Geometric and Electronic Structures of Nickel(II) Complexes of Redox Noninnocent Tetradentate Phenylenediamine Ligands

Five tetradentate ligands based on the N,N'-bis(2-amino-3,5-di-tert-butylphenyl)-o-phenylenediamine backbone were prepared, with different substituents at positions 4 and 5 (CH3 (3a), p-CH3O-C6H4 (3b), H (3c), Cl (3d), F (3e)). Their reaction with a nickel(II) salt in air affords the neutral sp...

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Veröffentlicht in:Inorganic chemistry Jg. 55; H. 2; S. 649 - 665
Hauptverfasser: Ciccione, Jérémie, Leconte, Nicolas, Luneau, Dominique, Philouze, Christian, Thomas, Fabrice
Format: Journal Article
Sprache:Englisch
Veröffentlicht: United States 19.01.2016
ISSN:1520-510X
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Abstract Five tetradentate ligands based on the N,N'-bis(2-amino-3,5-di-tert-butylphenyl)-o-phenylenediamine backbone were prepared, with different substituents at positions 4 and 5 (CH3 (3a), p-CH3O-C6H4 (3b), H (3c), Cl (3d), F (3e)). Their reaction with a nickel(II) salt in air affords the neutral species 4(a-e), which were isolated as single crystals. 4(a-e) feature two antiferromagnetically exchange-coupled diiminosemiquinonate moieties, both located on peripheral rings, and a diamidobenzene bridging unit. Oxidation of 4(a-e) with 1 equiv of AgSbF6 yields the cations 4(a-e)(+), which harbor a single diiminosemiquinonate radical. Significant structural differences were observed within the series. 4b(+) is mononuclear and contains a localized diiminosemiquinonate moiety. In contrast, 4c(+) is a dimer wherein the diiminosemiquinonate radical is rather delocalized over both peripheral rings. 4d(+) represents an intermediate case where the complex is mononuclear, but the radical is fully delocalized. Oxidation of 4(a-e) with 2 equiv of AgSbF6 produces the corresponding mononuclear dications. X-ray diffraction data on 4(b-d)(2+) reveals that the bridging ring retains its diamidobenzene character, whereas both peripheral rings have been oxidized into diiminobenzoquinone moieties. All the complexes were characterized by electrochemistry, EPR, and UV-vis-NIR spectroscopy. Remarkably, the electronic structures of the complexes differ from those reported by Wieghardt et al. for copper and zinc complexes of a related ligand involving a mixed N2O2 donor set (J. Am. Chem. Soc. 1999, 121, 9599). The easier oxidation of phenylenediamine moieties in comparison to aminophenols is proposed to account for the difference.
AbstractList Five tetradentate ligands based on the N,N'-bis(2-amino-3,5-di-tert-butylphenyl)-o-phenylenediamine backbone were prepared, with different substituents at positions 4 and 5 (CH3 (3a), p-CH3O-C6H4 (3b), H (3c), Cl (3d), F (3e)). Their reaction with a nickel(II) salt in air affords the neutral species 4(a-e), which were isolated as single crystals. 4(a-e) feature two antiferromagnetically exchange-coupled diiminosemiquinonate moieties, both located on peripheral rings, and a diamidobenzene bridging unit. Oxidation of 4(a-e) with 1 equiv of AgSbF6 yields the cations 4(a-e)(+), which harbor a single diiminosemiquinonate radical. Significant structural differences were observed within the series. 4b(+) is mononuclear and contains a localized diiminosemiquinonate moiety. In contrast, 4c(+) is a dimer wherein the diiminosemiquinonate radical is rather delocalized over both peripheral rings. 4d(+) represents an intermediate case where the complex is mononuclear, but the radical is fully delocalized. Oxidation of 4(a-e) with 2 equiv of AgSbF6 produces the corresponding mononuclear dications. X-ray diffraction data on 4(b-d)(2+) reveals that the bridging ring retains its diamidobenzene character, whereas both peripheral rings have been oxidized into diiminobenzoquinone moieties. All the complexes were characterized by electrochemistry, EPR, and UV-vis-NIR spectroscopy. Remarkably, the electronic structures of the complexes differ from those reported by Wieghardt et al. for copper and zinc complexes of a related ligand involving a mixed N2O2 donor set (J. Am. Chem. Soc. 1999, 121, 9599). The easier oxidation of phenylenediamine moieties in comparison to aminophenols is proposed to account for the difference.
Author Luneau, Dominique
Philouze, Christian
Thomas, Fabrice
Ciccione, Jérémie
Leconte, Nicolas
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  givenname: Jérémie
  surname: Ciccione
  fullname: Ciccione, Jérémie
  organization: Chimie Inorganique Redox, Département de Chimie Moléculaire (UMR CNRS 5250), Université Grenoble Alpes, UMR-5250 , 38041 Grenoble Cedex 9, France
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  givenname: Nicolas
  surname: Leconte
  fullname: Leconte, Nicolas
  organization: Chimie Inorganique Redox, Département de Chimie Moléculaire (UMR CNRS 5250), Université Grenoble Alpes, UMR-5250 , 38041 Grenoble Cedex 9, France
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  givenname: Dominique
  surname: Luneau
  fullname: Luneau, Dominique
  organization: Laboratoire des Multimatériaux et Interfaces (UMR CNRS 5615), Université Claude Bernard Lyon 1 , 69622 Villeurbanne cedex, France
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  givenname: Christian
  surname: Philouze
  fullname: Philouze, Christian
  organization: Chimie Inorganique Redox, Département de Chimie Moléculaire (UMR CNRS 5250), Université Grenoble Alpes, UMR-5250 , 38041 Grenoble Cedex 9, France
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  givenname: Fabrice
  surname: Thomas
  fullname: Thomas, Fabrice
  organization: Chimie Inorganique Redox, Département de Chimie Moléculaire (UMR CNRS 5250), Université Grenoble Alpes, UMR-5250 , 38041 Grenoble Cedex 9, France
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Snippet Five tetradentate ligands based on the N,N'-bis(2-amino-3,5-di-tert-butylphenyl)-o-phenylenediamine backbone were prepared, with different substituents at...
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Title Geometric and Electronic Structures of Nickel(II) Complexes of Redox Noninnocent Tetradentate Phenylenediamine Ligands
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