Synthesis and reactivity of non-polymeric tetracarboxylatochloro-diruthenium(II,III) complexes. Crystal structure of [Ru2Cl(μ-O2CCHMe2)4 (OPPh3)]

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Abstract
New non-polymeric diruthenium(II,III) carboxylates of the type [Ru 2 Cl(µ-O 2 CR) 4 ] (R = CHEt 2 1, CHMeEt 2 or CHMePh 3) were obtained by reaction of HO 2 CR with [Ru 2 Cl(µ-O 2 CMe) 4 ] in methanol–water. The mixed-ligand complex [Ru 2 Cl(µ-O 2 CMe) 2 (µ-O 2 CCMe 3 ) 2 ] 4 has also been prepared. The reactivity of these complexes and of the previously described [Ru 2 Cl(µ-O 2 CR) 4 ] (R = CMe 3 5 or CHMe 2 6) has been studied and compared with those found for polymeric [Ru 2 Cl(µ-O 2 CR) 4 ] (R = alkyl or aryl). The interaction of AgSCN with [Ru 2 Cl(µ-O 2 CR) 4 ] or [Ru 2 Cl(µ-O 2 CMe) 2 (µ-O 2 CCMe 3 ) 2 ] leads to [Ru 2 (µ-O 2 CR) 4 (SCN)] (R = CHEt 2 7, CHMePh 8 or CMe 3 9) and [Ru 2 (µ-O 2 CMe) 2 (µ-O 2 CCMe 3 ) 2 (SCN)] 10 respectively. The first derivatives of the type [Ru 2 X(µ-O 2 CR) 4 (OPPh 3 )] (X = Cl; R = CHEt 2 11, CHMeEt 12, CHMePh 13, CMe 3 14 or CHMe 2 15; X = SCN; R = CHEt 2 17, CHMePh 18 or CMe 3 19) and [Ru 2 Cl(µ-O 2 CMe) 2 (µ-O 2 CCMe 3 ) 2 (OPPh 3 )] 16 containing two different axial ligands have been obtained. Cationic compounds of the type [Ru 2 (µ-O 2 CR) 4 (thf) 2 ]BF 4 (R = CMe 3 20 or CHMe 2 21; thf = tetrahydrofuran), [Ru 2 (µ-O 2 CCHMe 2 ) 4 (OPPh 3 ) 2 ]BF 4 22 or [Ru 2 (µ-O 2 CCHMe 2 ) 4 (OPPh 3 )(thf)]BF 4 23 were also prepared. The crystal structure of 15 has been determined by X-ray crystallography. It has two ruthenium atoms linked by four bridging isobutyrate ligands with the axial positions being occupied by one chlorine atom and one OPPh 3 molecule.

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