Metals in organic syntheses. XIII. The isolation and molecular structure of trans-[PdCl(COC6H13-n)(PPh3)2], an intermediate in the hydrocarboalcoxylation of 1-hexene catalyzed by the precursor trans-[PdCl2(PPh3)2]

Abstract The complex trans -[PdCl(COC 6 H 13 -n)(PPh 3 ) 2 ] has been isolated in the course of 1-hexene hydrocarboalkoxylation catalyzed by the precursor trans -[PdCl 2 (PPh) 3 ) 2 ] in EtOH. The catalytic activity of the precursor and that of the acyl complex are practically the same, thus suggesting that the latter complex is an intermediate in the catalysis. The IR spectrum of the acyl complex shows ν(CO) at 1685 cm −1 . The crystal and molecular structure of the complex was determined from three dimensional X-ray diffractometer data. The complex crystallizes in the triclinic space group P 1 . Cell parameters were: a = 17.330(8), b = 11.963(7), c = 10.100(7) », α = 112.4(1), β = 97.7(1), γ = 99.8(1)°, Z = 2. Full-matrix least-squares refinement converged at R = 0.067. The coordination about the metal significantly deviates from planarity towards a tetrahedral configuration. No unusual dimensions were shown.