Bis [o-(hydrosilyl) phenyl] cuprates and bis [o-(fluorosilyl) phenyl] cuprates were prepared by reacting [o-(hydrosilyl) phenyl] lithiums and [o-(fluorosilyl) phenyl] lithiums, respectively, with copper salts, such as CuCN and Cu (OPiv) 2. The phenylcuprates underwent oxidative coupling to afford 2, 2′-bis (hydrosilyl) biphenyls and 2, 2′-bis (fluorosilyl) biphenyls.