Reactivity of functionalized halo-derivatives with transition metal complexes. Synthesis and X-ray diffraction study of [Ph3P(CH2CH2COCH3)]+[PdCl3(PPh3)]- obtained by reaction of trans-[PdCl2(PPh3)2] with CH3COCH2CH2Cl

The complex [PdCl3(PPh3)]−[Ph3P(CH2CH2COCH3)]+ (I) was prepared by reacting trans-[PdCl2(PPh3)2] with CH3COCH2CH2Cl in boiling ethanol. The i.r. spectrum of (I) shows a band of strong intensity at 1717 cm−1 for v(CO) and bands attributable to v(PdCl) at 343(s), 301(w) and 277(m) cm−1. The crystal and molecular structure of complex (I) has been determined from three-dimensional X-ray diffractometer data. The complex crystallizes in the monoclinic space group P21/n. Cell parameters are as follows: a = 18.849(9), b = 21.301(9), c = 9.156(7) A, β = 92.8(1)°, Z = 4. Full-matrix least-squares refinement converged at R = 0.063 (Rw = 0.055). The anion [PdCl3(PPh3)]− has approximately square planar geometry. The cation [Ph3P(CH2CH2COCH3)]+ shows the usual angular distortions from the tetrahedral value at the phosphorus atom.