a Bruker ELEXSYS E500 EPR spectrometer operating at cryogenic temperatures via
an Oxford Instruments ESR900 liquid helium cryostat interfaced with an ITC503
temperature controller from the same manufacturer. Samples were 250 μl in
Wilmad 4 mm o.d. quartz tubes. Sample temperatures were as stated, microwave
power was 10 μW, modulation amplitude was 1.5 G. Pulsed electron nuclear
double resonance (ENDOR) spectra were obtained at 65 K using a Bruker ELEXSYS
E580 spectrometer equipped with an EN 4118X-MD4 dielectric resonator.
Temperature control was effected using an Oxford Instruments CF935 cryostat and
ITC503 temperature controller. The Davies pulsed ENDOR sequence was employed at
intermediate Q using soft microwave pulses and FID detection (π/2 = 200
ns) with a 9 ms radiofrequency π pulse.