Unambiguous assignment of redox sites on ferrocene coupled N-heterocyclic carbene gold(I) complexes [(Fc-NHC)₂Au(I)]⁺ is critical to gain a greater mechanistic understanding of their activity in a cellular environment. Such information can be garnered with isolation and detailed characterization of the oxidized version of [(Fc-NHC)₂Au(I)]⁺. Herein we disclose a study that unambiguously illustrates redox events pertaining to [(Fc-NHC)₂Au(I)]⁺ that stem exclusively from ferrocene sites. This work also describes novel synthetic methodologies for isolating ferrocenium coupled N-heterocyclic carbene gold(I) complexes.