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Synthesis and characterization of heteromultinuclear Ni/M clusters (M = Fe, Ru, W) including a paramagnetic
Hsien-Cheng Yu1, Joshua Telser2, Neal P Mankad1
1Department of Chemistry, University of Illinois at Chicago, 845 W. Taylor St., Chicago, Illinois 60607, United States.
Abstract:
A diverse range of heteromultinuclear NiI/[MCO] clusters (MCO = CpFe(CO)2, CpRu(CO)2, Cp*W(CO)3) supported by a N-heterocyclic carbene ligand have been synthesized by reacting the NiI precursor, [IPrNi(μ-Cl)]2, with [MCO]- reagents under various conditions. Clusters with Ni2Fe2, NiFe2, Ni2Ru, Ni2Ru2, NiRu2, and Ni2W, and NiW cores were all characterized using NMR and IR spectroscopies and X-ray crystallography. The NiI-containing paramagnetic heterobinuclear species, IPrNi-Wp* (7), was further characterized by EPR spectroscopy and DFT calculations. Notably, unlike previously studied (NHC)CuI-[MCO] derivatives, complex 7 was found to coordinate Lewis bases like 3-chloropyridine to produce (IPr)(3-Clpy)NiWp* (9). Complex 9 further underwent thermolytic C-Cl activation, proposed to involve NHC-free [(3-Clpy)Ni(μ-Wp*)]2 (10), to provide the C-arylated N-heterocyclic carbene product, [IPr(py-3-yl)]+[Cp*WCl2(CO)2]- (11).
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