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

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 th...

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Detalles Bibliográficos
Autores: Nicolás Utrilla, María Pilar, Royo Gracia, Pascual
Tipo de recurso: artículo
Fecha de publicación:2005
País:España
Institución:Universidad de Alcalá (UAH)
Repositorio:e_Buah Biblioteca Digital Universidad de Alcalá
Idioma:inglés
OAI Identifier:oai:ebuah.uah.es:10017/4177
Acceso en línea:http://hdl.handle.net/10017/4177
https://dx.doi.org/10.1016/j.ica.2004.09.017
Access Level:acceso abierto
Palabra clave:Niobium
Tantalum
Imido
Cyclopentadienyl
Ciencia
Química inorgánica
Science
Chemistry, inorganic
Descripción
Sumario: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.