Synthesis and characterization of ruthenium and osmium complexes of heterocyclic bidentate ligands (N,X), X=S, Se
作者:Antonio Sousa-Pedrares、Maria Luz Durán、Jaime Romero、José Arturo García-Vázquez、Juan C. Monteagudo、Antonio Sousa、Jonathan R. Dilworth
DOI:10.1016/j.ica.2005.06.009
日期:2006.2
The reaction of [RuCl2(PPh3)(3)] and [OsBr2(PPh3)(3)] precursors with a series of heterocyclic bidentate (N, X) ligands, X = S, Se, gave complexes [M(R-pyS)(2)(PPh3)(2)], (R = H, 3-CF3, 5-CF3, 3-Me3Si);[M(R-pymS)(2)(PPh3)(2)], (R = 4-CF3, 4,6-MeCF3) and [M(R-pySe)(2)(PPh3)(2)], (R = H, 3-CF3, 5-CF3) where M is Ru or Os, pyS and pymS the anions of pyridine-2-thione and pyrimidine-2-thione,respectively, and pySe is the anion produced by the reductive cleavage of the Se-Se bond in the dipyridyl-2,2'-diselenide. All of the compounds obtained were characterized by microanalysis, IR, FAB, NMR spectroscopy and by cyclic voltammetry. Compounds [Ru(3-CF3-pyS)(2)(PPh3)(2)]center dot 2(CH2Cl2) (2), [Ru(3-Me3Si-pyS)(2)(PPh3)(2)] (4), [Ru(4-CF3-pymS)(2)(PPh3)(2)] (5), [Ru(3-CF3-pySe)(2)(PPh3)(2)]center dot 2(CH2Cl2) (8), [Os(3-CF3-pyS)(2)(PPh3)(2)]center dot(CHCl3) (11), [Os(3-Me3Si-PYS)(2)(PPh3)(2)](13), [Os(3-CF3-pySe)(2)(PPh3)(2)]center dot 2(CH2Cl2) (17), [Os(5-CF3-pySe)(2)(PPh3)(2)]center dot(2)(H2O) (18) and [OSCl2(4,6-MeCF3-pymS)(PPh3)(2)](19) were also characterized by X-ray diffraction. In all cases, the metal is in a distorted octahedral environment with the heterocyclic ligand acting as a bidentate (N, S) chelate system. (c) 2005 Elsevier B.V. All rights reserved.