New palladacyclopentadiene complexes containing an N,P-donor setting. Crystal structure of [Pd{C4(COOMe)4}(o-Ph2PC6H4-CH=NiPr)] (original) (raw)

2002, Inorganica Chimica Acta

The synthesis of palladacyclopentadiene derivatives with the mixed-donor bidentate ligands o-Ph 2 PC 6 H 4 CH NR (N P) has been achieved. The new complexes of general formula [Pd{C 4 (COOMe) 4 }(o-Ph 2 PC 6 H 4 CH NR)] [R=Me (1), Et (2), i Pr (3), t Bu (4), NH Me (5)] have been prepared by reaction between the precursor [Pd{C 4 (COOMe) 4 }] n and the corresponding iminophosphine. The polymer complex [Pd{C 4 (COOMe) 4 }] n also reacts with pyridazine (C 4 H 4 N 2) to give the insoluble dinuclear complex [Pd{C 4 (COOMe) 4 }(m-C 4 H 4 N 2)] 2 (6), which has been successfully employed as precursor in the synthesis of pyridazine-based palladacyclopentadiene complexes. The reaction of 6 with tertiary phosphines yielded complexes containing an N,P-donor setting of formula [Pd{C 4 (COOMe) 4 }(C 4 H 4 N 2)(L)] (L =PPh 3 (7), PPh 2 Me (8), P(p-MeOC 6 H 4) 3 (9), P(p-FC 6 H 4) 3 (10)). The new complexes were characterized by partial elemental analyses and spectroscopic methods (IR, 1 H, 19 F and 31 P NMR). The molecular structure of complex 3 has been determined by a single-crystal diffraction study, showing that the iminophosphine acts as chelating ligand with coordination around the palladium atom slightly distorted from the square-planar geometry.

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