that allows measurement of the distance during the irradiation. Our approach could thus significantly extend the accessible distances.
Andreas Scherer, Sonja Tischlik, Sabrina Weickert, Valentin Wittmann, and Malte Drescher
Magn. Reson., 1, 59–74, https://doi.org/10.5194/mr-1-59-2020, https://doi.org/10.5194/mr-1-59-2020, 2020
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The determination of distance distributions in the nanometre range is an important application of pulsed electron paramagnetic resonance spectroscopy. However, low sensitivity is often a major challenge. In this paper, we compare several broadband-shaped pulses and compare their performance to classical rectangular pulses in order to increase the sensitivity of double electron–electron resonance to a commercial setup. We show that improvements in sensitivity of up to 86 % are possible.
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Short summary
With a pulsed dipolar electron paramagnetic resonance technique named double electron–electron resonance (DEER), we measure nanometer distances between spin labels attached to biomolecules. If more than one spin type is present (A and B), we can separately address AA, AB, and BB distances via distinct spectroscopic channels, increasing the information content per sample. Here, we investigate the appearance of unwanted channel crosstalks in DEER and suggest ways to identify and suppress them.
With a pulsed dipolar electron paramagnetic resonance technique named double electron–electron...