The synthesis of new Pd/Pt metallacyclopropa[60]fullerene complexes containing unsymmetrical phosphorus ylides [Ph2P(CH2)nPPh2=C(H)C(O)C6H4-p-OMe] (n=1, (Y1); n=2, (Y2)) has been reported. The synthesized complexes exhibit different structures, including two P,C– chelated [(η2-C60)Pd(κ2-Y1)] (1) and [(η2-C60)Pt(κ2- Y1)] (2) complexes and two P-coordinated [(η2-C60)Pd(Y2)2] (3) and [(η2-C60)Pt(Y2)2] (4) complexes with chain structures. Characterization of all compounds was performed by multi-neclear NMR spectroscopies (1H, 13C and 31P NMR) and other conventional techniques such as IR, UV–Vis, SEMand cyclic voltammetry (CV) analyses. In this regard, the presence of all characteristic chemical shifts in the IR and NMR spectra proposed the formation of desired products. Also, theoretical studies were used to investigate the nature of metal–ligands in all complexes. In addition, a comparison between the catalytic activity of Pd complexes 1 and 3 was evaluated in the Suzuki-Miyaura reaction of various aryl chlorides with phenylboronic acid, which revealed ameaningful difference between the catalytic activity of complexes 1 and 3.
