Abstract
The incorporation of a PPC donor ligand set onto nickel is described. While C–H activation routes using Ni(II) precursors and benzyl- and phenethyl-substituted diphosphines But2PCH2CH2P(But)R failed, success was achieved via oxidative addition of the 2-bromo-benzyl-ligand precursor But2PCH2CH2P(But)(CH2-o-C6H4Br) with Ni(COD)2 to generate [κ3-BnPPC]NiBr. Subsequent reaction with KBEt3H resulted in decomposition unless PPh3 was present, which allowed isolation of the tricoordinate Ni(0) complex [κ2-BnPP]Ni(PPh3). Reaction of [κ3-BnPPC]NiBr with EtMgCl also resulted in the formation of the Ni(0) ethylene complex, [κ2-BnPP]Ni(η2-C2H4), via β-elimination followed by reductive elimination. Deuterium-labeling studies are consistent with a reversible β-elimination process prior to reductive elimination, which scrambles the deuterium isotopes. Reaction of [κ3-BnPPC]NiBr with CH3Li results in the formation of the Ni(II) methyl complex, [κ3-BnPPC]Ni(CH3). Heating this species in the presence of PPh3 results in the ...
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