At the Borderline between Metal-Metal Mixed Valency and a Radical Bridge Situation: Four Charge States of a Diruthenium Complex with a Redox-Active Bis( mer-tridentate) Ligand

The complex ions [L Ru(μ,η :η -BL)RuL ] (1 , L = 4,4',4″-tri- tert-butyl-2,6,2',6″-terpyridine and H BL = 1,2-bis(salicyloyl)hydrazide(2-)) were isolated with PF or ClO counterions ( n = 1) and as bis(hexafluorophosphate) ( n = 2). Structural, electrochemical, and spectroscopic characteriz...

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Veröffentlicht in:Inorganic chemistry Jg. 57; H. 7; S. 3983
Hauptverfasser: Mondal, Sudipta, Schwederski, Brigitte, Frey, Wolfgang, Fiedler, Jan, Záliš, Stanislav, Kaim, Wolfgang
Format: Journal Article
Sprache:Englisch
Veröffentlicht: United States 02.04.2018
ISSN:1520-510X, 1520-510X
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Abstract The complex ions [L Ru(μ,η :η -BL)RuL ] (1 , L = 4,4',4″-tri- tert-butyl-2,6,2',6″-terpyridine and H BL = 1,2-bis(salicyloyl)hydrazide(2-)) were isolated with PF or ClO counterions ( n = 1) and as bis(hexafluorophosphate) ( n = 2). Structural, electrochemical, and spectroscopic characterization reveals the monocation as intermediate ( K = 10 ) in the three-step reversible redox system 1 . The 1 ion has the molecule-bridged (Ru- - -Ru 4.727 Å) ruthenium centers involved in five- and six-membered chelate rings, and it exhibits long-wavelength absorptions at λ 2240, 1660, and 1530 nm (ε = 1000, 3000, and 8000 M cm , respectively), which would be compatible with a Ru Ru mixed-valent situation or with a coordinated radical ion bridge. In fact, EPR and DFT analysis of 1 reveals that the spin is equally distributed over the ligand bridge and over both metals. The oxidized paramagnetic ions 1 and 1 have been studied by H NMR and EPR and by TD-DFT supported UV-vis-NIR and MIR (mid-IR) spectroelectrochemistry. The capacity of various kinds of bis( mer-tridentate) bridging ligands (π donors or π acceptors, cyclometalated or noncyclometalated) for mediating metal-metal interactions is discussed.
AbstractList The complex ions [L Ru(μ,η :η -BL)RuL ] (1 , L = 4,4',4″-tri- tert-butyl-2,6,2',6″-terpyridine and H BL = 1,2-bis(salicyloyl)hydrazide(2-)) were isolated with PF or ClO counterions ( n = 1) and as bis(hexafluorophosphate) ( n = 2). Structural, electrochemical, and spectroscopic characterization reveals the monocation as intermediate ( K = 10 ) in the three-step reversible redox system 1 . The 1 ion has the molecule-bridged (Ru- - -Ru 4.727 Å) ruthenium centers involved in five- and six-membered chelate rings, and it exhibits long-wavelength absorptions at λ 2240, 1660, and 1530 nm (ε = 1000, 3000, and 8000 M cm , respectively), which would be compatible with a Ru Ru mixed-valent situation or with a coordinated radical ion bridge. In fact, EPR and DFT analysis of 1 reveals that the spin is equally distributed over the ligand bridge and over both metals. The oxidized paramagnetic ions 1 and 1 have been studied by H NMR and EPR and by TD-DFT supported UV-vis-NIR and MIR (mid-IR) spectroelectrochemistry. The capacity of various kinds of bis( mer-tridentate) bridging ligands (π donors or π acceptors, cyclometalated or noncyclometalated) for mediating metal-metal interactions is discussed.
