The molecular structure of chlorothiomethoxymethyl-bis(triphenylphosphine)palladium(II) methylenechloride solvate at −160°C

Abstract

The precise molecular structure of [PdCl(CH 2SCH 3)(PPh 3) 2] has been determined from three-dimensional X-ray diffraction data collected at −160°C. The CH 2Cl 2 solvated crystal ([PdCl(CH 2SCH 3)(PPh 3) 2 · CH 2Cl 2]) belongs to the monoclinic system, space group P2 1/ n, with four formula units in a cell of dimensions: a 14.973(3), b 15.333(3), c 17.377(3) Å and β 115.77(1)° at −160°C. The structure was solved by the conventional heavy atom method and refined by the least-squares procedure to R = 0.035 for observed reflections. The geometry around the palladium atom is square-planar. The phosphorus atoms of the two triphenylphosphine ligands are mutually trans. The CH 2SCH 3 group is bonded to the palladium atom only through the PdC σ-bond and the sulfur atom is not bonded to the metal atom (PdC(1) 2.061(3), SC(1) 1.796(3), SC(2) 1.817(5), Pd⋯S 2.973(1) Å, PdC(1)S 100.64(14)° and C(1)SC(2) 101.28(18)°). The structure is in contrast to that of [PdCl(CH 2SCH 3)(PPh 3)], in which both the carbon and sulfur atoms of the CH 2SCH 3 group are bonded to the palladium atom.