Magnetic Resonance
Magnetic Resonance
MR
Articles | Volume 1, issue 2
Articles | Volume 1, issue 2
https://doi.org/10.5194/mr-1-301-2020
© Author(s) 2020. This work is distributed under
the Creative Commons Attribution 4.0 License.
https://doi.org/10.5194/mr-1-301-2020
© Author(s) 2020. This work is distributed under
the Creative Commons Attribution 4.0 License.
Articles | Volume 1, issue 2
Research article
 | 
09 Dec 2020
Research article |  | 09 Dec 2020

High-sensitivity Gd3+–Gd3+ EPR distance measurements that eliminate artefacts seen at short distances

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

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Cited articles

Bahrenberg, T., Rosenski, Y., Carmieli, R., Zibzener, K., Qi, M., Frydman, V., Godt, A., Goldfarb, D., and Feintuch, A.: Improved sensitivity for W-band Gd(III)-Gd(III) and nitroxide-nitroxide DEER measurements with shaped pulses, J. Magn. Reson., 283, 1–13, https://doi.org/10.1016/j.jmr.2017.08.003, 2017. 
Clayton, J. A., Keller, K., Qi, M., Wegner, J., Koch, V., Hintz, H., Godt, A., Han, S., Jeschke, G., Sherwin, M. S., and Yulikov, M.: Quantitative analysis of zero-field splitting parameter distributions in Gd(iii) complexes, Phys. Chem. Chem. Phys., 20, 10470–10492, https://doi.org/10.1039/C7CP08507A, 2018. 
Cohen, M. R., Frydman, V., Milko, P., Iron, M. A., Abdelkader, E. H., Lee, M. D., Swarbrick, J. D., Raitsimring, A., Otting, G., Graham, B., Feintuch, A., and Goldfarb, D.: Overcoming artificial broadening in Gd3+-Gd3+ distance distributions arising from dipolar pseudo-secular terms in DEER experiments, Phys. Chem. Chem. Phys., 18, 12847–12859, https://doi.org/10.1039/c6cp00829a, 2016. 
Collauto, A., Frydman, V., Lee, M. D., Abdelkader, E. H., Feintuch, A., Swarbrick, J. D., Graham, B., Otting, G., and Goldfarb, D.: RIDME distance measurements using Gd(iii) tags with a narrow central transition, Phys. Chem. Chem. Phys., 18, 19037–19049, https://doi.org/10.1039/c6cp03299k, 2016. 
Cruickshank, P. A., Bolton, D. R., Robertson, D. A., Hunter, R. I., Wylde, R. J., and Smith, G. M.: A kilowatt pulsed 94GHz electron paramagnetic resonance spectrometer with high concentration sensitivity, high instantaneous bandwidth, and low dead time, Rev. Sci. Instrum., 80, 103102, https://doi.org/10.1063/1.3239402, 2009. 
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Short summary
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.
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