Abstract
The reaction of K2[RuCl5(H2O)] with NNN′N′-tetramethyl-3,6-dimethyl-3,6-diazaoctane-1,8-diamine (L1) in ethanol yielded cis-[RuIII(L1)Cl2]+, which was isolated as the ClO4– salt. The optical spectrum of cis-[RuIII(L1)Cl2]ClO4 in acetonitrile displays one intense band at 375 nm attributed to a pπ(Cl)→dπ*(Ru) transition. cis.-[RuIII(L1)Cl2]ClO4 has been characterized by X-ray crystallography: space group P21/c, a= 11.716(5), b= 13.089(4), c= 12.981(5)Å, β= 94.28(2)°, Z= 4, and R= 0.076 for 1 913 observed Mo-Kα data. The co-ordination geometry around the metal ion is distorted octahedral with cis arrangement of the two chloride ligands. The average Ru–N and Ru–Cl bond distances are 2.17(1) and 2.345(4)Å, respectively. Treatment of cis-[RuIII(L1)Cl2]ClO4 with silver(I)p-toluenesulphonate in hot water and then H2O2 gave [RuVI(L1)(O)2]2+ isolated as the ClO4– salt. [RuVI(L1)(O)2][ClO4]2 is diamagnetic (µeff.= 0) and has an intense i.r. band at ca. 850 cm–1 attributed to νasym(RuO) stretching. The E½ value of the [RuVI(L1)(O)2]2+/[RuIV(L1)(O)(H2O)]2+ couple in 0.1 mol dm–3 CF3CO2H is 0.79. V vs. a saturated calomel electrode. The reaction of [RuIV(L1)(O)2][ClO4]2 with styrene produced benzaldehyde.
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