Crystal structure of trans-(dicyano)bis(triphenylphosphine)palladium(II) dichloromethane solvate.

was obtained from the reaction of Pd(PPh3)4 with Me3SiCN (1:1 molar ratio) in benzene (at 80 ̊C for 2 h). Crystals suitable for X-ray diffraction analysis were obtained by recrystallization from a mixture of CH2Cl2 and C6H6 (ca. 1:4 by volume). Table 1 summarizes the crystal and experimental data. During the data collection at room temperature, decay was not observed. All intensity data were corrected for Lorentz and polarization factors, but not for absorption. The structure was solved by a direct method (sir 92), and refined by full-matrix least-squares with anisotropic thermal parameters for the non-hydrogen atoms. The hydrogen atoms were located geometrically and were not refined. The final atomic parameters are given in Table 2. The Pd complex molecule and the solvate molecule lay on a crystallographic twofold axis. Some selected geometric parameters are given in Table 3. As shown in Fig. 2, the Pd atom was coordinated by two P and two C atoms in squareplanar arrangement. The coordination geometry around Pd atom was essentially identical with the geometries found in 469 ANALYTICAL SCIENCES MARCH 2001, VOL. 17 2001 © The Japan Society for Analytical Chemistry