Pentamethylcyclopentadienyl-arene-ruthenium Hexafluorophosphates. Synthesis, N M R Spectra, Reduction Potentials, Crystal Structure M ononuclear and binuclear com pounds [(C5M e5)Ru(//6-arene)PF6 and [(C5M e5R u)2(//6,/76-arene)](PF6)-, were prepared by reacting (C5M e5)RuCl2, the arene and silver acetate with subsequent addition o f N H 4PF6, for arene = phenanthrene, chrysene, triphenylene, fluorene, bifluorene. biphenyl and 4,4'-biphenyl. The mononuclear com pounds were also prepared for arene = naphthalene, anthracene, pyrene and coronene. The 'H and l3C N M R spectra are reported. By cyclic voltammetry all compounds show a first reduction potential that is considerably more positive compared with the free arene. The first cathodic wave is irreversible for a wide range o f scanning speeds. However, the mononuclear coronene and the binuclear phenanthrene com pounds show reversibility. The crystal structure o f [(CsM es)Ru(/76-chrysene)]PF6-0.5 Me^CO was determined by X-ray diffraction (3797 unique observed reflexions, R = 0.098). Crystal data: a = 1689.2(2), b = 1524.0(8), c = 2263.5(3) pm, ß = 107.22(1) , space group P 2,/«, Z = 8. Crystallographically independent, two cations [(C5M e5)Ru(>76-chrysene)]+ and two anions PF6~ are present, but their structures are essentially equal. The [C5M esRu]+ unit is bonded to one o f the terminal benzene rings o f the chrysene in a sandwich manner; the rings bonded to Ru are nearly coplanar. The PF6~ ions and the C5M e5 rings exhibit strong thermal vibrations. Unauthenticated Download Date | 4/22/17 2:05 PM
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