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Synthesis of water-soluble and ether-soluble tetra-μ-acetatodiruthenium(II,III) complexes and X-ray crystal structure of [Ru2(μ-O2CC6H5)4(C2H5OH)2][Ru2(μ-O2CC6H5)4(HSO4)2]

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DOI: 10.1016/s0277-5387(00)88207-8


Abstract [Ru 2(μ-O 2CCH 3) 4Cl] reacts readily with aqueous Ag 2SO 4 (2: 1 molar ratio) to give the sulphate salt [Ru 2(μ-O 2CCH 3) 4(H 2O) 2] 2(SO 4) ( 1). Addition of NaBPh 4 to an aqueous solution of 1 produces the ether-soluble tetraphenylborate salt [Ru 2(μ-O 2CCH 3) 4(H 2O) 2][BPh 4] ( 2). A methanolic solution of 1 reacts with Ba(C 6H 5CCCO 2) 2 · H 2O to give the tetraacetatemonophenylpropynoate complex [Ru 2(μ-O 2CCH 3) 4(O 2CCCC 6H 5)] · H 2O ( 3). The reaction of an ethanolic suspension of [Ru 2(μ-O 2CC 6H 5) 4Cl] with Ag 2SO 4 and H 2SO 4 (2 : 1 : 1 molar ratio) leads to the tetra-μ-benzoatodiruthenium(II,III) double complex salt [Ru 2(μ-O 2CC 6H 5) 4(C 2H 5OH) 2][Ru 2(μ-O 2CC 6H 5) 4(HSO 4) 2] ( 4). Complex 4 is also obtained by reacting an ethanolic solution of 1 with an excess of benzoic acid in the presence of H 2SO 4. The X-ray crystal structure of 4 shows it to consist of [Ru 2(μ-O 2CC 6H 5) 4(C 2H 5OH) 2] + and [Ru 2(μ-O 2CC 6H 5) 4(HSO 4) 2] − ions, which are linked together by hydrogen bonds into an infinite polymeric chain. The RuRu distances in the cation and anion are very similar [2.265(2) and 2.272(2) Å, respectively]. Spectroscopic, magnetic, conductivity and cyclic voltammetry data are given for the complexes.

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