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Nine‐ and ten‐membered N‐heterocyclic carbene (NHC) ligands have been developed and for the first time their gold(I) complexes were synthesized. The protonated NHC pro‐ligands  2 a – h  were prepared by the reaction of readily available  N , N′ ‐diarylformamidines with bis‐electrophilic building blocks, followed by anion exchange. In situ deprotonation of the tetrafluoroborates  2 a – h  with  t BuOK in the presence of AuCl(SMe 2 ) provided fast access to NHC‐gold(I) complexes  3 – 10 . These new NHC‐gold(I) complexes show very good catalytic activity in a cycloisomerization reaction (0.1 mol % catalyst loading, up to 100 % conversion) and their solid‐state structures reveal high steric hindrance around the metal atom (% V  bur  up to 53.0) which is caused by their expanded‐ring architecture.

Gold(I) Complexes Stabilized by Nine‐ and Ten‐Membered N‐Heterocyclic Carbene Ligands