Synthesis and characterization of η5-cyclopentadienyl-silylallyl niobium and tantalum complexes

Authors
Nicolás Utrilla, María Pilar; Royo Gracia, PascualUniversity of Alcalá Author
Identifiers
Permanent link (URI): http://hdl.handle.net/10017/4177
DOI: 10.1016/j.ica.2004.09.017
ISSN: 0020-1693
Publisher
Elsevier
Date
2005
Affiliation
Universidad de Alcalá. Departamento de Química Inorgánica
Funders
Financial support of our work by MCyT (Project MAT2001-1309) is gratefully acknowledged.
Bibliographic citation
Inorganica Chimica Acta, 2005, v. 358, p. 1494-1500
Keywords
Niobium
Tantalum
Imido
Cyclopentadienyl
Project
MAT2001-1309 (Ministerio de Ciencia y Tecnología)
Document type
info:eu-repo/semantics/article
Version
info:eu-repo/semantics/publishedVersion
Publisher's version
http://dx.doi.org/10.1016/j.ica.2004.09.017
Rights
(c) Elsevier, 2005
Access rights
info:eu-repo/semantics/openAccess
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Abstract
Reaction of the disilylcyclopentadiene 1,1-[SiMe2(CH2CHdouble bond; length as m-dashCH2)]2C5H4 with NbCl5 gave the new allylsilyl-substituted monocyclopentadienyl niobium complex [Nb{η5-C5H4SiMe2(CH2CHdouble bond; length as m-dashCH2)}Cl4]. This compound was reacted with LiNHtBu or NH2tBu to give the imido derivative [Nb{η5-C5H4SiMe2(CH2CHdouble bond; length as m-dashCH2)}(NtBu)Cl2], which was further alkylated to the imido alkyl complexes [Nb{η5-C5H4SiMe2(CH2CHdouble bond; length as m-dashCH2)}(NtBu)R2] (R = Me, CH2Ph) and [Nb{η5-C5H4SiMe2(CH2CHdouble bond; length as m-dashCH2)}(NtBu)Cl (CH2Ph)]. Reaction of the imido complexes with the corresponding lithium cyclopentadienides gave the dicyclopentadienyl-imido complexes [M(η5-C5R5){η5-C5H4SiMe2(CH2CHdouble bond; length as m-dashCH2)}(NtBu)Cl] (M = Nb, Ta; R = H, Me). Metallocene dichlorides [M(η5-C5R5){η5-C5H4SiMe2(CH2CHdouble bond; length as m-dashCH2)}Cl2] (M = Nb, Ta; R = H, Me) were easily prepared by reduction with Na/Hg and simultaneous transmetallation of [Ta(η5-C5R5)Cl4] with Li[C5H4SiMe2(CH2CHdouble bond; length as m-dashCH2)] and of [Nb{η5-C5H4SiMe2(CH2CHdouble bond; length as m-dashCH2)}Cl4] with Li(C5R5). All of the new compounds have been characterized by elemental analysis, and IR and NMR spectroscopy.
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