Synthesis and characterization of η5-tetramethylcyclopentadienyl hydrido-and -chloro-silyl-η1 -amido zirconium complexes

Authors
Vázquez García, Ana BelénUniversity of Alcalá Author; Royo Gracia, PascualUniversity of Alcalá Author
Identifiers
Permanent link (URI): http://hdl.handle.net/10017/4191
DOI: 10.1016/S0022-328X(03)00122-0
ISSN: 0022-328X
Publisher
Elsevier
Date
2003
Affiliation
Universidad de Alcalá. Departamento de Química Inorgánica
Funders
We thank Ministerio de Ciencia y Tecnología for support of this work (Project MCyT-MAT2001-1309 and predoctoral fellowship to A.B.V.
Bibliographic citation
Journal of Organometallic Chemistry, 2003, v. 671, p. 172-178
Keywords
Zirconium
Linked amido-cyclopentadienyl ligand
Synthesis
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/S0022-328X(03)00122-0
Rights
(c) Elsevier, 2003
Access rights
info:eu-repo/semantics/openAccess
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Abstract
The silylated tetramethylcyclopentadienes C5Me4(SiMeCl2)(SiMe3) (1) and C5Me4H(SiMeHCl) (3) were isolated by reaction of their corresponding trimethylsilyltetramethylcyclopentadienyl and tetramethylcyclopentadienyl lithium salts with SiMeCl3 and SiMeHCl2, respectively. Reaction of a toluene suspension of ZrCl4 with one equivalent of 1 afforded the monocyclopentadienyl zirconium complex [Zr(h5 -C5Me4SiMeCl2)Cl3] (2). Reaction of 3 with NH2 t Bu gave C5Me4H[SiMeH(NHt Bu)] (4) which was further metallated to give Li2[C5Me4SiMeH(Nt Bu)] (5), used to prepare the silyl-h1 -amido zirconium derivative [Zr(h5 -C5Me4SiMeH-h1 - Nt Bu)Cl2] (6) by reaction with ZrCl4(THF)2. Chlorination of 6 with BCl3 afforded [Zr(h5 -C5Me4SiMeCl-h1 -Nt Bu)Cl2] (12). Alkylation and amidation of 6 and 12 provided the corresponding disubstituted [Zr(h5 -C5Me4SiMeH-h1 -Nt Bu)R2] (R /Me 7, CH2Ph 8, NMe2 9) and [Zr(h5 -C5Me4SiMeCl-h1 -Nt Bu)Me2] (13) and monosubstituted [Zr(h5 -C5Me4SiMeH-h1 -Nt Bu)ClR] (R / C6F5 10, N(SiMe3)2 11) and [Zr(h5 -C5Me4SiMeCl-h1 -Nt Bu)Cl{N(SiMe3)2}] (14). All of the new compounds reported were characterized by elemental analyses and NMR spectroscopy.
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