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