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The synthesis and characterization of rhenium nitrosyl complexes. The X-ray crystal structures of [ReBr2(NO)(NCMe)3], [Re(NO)(N5)](BPh4)2] and [ReBr2(NO)(NCMe){py-CH2-NH∼CH2CH2-N(CH2-py)2}]


Mahmood, A; Akgun, Z; Peng, Y; Müller, P; Jiang, Y; Berke, H; Jones, A G; Nicholson, T (2013). The synthesis and characterization of rhenium nitrosyl complexes. The X-ray crystal structures of [ReBr2(NO)(NCMe)3], [Re(NO)(N5)](BPh4)2] and [ReBr2(NO)(NCMe){py-CH2-NH∼CH2CH2-N(CH2-py)2}]. Inorganica Chimica Acta, 405:455-460.

Abstract

Reactions of low oxidation state rhenium–nitrosyl complexes with polyamine ligands have been examined. Rhenium(II)–nitrosyl complexes gave an array of unstable products that were difficult to isolate cleanly. The rhenium(I)–nitrosyl complex [ReBr2(NO)(NCMe)3] gave multiple products which were more easily isolated.
The major product from the reaction of [ReBr2(NO)(NCMe)3] with the potentially pentadentate ligand N1,N1,N2-tris(2-pyridinylmethyl)-1,2 ethanediamine was the dicationic species [Re(NO)(N5)]2+, which was isolated as the bis-tetraphenylborate salt. The other major product [ReBr2(NO)(NCMe){py-CH2NH∼CH2CH2N(CH2-py)2}], was separated from a number of other neutral species via chromatography. This species contains the same potentially pentadentate ligand, only here it is coordinated through only two of its amine functional groups. Left dangling is the secondary amine and both of its pyridyl groups.
Both amine complexes are diamagnetic and both display their respective parent ions in the ESI(+) mass spectra. The dication [Re(NO)(N5)]2+ shows its half mass parent peak at 275 m/z while [ReBr2(NO)(NCMe){py-CH2NH∼CH2CH2N(CH2-py)2}] shows its parent peak at 751 m/z. The infrared spectrum of [ReBr2(NO)(NCMe){py-CH2NH∼CH2CH2N(CH2-py)2}] displays its ν(Ndouble bond; length as m-dashO) at 1676 cm−1. And the infrared spectrum of [Re(NO)(N5)](BPh4)2 displays its ν(Ndouble bond; length as m-dashO) at 1714 cm−1.

Abstract

Reactions of low oxidation state rhenium–nitrosyl complexes with polyamine ligands have been examined. Rhenium(II)–nitrosyl complexes gave an array of unstable products that were difficult to isolate cleanly. The rhenium(I)–nitrosyl complex [ReBr2(NO)(NCMe)3] gave multiple products which were more easily isolated.
The major product from the reaction of [ReBr2(NO)(NCMe)3] with the potentially pentadentate ligand N1,N1,N2-tris(2-pyridinylmethyl)-1,2 ethanediamine was the dicationic species [Re(NO)(N5)]2+, which was isolated as the bis-tetraphenylborate salt. The other major product [ReBr2(NO)(NCMe){py-CH2NH∼CH2CH2N(CH2-py)2}], was separated from a number of other neutral species via chromatography. This species contains the same potentially pentadentate ligand, only here it is coordinated through only two of its amine functional groups. Left dangling is the secondary amine and both of its pyridyl groups.
Both amine complexes are diamagnetic and both display their respective parent ions in the ESI(+) mass spectra. The dication [Re(NO)(N5)]2+ shows its half mass parent peak at 275 m/z while [ReBr2(NO)(NCMe){py-CH2NH∼CH2CH2N(CH2-py)2}] shows its parent peak at 751 m/z. The infrared spectrum of [ReBr2(NO)(NCMe){py-CH2NH∼CH2CH2N(CH2-py)2}] displays its ν(Ndouble bond; length as m-dashO) at 1676 cm−1. And the infrared spectrum of [Re(NO)(N5)](BPh4)2 displays its ν(Ndouble bond; length as m-dashO) at 1714 cm−1.

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Item Type:Journal Article, refereed, original work
Communities & Collections:07 Faculty of Science > Department of Chemistry
Dewey Decimal Classification:540 Chemistry
Language:English
Date:2013
Deposited On:07 Feb 2014 15:30
Last Modified:07 Dec 2017 08:43
Publisher:Elsevier
ISSN:0020-1693
Publisher DOI:https://doi.org/10.1016/j.ica.2013.01.017

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