spectra were recorded
on a Cary 8454 spectrophotometer. 1H NMR spectra were recorded
on a 400 MHz Bruker Avance III HD spectrometer (equipped with a 5-mm
BB/1H SmartProbe) at a temperature of 298 K in tetrahydrofuran
(THF)-d8 and referenced to residual THF
protons at 3.48 and 2.37 ppm. High-resolution (HR) mass spectra were
recorded (typically in the positive-ion mode) on a Thermo LTQ Orbitrap
XL spectrometer equipped with an electrospray ION MAX source. Elemental
analyses were performed by Atlantic Microlab, Inc.
Cyclic voltammetry
was carried out at 298 K with an EG&G model 263A potentiostat
having a three-electrode system: a glassy carbon working electrode,
a platinum wire counterelectrode, and a standard calomel reference
electrode (SCE). Tetra-n-butylammonium perchlorate,
recrystallized twice from absolute ethanol and dried in a desiccator
for at least two weeks, was used as the supporting electrolyte. Anhydrous
CH2Cl2 (Sigma-Aldrich) was used as a solvent.
The reference electrode was separated from the bulk solution by a
fritted-glass bridge filled with a saturated AgCl/KCl mixture. The
electrolyte solution was purged with argon for at least 2 min, and
all measurements were carried out under an argon blanket. All potentials
were referenced to the SCE.