Coordination of polythiaether macrocycles to metal cluster complexes. 1. Synthesis and structural characterization of Ru[sub 5](CO)[sub 13]([mu]-[eta][sup 1]-12S3)([mu][sub 5]-C) and Ru[sub 5](CO)[sub 11]([mu]-[eta][sup 3]-12S3)([mu][sub 5]-C), 12S3 = 1,5,9-trithiacyclododecane
- Univ. of South Carolina, Columbia, SC (United States)
The reaction of Ru[sub 5](CO)[sub 15]([mu][sub 5]-C), 1, with 1,5,9-trithiacyclododecane (12S3) in hexane solvent at reflux has yielded the new cluster complex Ru[sub 5](CO)[sub 13]([mu]-[eta][sup 1]-12S3)([mu][sub 5]-C), 2, in 86% yield. When 1 and 12S3 were heated to reflux in octane solvent the new complex Ru[sub 5](CO)[sub 11]([mu]-[eta][sup 3]12S3)([mu][sub 5]-C), 3, was formed in 75% yield. Compound 2 and be converted to 3 in 80% yield at 125[degrees]C. Compounds 2 and 3 were both characterized by single crystal X-ray diffraction analyses. Both compounds contain a square pyramidal cluster of five ruthenium atoms with a [mu][sub 5]-carbido ligand. In 2 the 12S3 ligand bridges one edge of the square base of the Ru[sub 5]([mu][sub 5]-C) cluster by using only one of its sulfur atoms. The other two sulfur atoms are uncoordinated. In the transformation of 2 to 3, two CO ligands were eliminated and the two uncoordinated sulfur atoms became coordinated to one of the sulfur-bridged ruthenium atoms. Crystal data for 2: space group = P2[sub 1]/n, a = 14.335(3) angstroms, b = 15.188(3) angstroms, c = 15.439(3) angstroms, [beta] = 91.83(2)[degrees], Z = 4, 2249 reflections, R = 0.034. For 3[center dot]CH[sub 2]Cl[sub 2]: space group = P2[sub 1]2[sub 1]2[sub 1], a = 14.213(4) angstroms, b = 17.431(4) angstroms, c = 13.713(4) angstroms, Z = 4, 2797 reflections, R = 0.036. 9 refs., 2 figs., 7 tabs.
- OSTI ID:
- 6730804
- Journal Information:
- Organometallics; (United States), Journal Name: Organometallics; (United States) Vol. 13:12; ISSN 0276-7333; ISSN ORGND7
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
400102 -- Chemical & Spectral Procedures
400201* -- Chemical & Physicochemical Properties
CHEMICAL REACTIONS
COHERENT SCATTERING
COMPILED DATA
COMPLEXES
CRYSTALLOGRAPHY
DATA
DIFFRACTION
HETEROCYCLIC COMPOUNDS
INFORMATION
LIGANDS
MAGNETIC RESONANCE
MOLECULAR STRUCTURE
NUCLEAR MAGNETIC RESONANCE
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC SULFUR COMPOUNDS
ORGANOMETALLIC COMPOUNDS
RESONANCE
RUTHENIUM COMPLEXES
SCATTERING
SPECTROSCOPY
SYNTHESIS
TRANSITION ELEMENT COMPLEXES
X-RAY DIFFRACTION