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A new tripod PPN bridging ligand and its copper, silver and palladium complexes: Syntheses, characterizations and X-ray structures

A new tripod bridging ligand 2-{bis(diisopropylphosphino)methyl}-1-methylimidazole, MeImCH(Pi-Pr2)2 (PPN) was synthesized conveniently by reacting 2-{bis(trimethylsilyl)methyl}-1- methylimidazole and chlorodiisopropylphosphine. The dicationic dinuclear complex [Cu2(PPN)2][CIO4]2 (1) was prepared by the reaction of the ligand with [Cu(MeCN)4]ClO4 in acetonitrile. The reaction of the ligand with AgNO3 in propane-2-ol followed by addition of NH4PF6 led to the formation of a similar type complex [Ag2(PPN)2][PF6]2 (2). The X-ray diffraction studies of 1 and 2 revealed a mu2-eta1:eta2 tripod-like bonding of the PPN ligand, with one P and one N atom chelating to one metal ion and the remaining one P atom binds to another metal ion, affording a face-to-face type molecule. An eight-membered M2P4C2 and a 10-membered M2P2N2C4 ring are thus formed with this new functional diphosphine ligand. In both complexes the two metal ions are held in very close proximity [2.6707 A? for 1 and 2.859(3) A? for 2]. Coplex 1 underwent a rapid ligand exchange process in solution. Besides these dinuclear complexes the ligand also afforded a mononuclear palladium complex, [PdCl2(PPN)] (3), when it was treated with an equimolar amount of [PdCl2(PhCN)2] in benzene. In 3 the ligand acts as a bidentate chelate through its two phosphorus atoms, leaving the imidazole donor dangling. On the other hand, a P,P-bridged dinuclear Pd(I) complex [Pd2Cl2(PPN)2] (4) was achieved by reacting two moles of the ligand with one mole of [PdCl2(PhCN)2], followed by the addition of one mole of Pd(dba)2 [dba = dibenzylideneacetone].

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Reference£º
Chapter 1 An introduction to palladium catalysis,
Palladium/carbon catalyst regeneration and mechanical application method