Abstract A catalytic method to synthesize a broad array of cyclometalated (C^N)gold(III) complexes is reported here. An unprecedented Rh‐to‐AuIII transmetalation allows the facile transfer of (C^N) ligands between these two metals in a redox‐neutral process. The reaction employs commercially available precursors and proceeds under mild and environmentally benign conditions. Both experimental and computational studies support a multistep transmetalation from rhodium to gold as the underlying mechanism for these transformations. This process involves first, a rate‐determining transfer of the C ligand followed by the subsequent incorporation of the N donor to form the monocyclometalated (C^N)gold(III) species.
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