Synthesis and characterization of [Ru(¦Ç6-C10H14)(dppf)X][PF6] (X = Cl, Br, I, SnF3) compounds: The X-ray structure of [Ru(¦Ç6-C10H14)(dppf)Cl][SnCl3
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The arene-ruthenium complex [Ru(¦Ç6-C10H14)(dppf)Cl]PF6 (1) was used as a precursor for the syntheses of the [Ru(¦Ç6-C10H14)(dppf)Br]PF6 (2), [Ru(¦Ç6-C10H14)(dppf)I]PF6 (3), [Ru(¦Ç6-C10H14)(dppf)SnF3]PF6 (4) and [Ru(¦Ç6-C10H14)(dppf)Cl][SnCl3]¡¤0.45CH2Cl2 (5) complexes by its reactions with KBr, KI, SnF2 and SnCl2, respectively. All of the compounds were characterized by NMR, IR, 57Fe and 119Sn-M?ssbauer spectroscopy, and cyclic voltammetry. The single-crystal X-ray structure analysis of the [Ru(¦Ç6-C10H14)(dppf)Cl][SnCl3]¡¤0.45CH2Cl2 complex revealed the expected piano-stool geometry. Cyclic voltammograms of the complexes showed only one quasi-reversible electrochemical process, involving the oxidation of Fe(II) and Ru(II) at the same potential, which was confirmed by exhaustive electrolysis experiments. 57Fe-M?ssbauer parameters obtained for the complexes (1-5) were fitted with one doublet corresponding to a site of one iron(II). The 119Sn-M?ssbauer parameters of the complex (4) indicate that tin is tetra covalent.
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