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Half-sandwich imido complexes of niobium bearing alkyne, benzyne and benzylidene ligands: relatives of the zirconocene family

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Citation

Chan, M. C. W., Cole, J. M., Gibson, V. C., Howard, J. A. K., Lehmann, C. W., Poole, A. D., et al. (1998). Half-sandwich imido complexes of niobium bearing alkyne, benzyne and benzylidene ligands: relatives of the zirconocene family. Journal of the Chemical Society, Dalton Transactions, (1), 103-112. doi:10.1039/A705197B.


Cite as: http://hdl.handle.net/11858/00-001M-0000-0024-6FE3-2
Abstract
Reactions of [Nb(C5H5)(NC6H3Pri2-2,6)Cl2] 1a and [Nb(C5Me5)(NCH3Pri2-2,6)Cl2] 1b with 1 and 2 equivalents of benzylpotassium respectively gave the niobium benzyl derivatives [Nb(C5H5)(NC6H3Pri2-2,6)Cl(CH2Ph)] 2 and [Nb(C5Me5)(NC6H3Pri2-2,6)(CH2Ph)2] 3. Treatment of 3 with trimethylphosphine afforded the benzylidene complex [Nb(C5Me5)(NC6H3Pri2-2,6)(PMe3)(=CHPh)] 4. Complex 1a reacted with phenylmagnesium chloride in the presence of PMe3 to give [Nb(C5H5)(NC6H3Pri2-2,6)Ph2(PMe3)] 5 which upon heating at 70 °C in heptane, converts to the η2-benzyne complex [Nb(C5H5)(NC6H3Pri2-2,6)(η2-C6H4)(PMe3)] 6. The niobium(III) complexes [Nb(CH5)(NCH4But-2)(PMe3)2] 8a and [Nb(C5Me5)(NCHPri2-2,6)(PMe3)] 8b were obtained upon magnesium reduction of 1a and 1b respectively in the presence of an excess of PMe3. They were converted into [Nb(C5H5)- (NC6H4But-2)(η2-R1C≡CR2)(PMe3) (R1 = R2 = Ph 9a; R1 = Ph, R2 = H 9b) and [Nb(C5Me5)(NC6H3Pri2-2,6)-(η2-PhC≡CPh)(PMe3)] 9c upon treatment with the appropriate alkyne. The molecular structures of the 2-tertbutylimido complexes [Nb(C5H5)(NCHBut-2)Cl2] 7 and 9a have been determined.