in dried glassware under an Ar atmosphere unless stated otherwise.
1,2-Dimethoxyethane (DME) (CHROMASOLV, for HPLC grade, Sigma-Aldrich)
was dried over activated basic Al2O3, filtered,
and distilled over liquid Na/K alloy. Caution: All steps involving
Na/K alloy should be carried out with extreme caution under strict
exclusion of air or moisture, under inert gas and appropriate personal
protection (hood, blast shields, face shield, protective, and fire-resistant
clothing) should be used and worn at all times. Tetrabutylammonium
hexafluorophosphate (TBAPF6) (for electrochemical analysis,
Sigma-Aldrich) was dried in vacuum (∼10–2 mbar) at 100 °C for 24 h. TBAPF6 (0.15 M) in DME
was prepared in a glovebox and used without further purification.