ISSN print edition: 0366-6352 ISSN electronic edition: 1336-9075 Registr. No.: MK SR 9/7 Published monthly

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)