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

Deuterated dinuclear ruthenium(II,III) 3,4,5-tri(ethoxy-d(5)) benzoate, [Ru-2{3,4,5-(C2D5O)(3)C6H2COO}(4)Cl](n), was synthesized by a reaction of [Ru-2(C2H5COO)(4)Cl](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 H-1 NMR spectra, and compared with those of the undeuterated complex [Ru-2{3,4,5-(C2H5O)(3)C6H2COO}(4)Cl](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 Ru-1-Cl-Ru-2 angle of 123.82(4)degrees. H-1 NMR spectra in CD2Cl2 displayed a broad signal attributable to o-H atoms on the phenyl rings of the benzoate ligands from approximately delta = 23 to delta = 32 at 25 degrees C and several signals from approximately delta = -50 to delta = 50 at -80 degrees 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. (C) 2010 Institute of Chemistry, Slovak Academy of Sciences