gold-catalyzed C(sp3)–C(sp2) Suzuki–Miyaura coupling reaction facilitated by ligand-enabled Au(I)/Au(III) redox catalysis was developed. The cross-coupling of alkylorganometallics was first realized in the redox catalytic cycle in gold chemistry, without the use of external oxidants. This gold-catalyzed C(sp3)–C(sp2) coupling reaction allows a variety of alkyl chain and useful methyl trifluoroborates to react