Inorganic Chemistry, Vol.33, No.21, 4804-4806, 1994
Dichlorobis(Tricyclohexylphosphine)Palladium(II) - Synthesis and Crystal-Structure - An Exceptionally Simple and Efficient Preparation of bis(Tricyclohexylphosphine)Palladium(0)
Dichlorobis(tricyclohexylphosphine)palladium(II), 1, is prepared in quantitative yield by the reaction of Na-2[PdCl4] with Cy(3)P in aqueous ethanol. Complex 1 possesses trans geometry in solution (NMR) and in the solid state (X-ray diffraction). The reaction between 1 and concentrated alkali in the presence of tricyclohexylphosphine and catalytic amounts of 18-crown-6 results in bis(tricyclohexylphosphine)palladium(0) in 85-90% yield. Crystallographic data for 1 : space group P1, a = 10.161(4) Angstrom, b = 10.604(4) Angstrom, c = 9.902(4) Angstrom, V = 916.0(6) Angstrom(3), Z = 1, R = 0.027, R(w) = 0.030.
Keywords:ALPHA-KETO ESTERS;PALLADIUM COMPLEXES;CATALYZED CARBONYLATION;PHOSPHINE COMPLEXES;ARYL CHLORIDES;PLATINUM;TRANS-DICHLOROBIS(TRIPHENYLPHOSPHINE)PALLADIUM(II);HALIDES;ALKALI