ISOLATION AND X-RAY CHARACTERIZATION OF A NEW CRYSTAL MODIFICATION OFPD-6(MU(2)-CO)(6)(MU-DPPM)(3) DURING THE SYNTHESIS OF THE NOVEL FLUXIONAL TRIANGULO PD(0) COMPLEX [PD-3(MU(2)-CO)(3)(DPPM)(2)](N) (N=1 OR 2)

The one-step synthesis of a new type of fluxional Pd-0-CO-bis(diphenyl phosphino)methane (dppm) cluster from Pd-II acetate is reported and th e complex has been identified as [Pd-3(mu(2)-CO)(3)(mu-dppm)(2)](n) (n = 1 or 2, 8) on the basis of microanalytical and spectroscopic data. During repeated attempts to grow suitable crystals of this complex for X-ray analysis, a second crystal modification (7) of Pd-6(mu(2)-CO)(3 )(mu-dppm)(3) was isolated as a 0.5 toluene solvate. This modification contains two Pd-6(mu(2)-CO)(3)(mu-dppm)(3) molecules in the asymmetri c unit cell each showing minor structural differences from each other as well as from the previously characterized Pd-6(mu(2)-CO)(6)(mu-dppm )(3) . CH2Cl2 (6). (C) 1997 Elsevier Science Ltd.