Issue 19, 2013

Preparation of tetrabutylammonium salt of a mono-Ru(iii)-substituted α-Keggin-type silicotungstate with a 4,4′-bipyridineligand and its electrochemical behaviour in organic solvents

Abstract

The tetrabutylammonium (TBA) salt of a mono-ruthenium(III)-substituted α-Keggin-type silicotungstate with a 4,4′-bipyridine (bipy) ligand, TBA5[α-SiW11O39RuIII(bipy)] (1), which is soluble in various organic solvents, was prepared by a cation exchange reaction of Cs5[α-SiW11O39RuIII(bipy)] with tetrabutylammonium bromide. Compound 1 was characterised using IR, 1H-NMR, elemental analysis, single crystal X-ray analysis, X-ray absorption near-edge structure (XANES) analysis (Ru L3-edge), electron spin resonance (ESR), cyclic voltammetry (CV) and UV-Vis. Single crystal X-ray analysis of 1 revealed that the RuIII unit was incorporated into the α-Keggin-type silicotungstate framework and coordinated by a bipy molecule through a Ru–N bond. CV indicated that the incorporated RuIII-bipy was reversibly oxidised to the RuIV-bipy derivative and reduced to the RuII-bipy derivative in organic solvents. The redox potential of RuIV/III-bipy was found to be affected by organic solvents. Moreover, the RuV-bipy derivative was observed in acetonitrile.

Graphical abstract: Preparation of tetrabutylammonium salt of a mono-Ru(iii)-substituted α-Keggin-type silicotungstate with a 4,4′-bipyridine ligand and its electrochemical behaviour in organic solvents

Supplementary files

Article information

Article type
Paper
Submitted
30 Jan 2013
Accepted
07 Mar 2013
First published
08 Mar 2013

Dalton Trans., 2013,42, 7190-7195

Preparation of tetrabutylammonium salt of a mono-Ru(III)-substituted α-Keggin-type silicotungstate with a 4,4′-bipyridine ligand and its electrochemical behaviour in organic solvents

S. Ogo, S. Moroi, T. Ueda, K. Komaguchi, S. Hayakawa, Y. Ide, T. Sano and M. Sadakane, Dalton Trans., 2013, 42, 7190 DOI: 10.1039/C3DT50300C

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