The complex ions [L3Ru(μ,η3:η3-BL)RuL3] n+ (1 n+, L3 = 4,4',4″-tri- tert-butyl-2,6,2',6″-terpyridine and H2BL2- = 1,2-bis(salicyloyl)hydrazide(2-)) were isolated with PF6- or ClO4- counterions ( n = 1) and as bis(hexafluorophosphate) ( n = 2). Structural, electrochemical, and spectroscopic characterization reveals the monocation as intermediate ( Kc = 108.2) in the three-step reversible redox system 10/+/2+/3+. The 1+ ion has the molecule-bridged (Ru- - -Ru 4.727 Å) ruthenium centers involved in five- and six-membered chelate rings, and it exhibits long-wavelength absorptions at λmax 2240, 1660, and 1530 nm (εmax = 1000, 3000, and 8000 M-1 cm-1, respectively), which would be compatible with a RuIIIRuII mixed-valent situation or with a coordinated radical ion bridge. In fact, EPR and DFT analysis of 1+ reveals that the spin is equally distributed over the ligand bridge and over both metals. The oxidized paramagnetic ions 12+ and 13+ have been studied by 1H NMR and EPR and by TD-DFT supported UV-vis-NIR and MIR (mid-IR) spectroelectrochemistry. The capacity of various kinds of bis( mer-tridentate) bridging ligands (π donors or π acceptors, cyclometalated or noncyclometalated) for mediating metal-metal interactions is discussed.The complex ions [L3Ru(μ,η3:η3-BL)RuL3] n+ (1 n+, L3 = 4,4',4″-tri- tert-butyl-2,6,2',6″-terpyridine and H2BL2- = 1,2-bis(salicyloyl)hydrazide(2-)) were isolated with PF6- or ClO4- counterions ( n = 1) and as bis(hexafluorophosphate) ( n = 2). Structural, electrochemical, and spectroscopic characterization reveals the monocation as intermediate ( Kc = 108.2) in the three-step reversible redox system 10/+/2+/3+. The 1+ ion has the molecule-bridged (Ru- - -Ru 4.727 Å) ruthenium centers involved in five- and six-membered chelate rings, and it exhibits long-wavelength absorptions at λmax 2240, 1660, and 1530 nm (εmax = 1000, 3000, and 8000 M-1 cm-1, respectively), which would be compatible with a RuIIIRuII mixed-valent situation or with a coordinated radical ion bridge. In fact, EPR and DFT analysis of 1+ reveals that the spin is equally distributed over the ligand bridge and over both metals. The oxidized paramagnetic ions 12+ and 13+ have been studied by 1H NMR and EPR and by TD-DFT supported UV-vis-NIR and MIR (mid-IR) spectroelectrochemistry. The capacity of various kinds of bis( mer-tridentate) bridging ligands (π donors or π acceptors, cyclometalated or noncyclometalated) for mediating metal-metal interactions is discussed.
Author Záliš, Stanislav
Schwederski, Brigitte
Fiedler, Jan
Mondal, Sudipta
Frey, Wolfgang
Kaim, Wolfgang
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  givenname: Brigitte
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  surname: Kaim
  fullname: Kaim, Wolfgang
  organization: Institut für Anorganische Chemie , Universität Stuttgart , Pfaffenwaldring 55 , D-70550 Stuttgart , Germany
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Snippet The complex ions [L Ru(μ,η :η -BL)RuL ] (1 , L = 4,4',4″-tri- tert-butyl-2,6,2',6″-terpyridine and H BL = 1,2-bis(salicyloyl)hydrazide(2-)) were isolated with...
The complex ions [L3Ru(μ,η3:η3-BL)RuL3] n+ (1 n+, L3 = 4,4',4″-tri- tert-butyl-2,6,2',6″-terpyridine and H2BL2- = 1,2-bis(salicyloyl)hydrazide(2-)) were...
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Title At the Borderline between Metal-Metal Mixed Valency and a Radical Bridge Situation: Four Charge States of a Diruthenium Complex with a Redox-Active Bis( mer-tridentate) Ligand
URI https://www.ncbi.nlm.nih.gov/pubmed/29528630
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