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 C-60 in toluene reacts with Pd(dba)(2) or Pd-2(dba)(3) (dba = dibenzylideneacetone) and monophosphanes in a 1:1:2 molar ratio to give the corresponding Pd monophosphane fullerene derivatives [Pd(eta(2)-C-60)L-2] [L = P(2-Fu)(3) (Fu = furyl) 1; L = P(2-Fu)Ph-2 2; L = PPh2H 3; L = P(Fc)Ph-2 (Fc = ferrocenyl) 4; L = P(Fc)(2)Ph 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(eta(2)-C-60){Ph2PCH2(CH2OCH2)(n)CH2PPh2}] (n = 1 6; n = 2 7; n = 3 8) and [Pt(eta(2) -C-60){Ph2PCH2(CH2OCH2)(n)CH2PPh2}] (n = 1 9; n = 2 10; n = 3 11). All the new fullerene complexes 1-11 were characterized by elemental analysis, IR, H-1 NMR and P-31 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. (C) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004.