Preparation and characterization of PdII-ylide complexes of type 3-2-XC3H4)>BF4 (X=H, Me; R=p-C6H4OMe, C(Me)3, Me, C6H11, p-c6H4NO2). Crystal structure of (η3-2-MeC3H4)>BF4

Article abstract of DOI:10.1016/0022-328X(89)87191-8

Seven compounds of general formula 3-2-XC3H4)>BF4 (X=H, R=p-C6H4OMe (1), R=C(Me)3 (2); X=Me, R=p-C6H4OMe (3), C(Me)3 (4), Me (5), C6H11 (6), p-C6H4NO2 (7)) have been prepared by chloride abstraction from PdCl(η³-2-XC3H4) (X=H, Me) with AgBF4 and subsequent reaction of the cationic intermediate with the appropriate isocyanide ligand.All the complexes have been characterized by analitical and spectroscopic (IR, 1H and 31P<1H> NMR) data.They have been shown to be mixture of two diastereoisomeric forms arising from the simultaneous presence on the palladium atom of the asymmetric ylidic carbon atom and the η³-allyl ligand.The determination of the crystal structure of complex 4 showed that in the solid state only diastereoisomer is present.The crystals are monoclinic, space group Pc with a 9.833(3), b 14.383(4), c 11.762(4) Angstroem, β 114.68(3) deg, and Z=2.Final full-matrix least-squares refinement, based on 2413 reflections, convergated to R=0.050.The keto-stabilized ylide ligand is C bonded to the metal with a Pd-C distance of 2.175(9) Angstroem.