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Anilino radical complexes of cobalt(III) and manganese(IV) and comparison with their phenoxyl analogues
Zitatschlüssel ISI:000090078900013
Autor Penkert, F N and Weyhermuller, T and Bill, E and Hildebrandt, P and Lecomte, S and Wieghardt, K
Seiten 9663-9673
Jahr 2000
ISSN 0002-7863
Adresse 1155 16TH ST, NW, WASHINGTON, DC 20036 USA
Journal J. Am. Chem. Soc
Jahrgang 122
Nummer 40
Monat OCT 11
Verlag AMER CHEMICAL SOC
Zusammenfassung The pendent arm macrocyclic aniline ligands 1-(2-amino-3,5-di-tert-butylbenzyl)-4,7-dimethyl-1,4,7-triazacyclononane , H[L-1], and 1,4,7-tris(2-amino-3,5-di-tert-butylbenzyl)-1,4,7-triazacyclononane, H-3[L-2], have been synthesized. The reaction of these ligands in methanol (1:1) and/or ethanol with Co-II(ClO4)(2). 6H(2)O and potassium di-tert-butylacetylacetonate (1:1) or Mn-II(acetate)(2). 4H(2)O in the presence of air produced the anilide complexes [Co-III(L-1)(Bu(2)acac)](ClO4) (1) and [Mn-IV(L-2)]X (X = ClO4 (2), BPh4 (2')), respectively. The reaction of H-3[L-2] and CuCl2. 2H(2)O in ethanol produced upon addition of NaClO4 blue crystals of [Cu-II(H3L2)Cl](ClO4) (3) containing two coordinated and one uncoordinated aniline pendent arm. Complexes 1, 2, and 3 have been structurally characterized by X-ray crystallography. Electrochemically, 1 is reversibly oxidized with formation of the paramagnetic anilino radical species [Co-III(L-1 .)(Bu(2)acac)(2+) (S = 1/2) whereas the cyclic voltammogram of 2 displays three ligand-centered one-electron-transfer oxidation waves where complexes [Mn-IV(L-2 .)](2+), [Mn-IV(L-2 . .)](3+), and {[Mn-IV(L-2 . . .)](4+) containing one, two, and three coordinated anilino radicals are formed successively. These anilino radical species have been characterized by UV-vis, X-band EPR, and resonance Raman spectroscopy. The characteristic spectroscopic features of coordinated anilino radicals have been elucidated. In the Mn-IV radical species strong intramolecular exchange coupling between the metal ion (t(2)g(3) configuration
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