Anionic (nitrophenyl)palladium(II) carbonyls. Crystal structure of cis-[PPh3(CH2Ph)][Pd(C6H 3Me-2,NO2-6)Cl2(CO)]

Article abstract of DOI:10.1021/om00057a017

Complexes [PPh₃(CH₂Ph)][Pd(R)Cl₂(CO)] [R = C₆H₃Me-2,NO₂-6 (1), C₆H₂(NO)₃-2,4,6 (2)] can be isolated by carbonylation, at room temperature and atmospheric pressure, of [PPh₃(CH₂Ph)]₂[Pd(R)Cl(μ-Cl]₂. Complex 1 is the first example of an organocarbonylpalladium(II) complex characterized by an X-ray diffraction study. Crystals are triclinic, space group P1, with Z = 2 in a unit cell of dimensions a = 10.446 (5) A?, b = 12.538 (7) A?, c = 14.148 (6) A?, α = 65.40 (2)°, β = 74.17 (2)°, and γ = 72.83 (2)°. The structure has been solved by Patterson and Fourier methods and refined by full-matrix least squares on the basis of 1274 observed reflections to R and R_w values of 0.0319 and 0.0440. In the anionic complex the Pd atom is in a square-planar arrangement with two Cl atoms in cis positions and the carbonyl group and the 2-methyl-6-nitrophenyl ligand trans to them. The Pd-CO bond [Pd-C = 1.853 (10) A?] is discussed on the basis of the IR and X-ray data.