一个二十面体碳笼内的扭曲四面体金属氧化物簇。Sc4(μ3-O)2@Ih-C80的合成、分离及结构表征
A distorted tetrahedral metal oxide cluster inside an icosahedral carbon cage. Synthesis, isolation, and structural characterization of Sc4(mu3-O)2@Ih-C80.
作者信息
Stevenson Steven, Mackey Mary A, Stuart Melissa A, Phillips J Paige, Easterling Michael L, Chancellor Christopher J, Olmstead Marilyn M, Balch Alan L
机构信息
Department of Chemistry, University of Southern Mississippi, Hattiesburg, Mississippi 39406, USA.
出版信息
J Am Chem Soc. 2008 Sep 10;130(36):11844-5. doi: 10.1021/ja803679u. Epub 2008 Aug 15.
The remarkably large cluster Sc4(mu3-O)2 has been obtained trapped inside an Ih-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(mu3-O)2@Ih-C80 has been determined by X-ray crystallography on a crystal of Sc4(mu3-O)2@Ih-C80.NiII(OEP).2(C6H6). The Sc4(mu3-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) A.
通过在低压氦气氛下添加空气流的电弧中蒸发掺杂有硝酸铜（II）和氧化钪（III）的石墨棒，获得了被困在Ih-C80笼内的非常大的簇合物Sc4(μ3-O)2。产物通过色谱法分离并通过高分辨率质谱法鉴定。Sc4(μ3-O)2@Ih-C80的结构已通过对Sc4(μ3-O)2@Ih-C80.NiII(OEP).2(C6H6)晶体进行X射线晶体学测定。Sc4(μ3-O)2单元由钪原子的扭曲四面体组成，氧原子桥接其两个面。Sc-Sc距离范围为2.946(7)至3.379(7)埃。
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