H2N2V1, Main, Exploration, bibRecord, 000806

Zirconium complexes supported by an N-perfluoro-arylated diamidopyridyl ligand: synthesis of hydrazinediido complexes.

Identifieur interne : 000806 ( Main/Exploration ); précédent : 000805; suivant : 000807

Zirconium complexes supported by an N-perfluoro-arylated diamidopyridyl ligand: synthesis of hydrazinediido complexes.

Auteurs : Solveig A. Scholl [Allemagne] ; Gudrun T. Plundrich ; Hubert Wadepohl ; Lutz H. Gade

Source :

Inorganic chemistry [ 1520-510X ] ; 2013.

RBID : pubmed:23941662

Abstract

The N-perfluoro-phenylated pyridyldiamine H2N2(PFP)N(py) (1) has been prepared by a palladium-catalyzed coupling of hexafluorobenzene and the diamine (H2NCH2)2C(CH3)(2-C5H4N) using the palladacycle trans-di(μ-acetato)bis[o-(di-o-tolylphosphino)benzyl]palladium(II) as catalyst. Reactions of H2N2(PFP)N(py) and Zr(NMe2)4 at room temperature or 90 °C led to the complexes [(N(PFP)N2(TFAP)N(py))ZrF(NMe2)] (2) and [(N2(TFAP)N(py))ZrF2] (3) in which one or two dimethylamido groups replaced one or two ortho fluorine atoms of the pentafluorophenyl groups in the ligand. Reaction of Me3SiX (X = Cl, I) with [(N2(TFAP)N(py))ZrF2] (3) resulted in the formation of mixed halogenated complexes [(N2(TFAP)N(py))ZrFI] (4) and [(N2(TFAP)N(py))ZrFCl] (5) in which the axially bound fluorido ligand is substituted. Reaction of [(N2(TFAP)N(py))ZrF2] (3) with LiNHNPh2 afforded the monohydrazido(1-) complex [(N2(TFAP)N(py))ZrF(NHNPh2)] (6) which was converted to the dimeric fluoro-potassium bridged hydrazinediido complex [Zr(N2(TFAP)N(py))FNNPh2K]2 (7) using KHMDS. The corresponding reaction with LiHMDS yielded the monomeric, donor free complex [Zr(N2(TFAP)N(py))NNPh2] (8).

DOI: 10.1021/ic401603y
PubMed: 23941662

Affiliations:

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<front><div type="abstract" xml:lang="en">The N-perfluoro-phenylated pyridyldiamine H2N2(PFP)N(py) (1) has been prepared by a palladium-catalyzed coupling of hexafluorobenzene and the diamine (H2NCH2)2C(CH3)(2-C5H4N) using the palladacycle trans-di(μ-acetato)bis[o-(di-o-tolylphosphino)benzyl]palladium(II) as catalyst. Reactions of H2N2(PFP)N(py) and Zr(NMe2)4 at room temperature or 90 °C led to the complexes [(N(PFP)N2(TFAP)N(py))ZrF(NMe2)] (2) and [(N2(TFAP)N(py))ZrF2] (3) in which one or two dimethylamido groups replaced one or two ortho fluorine atoms of the pentafluorophenyl groups in the ligand. Reaction of Me3SiX (X = Cl, I) with [(N2(TFAP)N(py))ZrF2] (3) resulted in the formation of mixed halogenated complexes [(N2(TFAP)N(py))ZrFI] (4) and [(N2(TFAP)N(py))ZrFCl] (5) in which the axially bound fluorido ligand is substituted. Reaction of [(N2(TFAP)N(py))ZrF2] (3) with LiNHNPh2 afforded the monohydrazido(1-) complex [(N2(TFAP)N(py))ZrF(NHNPh2)] (6) which was converted to the dimeric fluoro-potassium bridged hydrazinediido complex [Zr(N2(TFAP)N(py))FNNPh2K]2 (7) using KHMDS. The corresponding reaction with LiHMDS yielded the monomeric, donor free complex [Zr(N2(TFAP)N(py))NNPh2] (8).</div>
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Zirconium complexes supported by an N-perfluoro-arylated diamidopyridyl ligand: synthesis of hydrazinediido complexes.

Zirconium complexes supported by an N-perfluoro-arylated diamidopyridyl ligand: synthesis of hydrazinediido complexes.

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