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Synthesis of a Stable Tricobalt Carbide Cluster
Nicholas P Litak1, Shao-Liang Zheng1, Dongtao Cui1
1Department of Chemistry and Chemical Biology, Harvard University, Cambridge, Massachusetts 02138, United States.
None:
We report the synthesis and characterization of the anionic tricobalt carbide cluster [(FtbsL)Co3(μ3-C)]-. The source of the carbide ligand is a phosphorus ylide (R2MePCH2; R = Me, Ph) which substitutes pyridine in the all-cobalt(II) cluster (FtbsL)Co3(py) to afford the ylide adduct (FtbsL)Co3(CH2PMeR2). Deprotonation affords the anionic diylide cluster [(FtbsL)Co3(κ2-η1:η1-(CH2)2PR2)]- which eliminates MePR2 upon heating to furnish the anionic methylidyne cluster [(FtbsL)Co3(μ3-CH)]-. Oxidation of the anionic methylidyne complex with ferrocenium hexafluorophosphate generates the diamagnetic methylidyne complex (FtbsL)Co3(μ3-CH). The methylidyne ligand can be deprotonated with Li- or KN(SiMe3)2 to afford carbide complexes (FtbsL)Co3(μ4-C)Li(OEt2) or [K(C222)][(FtbsL)Co3(μ3-C)], respectively. Isotopic enrichment of the carbide with 13C reveals downfield-shifted 13C NMR chemical shifts (δ/ppm) of 389, Co3(μ3-CH); 731, Co3(μ4-CLi); and 769, Co3(μ3-C)-; the latter of which is the most downfield resonance for a transition metal carbide reported to date.
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