Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) of DiKTa3 in degassed DCM with 0.1 M [ n Bu4N]PF6 as the supporting electrolyte and Fc/Fc + as the internal reference (0.46 V vs. SCE) were measured to experimentally determine the HOMO and LUMO energy levels (Figure ). DiKTa3 shows a reversible reduction wave and an irreversible oxidation wave, electrochemical behavior that is consistent with that of DiKTa. The reduction potential, Ered, and oxidation potential, Eox, of DiKTa3, obtained from the peak values in the DPV are -1.02 and 1.83 V vs. SCE. Both values are cathodically shifted compared to DiKTa (Ered of -1.34 V and Eox of 1.78 V vs. SCE) and closer to those of Hel-DiDiKTa (Ered of -1.16 V and Eox of 1.81 V vs. SCE). The corresponding HOMO and LUMO energies are -6.17 and -3.32 eV with energy gap DE of 2.85 eV (Table ).