Synthesis, Characterization and Properties of Transition Metal Pd/Pt [60]Fullerene Complexes Containing Phosphane Ligands − Crystal Structure of [Pd(η2‐C60){Ph2PCH2(CH2OCH2)2CH2PPh2}]

A solution of C60 in toluene reacts with Pd(dba)2 or Pd2(dba)3 (dba = dibenzylideneacetone) and monophosphanes in a 1:1:2 molar ratio to give the corresponding Pd monophosphane fullerene derivatives [Pd(η2‐C60)L2] [L = P(2‐Fu)3 (Fu = furyl) 1; L = P(2‐Fu)Ph2 2; L = PPh2H 3; L = P(Fc)Ph2 (Fc = ferrocenyl) 4; L = P(Fc)2Ph 5], whereas reaction with M(dba)2 (M = Pd, Pt) and subsequent treatment with diphosphanes in 1:1:1 molar ratio afforded the corresponding Pd/Pt diphosphane fullerene complexes [Pd(η2‐C60){Ph2PCH2(CH2OCH2)nCH2PPh2}] (n = 1 6; n = 2 7; n = 3 8) and [Pt(η2‐C60){Ph2PCH2(CH2OCH2)nCH2PPh2}] (n = 1 9; n = 2 10; n =3 11). All the new fullerene complexes 1−11 were characterized by elemental analysis, IR, 1H NMR and 31P NMR spectroscopy, as well as by X‐ray diffraction analysis (for 7). The optical limiting properties of 3−5 were determined and the possible pathways for the “one pot” reactions leading to 1−11 are briefly discussed. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004)