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Synthesis and reactivity of imido niobium complexes containing the functionalized (dichloromethylsilyl)cyclopentadienyl ligand

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Authors
Postigo Galindo, LorenaUniversity of Alcalá Author; Sánchez-Nieves Fernández, JavierUniversity of Alcalá Author; Royo Gracia, PascualUniversity of Alcalá Author
Identifiers
Permanent link (URI): http://hdl.handle.net/10017/4172
DOI: 10.1016/j.ica.2006.02.026
ISSN: 0020-1693
Publisher
Elsevier
Date
2007
Affiliation
Universidad de Alcalá. Departamento de Química Inorgánica
Funders
Universidad de Alcalá
Bibliographic citation
Inorganica Chimica Acta, 2007, v.360, n.4, p.1305-1309
Keywords
Niobium
Constrained-geometry
Half-sandwich
Imido
Monocyclopentadienyl
Project
MAT2004-02614 (Ministerio de Educación y Ciencia)
GR/MAT/0622/2004 (Comunidad de Madrid)
Document type
info:eu-repo/semantics/article
Version
info:eu-repo/semantics/publishedVersion
Publisher's version
http://dx.doi.org/10.1016/j.ica.2006.02.026
Rights
© Elsevier, 2006
Access rights
info:eu-repo/semantics/openAccess
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Abstract
The niobium complex [NbCpClCl4] (CpCldouble bond; length as m-dashη5-C5H4(SiCl2Me)) (1) with a functionalized (dichloromethylsilyl)cyclopentadienyl ligand was isolated by the reaction of [NbCl5] with C5H4(SiCl2Me)(SiMe3). Complex 1 was a precursor for the imido silylamido derivative [NbCpNCl2(NtBu)] (CpNdouble bond; length as m-dashη5-C5H4[SiClMe(NHtBu)]) (2) after addition of LiNHtBu, which subsequently gave the dichlorosilyl compound [NbCpClCl2(NtBu)] (3) when reacted with SiCl3Me. Addition of LiNHtBu to complex 2 gave the niobium amido complex [NbCpNCl(NHtBu)(NtBu)] (4), which slowly evolved with exchange of the niobium-amido and the silicon-chloro groups to give the dichloroniobium complex [NbCpNNCl2(NtBu)] (CpNNdouble bond; length as m-dashη5-C5H4[SiMe(NHtBu)2]) (5). Reaction of 2 with excess LiNHtBu gave the silyl-η-amido constrained geometry complexes [Nb{η5-C5H4[SiMe(NHtBu)(-η-NtBu)]}(NHtBu)(NtBu)] (6) and [Nb{η5-C5H4[SiClMe(-η-NtBu)]}(NHtBu)(NtBu)] (7), whereas addition of one equimolecular amount of LiNHtBu to 5 in C6D6 afforded complex [NbCpNNCl(NHtBu)(NtBu)] (8). All of the new complexes were characterized by 1H, 13C and 29Si NMR spectroscopy.
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