A distorted tetrahedral metal oxide cluster inside an lcosahedral carbon cage.: Synthesis, isolation, and structural characterization of Sc4(μ3-O)2@Ih-C80

A distorted tetrahedral metal oxide cluster inside an lcosahedral carbon cage.: Synthesis, isolation, and structural characterization of Sc4(μ3-O)2@Ih-C80
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DOI:
10.1021/ja803679u
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发表时间:
2008-09-10
影响因子:
15
通讯作者:
Balch, Alan L.
Balch, Alan L.
中科院分区:
化学1区
文献类型:
--
作者:
Stevenson, Steven;Mackey, Mary A.;Balch, Alan L.

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通过在低压氦气氛和附加空气流下在电弧中对掺杂有硝酸铜(II)和氧化钪(III)的石墨棒进行汽化,获得了捕获在Ih-C80笼内的非常大的簇Sc4(μ3-O)2。该产物已通过色谱法分离并通过高分辨率质谱法鉴定。通过X射线晶体学方法对Sc4(μ3-O)2@Ih-C80·NiII(OEP)·2(C6H6)晶体确定了Sc4(μ3-O)2@Ih-C80的结构。 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) Å。
The remarkably large cluster Sc4(μ3-O)2has been obtained trapped inside anIh-C80cage 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@Ih-C80has been determined by X-ray crystallography on a crystal of Sc4(μ3-O)2@Ih-C80·NiII(OEP)·2(C6H6). The Sc4(μ3-O)2unit 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.