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 121 for v(C=O) and bands attributable to v(Pd-Cl) at 343(s), 301(w) and 277(m) cm 121. 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) \uc5, \u3b2 = 92.8(1)\ub0, Z = 4. Full-matrix least-squares refinement converged at R = 0.063 (Rw =0.055). The anion [PdCl3(PPh3)] 12 has approximately square planar geometry. The cation [Ph3P(CH2CH2COCH3)]+ shows the usual angular distortions from the tetrahedral value at the phosphorus atom