Synthesis and structural characterization of diene and benzene pentaruthenium clusters
1993 | journal article. A publication with affiliation to the University of Göttingen.
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Braga, Dario, Fabrizia Grepioni, Piera Sabatino, Paul J. Dyson, Brian F. G. Johnson, Jack Lewis, Philip J. Bailey, Paul R. Raithby, and Dietmar Stalke. "Synthesis and structural characterization of diene and benzene pentaruthenium clusters." Dalton Transactions no. 6 (1993): 985-992. https://doi.org/10.1039/DT9930000985.
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Details
- Authors
- Braga, Dario; Grepioni, Fabrizia; Sabatino, Piera; Dyson, Paul J.; Johnson, Brian F. G.; Lewis, Jack; Bailey, Philip J.; Raithby, Paul R.; Stalke, Dietmar
- Abstract
- Reaction of the square-pyramidal cluster [Ru5C(CO)15]1 with cyclohexa-1,3-diene and Me3NO in CH2Cl2 at ambient temperature affords the novel species [Ru5C(CO)13(µ-2:2-C6H8)]2 which has been fully characterized by X-ray diffraction studies [monoclinic, space group P21/n, a= 16.193(3), b= 9.897(2), c= 19.536(4)Å, = 98.80(3)° and Z= 4]. Further reaction of compound 2 with Me3NO in the same solvent results in the dehydrogenation of the C6H8 ligand and the production of two isomers 3a and 3b of the benzene derivative [Ru5C(CO)12(C6H6)]. In agreement with mass spectroscopic and 1H NMR data, the X-ray diffraction analysis shows that the benzene ligand is bound in a face-capping mode in [Ru5C(CO)12(µ3-2:2:2-C6H6)]3a and in a terminal mode in [Ru5C(CO)12(6-C6H6)]3b, respectively. Compound 3a is triclinic, space group P1–, a= 9.525(2), b= 14.574(3), c= 9.484(4)Å, = 96.29(2), = 112.37(3), = 82.33(2)° and Z= 2; 3b is monoclinic, space group P21/c, a= 15.26 (2), b= 16.675(9), c= 19.016(9)Å, = 96.04(7)° and Z= 8. On heating 3a in hexane a quantitative and irreversible conversion to 3b is observed. Treatment of 3b with carbon monoxide produces the adduct [Ru5C(CO)13(6-C6H6)]4a, which, on the basis of a single crystal X-ray diffraction study, has been shown to contain a bridged-butterfly arrangement of five ruthenium atoms. Compound 4a is monoclinic, space group P21/n, a= 9.792(4), b= 15.718(2), c= 16.446(3)Å, = 96.37(2)° and Z= 4. On standing in CH2Cl2, 4a undergoes loss of carbon monoxide to give the apical isomer [Ru5C(CO)12(C6H6)]3c. On heating in hexane over a prolonged period 3c undergoes quantitative isomerization to 3b.
- Issue Date
- 1993
- Journal
- Dalton Transactions
- Organization
- Fakultät für Chemie
- File Format
- application/pdf
- Language
- English