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A three-compartment ¡°H-type¡± electrolytic cell having compartments for the working, counter, and reference electrodes separated by a fine glass frit was used for voltammetry and to carry out controlled potential electrosynthesis. The experimental reference electrode was a silver/silver chloride wire prepared by deposition of AgCl onto silver, the counter electrode was a Pt mesh, and the working electrode for voltammetric analyses was either glassy carbon, nickel, gold or platinum by BASi. The electrode surfaces were pretreated using a sequence of polishing with diamond paste of decreasing particle sizes (15 to 1 ¦Ìm), interspersed by washings with nanopure water, and finally vacuum drying prior to use. The bulk coulometric technique was conducted using a graphite, nickel basket, nickel-chromium wire or platinum (Strem or BASi) basket electrode that was vacuum-dried at 120 ¡ãC for about 24 hours. The ferrocene/ferrocenium potential was determined with ferrocene in cyclic voltammetry experiments. All reported potentials are with ferrocene/ferrocenium as an internal standard, reduction-oxidation half potential (E1/2) is 0.0 volt as recommended elsewhere2, and with a precision of 5 mV. All electrochemistry was conducted using Schlenk conditions or in an MBRAUN glovebox under argon (99.9%), using a PAR 273A potentiostat interfaced to a personal computer

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