The methylpalladium and ‐platinum complexes [Pd(AcNac)(PMe3)CH3], [Pd(SacNac)(PMe3)CH3], and [Pt(SacNac)(PMe3)CH3] have been prepared from protonation reactions between AcNac [H3CC(O)CHC(NAr)CH3; Ar = 2,6‐iPr‐C6H3 = Dipp (L1); Ar = 2,4,6‐MeC6H2 = Mes (L2)] or SacNac [H3CC(S)CHC(NAr)CH3; Ar = 2,6‐iPr‐C6H3 = Dipp (L3); Ar = 2,4,6‐MeC6H2 = Mes (L4)] ligands and dimethyl–metal complexes of the composition [M(L′)Me2] (M = Pd, L′ = tmeda = N,N,N′N′‐tetramethylethylenediamine; M = Pt, L′ = cod = 1,5‐cyclooctadiene) and PMe3 in acetonitrile. Only one isomer was formed in each case and X‐ray crystallographic analysis showed that the PMe3 co‐ligand is found in the cis position with respect to the sulfur or oxygen atom in all complexes.
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