Carbon-carbon coupling reactions were carried out by using the triphenylbismuth (V) ) and a variety of olefins in the presence of palladium nanoparticles immobilized in spherical polyelectrolyte brushes (Pd@SPB) under mild conditions (50°C). The effects of the organobismuth derivatives and the unsaturated compounds and the influence of the ratio of solvents (THF and water) on the yield of cross-coupled products were studied. The most active organobismuth compound studied was triphenylbismuth bis(trifluoroacetate), Ph 3 Bi-