Cyclic voltammograms starting from open circuit potential (EOC) towards positive potentials and negative potentials, recorded on the dC12TEMPONOBF4 molecule (compound prepared with an excess of NOBF4, Figure ) showed respectively a weak oxidation peak and a high reduction peak at each first vertex, indicating a significant presence of oxidized TEMPO species coexisting with radical species. For the dC12TEMPOtBuONO/BF3 compound (prepared with tBuONO and BF₃-CH3CN, Figure ), the near absence of an oxidation peak and a higher reduction peak potential observed during the initial vertexes, combined with a +70 mV shift in the EOC relative to dC12TEMPONOBF4 compound, indicated a strong predominance of oxidized TEMPO species over the radical form. Additionally, an important decrease in the overall current indicates a significantly lower concentration of electroactive species compared to Figure . These observations point to possible side reactions altering the redox balance of the TEMPO system.