Protonolysis of β-diketiminato (nacnac) rare-earth metal bis-alkyl complexes L nacnac LnR 2 (THF) (Ln = Y and Lu) with 2 equiv of Ph 2 PNHPh or Ph 2 PCH 2 NHPh afforded the bis-amido complexes L nacnac Y(Ph 2 PNPh) 2 and L nacnac Ln-(Ph 2 PCH 2 NPh) 2 (Ln = Y and Lu). Metalation of the latter complexes with 1 equiv of Ni(COD) 2 led to the isolation of unusual heterobimetallic Ni(II)−Ln(III) complexes formed via P−C bond cleavage of one [Ph 2 PCH 2 NPh] − ligand. Notably, both the imine PhNCH 2 and phosphide Ph 2 P − fragments from the P−C bond cleavage were trapped in the Ni(II)−Ln(III) core with a relatively weak interaction between the two metal centers. The Ni(II)−Y(III) complex have exhibited versatile reactivity, such as coordination of isonitrile to the Ni(II) center, insertion of nitrile with the coordinated imine, and ring-opening of the epoxide by nucleophilic attack from the phosphide group.
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