期刊
MAGNETIC RESONANCE IN CHEMISTRY
卷 43, 期 -, 页码 S248-S255出版社
WILEY
DOI: 10.1002/mrc.1681
关键词
high-field/high-frequency pulsed EPR; ENDOR; PELDOR; DEER; librational motion; Ras center dot Mn2+center dot GDP; tyrosyl radical
Within this review, we describe a home-built pulsed electron paramagnetic resonance (EPR) spectrometer operating at 180 GHz as well as the incorporation of two double resonance techniques, electron nuclear double resonance (ENDOR) and pulsed electron double resonance (PELDOR), along with first applications. Hahn-echo decays on a TEMPO/polystyrene sample are presented, demonstrating that the observation of anisotropic librational motions is possible in a very precise manner at high magnetic fields. Bisdiphenylenephenyl-allyl is used as a model system to illustrate the performance of the setup for H-1-ENDOR using the Mims as well as the Davies sequence. Furthermore, first H-1-Mims and Davies ENDOR spectra on a biological sample, the wild-type Ras(.)Mn(2+.)GDP protein, are reported. The capability of the 180-GHz PELDOR setup is demonstrated using the three-pulse ELDOR sequence on the protein ribonucleotide reductase (RNR) subunit R2 from Escherichia coli, which contains two tyrosyl radicals at a 33 A distance. At 180 GHz, orientation selectivity is observed and the modulation frequency is found to be in good agreement with theoretical predictions. Copyright (c) 2005 John Wiley & Sons, Ltd.
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