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Synthesis, crystal structure, and 1H NMR spectra of a chloride-bridged chain complex of dinuclear ruthenium(II,III) 3,4,5-tri(ethoxy-d5)benzoate

Hideaki Ishida, Makoto Handa, Takahisa Ikeue, Jun Taguchi, and Masahiro Mikuriya

Department of Chemistry and Research Center for Coordination Molecule-based Devices, School of Science and Technology, Kwansei Gakuin University, 2-1 Gakuen, Sanda, 669-1337 Japan

 

E-mail: junpei@kwansei.ac.jp

Abstract: Deuterated dinuclear ruthenium(II,III) 3,4,5-tri(ethoxy-d 5)benzoate, [Ru2{3,4,5-(C2D5O)3C6H2-COO}4Cl] n , was synthesized by a reaction of [Ru2(C2H5COO)4Cl] n and 3,4,5-tri(ethoxy-d 5)benzoic acid and characterized by single-crystal X-ray analysis as well as IR, UV-VIS, and 1H NMR spectra, and compared with those of the undeuterated complex [Ru2{3,4,5-(C2H5O)3C6H2COO}4Cl] n . Single-crystal X-ray analysis showed that chloride ligands bridge the dinuclear ruthenium(II,III) units at the axial positions to form a zigzag chain molecule with the Ru1-Cl-Ru2 angle of 123.82(4)°. 1H NMR spectra in CD2Cl2 displayed a broad signal attributable to o-H atoms on the phenyl rings of the benzoate ligands from approximately δ = 23 to δ = 32 at 25°C and several signals from approximately δ = −50 to δ = 50 at −80°C. These spectra show the preservation of the polymeric or oligomeric chain structure in dichloromethane, which is supported by the solution behavior confirmed by the UV-VIS spectra and electronic conductance.

Keywords: dinuclear ruthenium(II,III) carboxylate - benzoate complex - chlorido bridging - crystal structure - 1H NMR spectra - UV-VIS spectra

Full paper is available at www.springerlink.com.

DOI: 10.2478/s11696-010-0071-1

 

Chemical Papers 64 (6) 767–775 (2010)

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