Challenges in chemical synthesis at the border of solution-based and solid-state chemistry—Synthesis and structure of [CH3CH2Ge9{Si(SiMe3)3}]2? - 12/05/18
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Abstract |
Polyanionic [Ge9]4– clusters are accessible in good yields by a solid-state reaction of the elements Ge and K. The nine-atom deltahedral germanium clusters are transformed to silylated species, which in a subsequent reaction allow for addition of an organic moiety. We present a synthetic method for a stepwise ligand exchange reaction at a Zintl ion. Herein, we functionalized the [Ge9{Si(SiMe3)3}2]2− cluster with an ethyl group by a reaction with bromoethane. The obtained anion [CH3CH2Ge9{Si(SiMe3)3}2]− was characterized by NMR spectroscopy and mass spectrometry. After addition of 2,2,2-crypt an abstraction of one silyl ligand was observed resulting in the crystallization of [K(2,2,2-crypt)]2[CH3CH2Ge9{Si(SiMe3)3}] representing the first monosilylated Ge9 Zintl cluster, which carries an additional ethyl group. The latter compound was characterized by single crystal X-ray crystallography, NMR spectroscopy, and elemental analysis.
Le texte complet de cet article est disponible en PDF.Keywords : Zintl cluster, Germanium, Crystal structure, Silyl ligand abstraction, Organofunctionalization
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