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), Vol. 13:12; ISSN 0276-7333
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
RUTHENIUM COMPLEXES
CHEMICAL REACTIONS
CRYSTALLOGRAPHY
MOLECULAR STRUCTURE
NUCLEAR MAGNETIC RESONANCE
SPECTROSCOPY
SYNTHESIS
X-RAY DIFFRACTION
COMPILED DATA
HETEROCYCLIC COMPOUNDS
LIGANDS
ORGANIC SULFUR COMPOUNDS
ORGANOMETALLIC COMPOUNDS
COHERENT SCATTERING
COMPLEXES
DATA
DIFFRACTION
INFORMATION
MAGNETIC RESONANCE
NUMERICAL DATA
ORGANIC COMPOUNDS
RESONANCE
SCATTERING
TRANSITION ELEMENT COMPLEXES
400201* - Chemical & Physicochemical Properties
400102 - Chemical & Spectral Procedures