X-ray diffraction studies of group 9 transition-metal complexes containingan sp(3) C-H activated functionalized triphenylphosphine

Treatment of the hemilabile tertiary phosphino amide o-Ph2PC6H4CH2N(Me)C(O) Et (DPPBA; 1) with the appropiate Rh(I) or Ir(I) precursor complex results in cyclometalation by oxidative addition of the benzylic C-H bond to the me tal center. The solution structures of the two synthesized complexes [RhH(P Ph3)(2)(DPPBA)][PF6] (2) and [IrH(1,5-COD)(DPPBA][BF4] (3) have been unambi guously identified by various NMR spectroscopic techniques. Also, single-cr ystal X-ray diffraction studies have been performed for 2 and 3. These are the first crystal structures obtained with DPPBA as a ligand, giving final confirmation of the capability of 1 to trischelate in platinum group metal complexes.