A Distorted Tetrahedral Metal Oxide Cluster inside an Icosahedral Carbon Cage. Synthesis, Isolation, and Structural Characterization of Sc4(μ3-O)2@I h -C80

The remarkably large cluster Sc4(μ3-O)2 has been obtained trapped inside an I h -C80 cage by conducting the vaporization of graphite rods doped with copper(II) nitrate and scandium(III) oxide in an electric arc under a low pressure helium atmosphere with an added flow of air. The product has been is...

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Bibliographic Details
Published in:Journal of the American Chemical Society 2008-09, Vol.130 (36), p.11844-11845
Main Authors: Stevenson, Steven, Mackey, Mary A, Stuart, Melissa A, Phillips, J. Paige, Easterling, Michael L, Chancellor, Christopher J, Olmstead, Marilyn M, Balch, Alan L
Format: Article
Language:English
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Summary:The remarkably large cluster Sc4(μ3-O)2 has been obtained trapped inside an I h -C80 cage by conducting the vaporization of graphite rods doped with copper(II) nitrate and scandium(III) oxide in an electric arc under a low pressure helium atmosphere with an added flow of air. The product has been isolated by chromatography and identified by high-resolution mass spectrometry. The structure of Sc4(μ3-O)2@I h -C80 has been determined by X-ray crystallography on a crystal of Sc4(μ3-O)2@I h -C80·NiII(OEP)·2(C6H6). The Sc4(μ3-O)2 unit consists of a distorted tetrahedron of scandium atoms with oxygen atoms bridging two of its faces. The Sc−Sc distances range from 2.946(7) to 3.379(7) Å.
ISSN:0002-7863
1520-5126
DOI:10.1021/ja803679u