Department of Chemistry, Chemistry Research Laboratory, University of Oxford, UK.
J Am Chem Soc. 2009 Mar 4;131(8):2802-3. doi: 10.1021/ja900055j.
Reaction of an ethylenediamine (en) solution of the Zintl phase precursor K(4)Ge(9) with FeAr(2) (Ar = 2,6-Mes(2)C(6)H(3)) in the presence of 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane) yielded the endohedral Zintl ion Fe@Ge(10) (1) which was crystallographically characterized as a K(2,2,2-crypt) salt in K(2,2,2-crypt)[Fe@Ge(10)]*2en. This unprecedented Zintl ion exhibits a pentagonal prismatic 10-atom germanium cage with an interstitial iron atom in the central cavity. Confirmation of the existence of the cluster anion in solution was corroborated by positive and negative ion mode electrospray mass spectrometry.
在 2,2,2-三氮杂环十二烷（4,7,13,16,21,24-六氧杂-1,10-二氮杂环辛烷）存在下，乙二胺（en）溶液中的 Zintl 相前体 K(4)Ge(9)与 FeAr(2)（Ar = 2,6-二甲基苯）反应，生成了笼状 Zintl 离子 Fe@Ge(10)（1），并用单晶 X 射线衍射进行了结构表征。1 是 [K(2,2,2- 三氮杂环十二烷)]（+）盐的形式存在于 [K(2,2,2-三氮杂环十二烷)]（3）[Fe@Ge(10)]*2en 中。这种前所未有的 Zintl 离子呈现出五角棱柱形的 10 原子锗笼，其中铁原子位于中央腔体内。通过正离子和负离子模式电喷雾质谱证实了溶液中阴离子簇的存在。
