Abstract
In this work, the experimental conditions and parameters necessary to optimize the long-distance (≥60 Å) double electron–electron resonance (DEER) measurements of biomacromolecules labeled with Gd(III) tags are analyzed. The specific parameters discussed are the temperature, microwave band, the separation between the pumping and observation frequencies, pulse train repetition rate, pulse durations and pulse positioning in the electron paramagnetic resonance spectrum. It was found that: (1) in optimized DEER measurements, the observation pulses have to be applied at the maximum of the electron paramagnetic resonance spectrum; (2) the optimal temperature range for Ka-band measurements is 14–17 K, while in W-band the optimal temperatures are between 6 and 9 K; (iv) W-band is preferable to Ka-band for DEER measurements. Recent achievements and the conditions necessary for short-distance measurements (<15 Å) are also briefly discussed.
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Acknowledgments
This research was supported by the Binational Science Foundation (USA–Israel, BSF#2006179), NIH 1R01 EB005866-01, 5R01EB00586-6 and S10RR020959, NSF DBI-0139459, DBI-9604939 and BIR-922443. A portion of this research was performed using EMSL, a national scientific user facility sponsored by the Department of Energy’s Office of Biological and Environmental Research and located at Pacific Northwest National Laboratory. A.R. thanks Dr. A. Potapov for a helpful discussion of distance distribution function between Gd(III) in the trimer.
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Raitsimring, A., Astashkin, A.V., Enemark, J.H. et al. Optimization of Pulsed-DEER Measurements for Gd-Based Labels: Choice of Operational Frequencies, Pulse Durations and Positions, and Temperature. Appl Magn Reson 44, 649–670 (2013). https://doi.org/10.1007/s00723-012-0434-6
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DOI: https://doi.org/10.1007/s00723-012-0434-6