Salicylaldimines: Formation via Ring Contraction and Synthesis of Mono- and Heterobimetallic Alkali Metal Heterocubanes,Inorganic Chemistry

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Salicylaldimines: Formation via Ring Contraction and Synthesis of Mono- and Heterobimetallic Alkali Metal Heterocubanes
Inorganic Chemistry ( IF 4.3 ) Pub Date : 2020-11-23 , DOI: 10.1021/acs.inorgchem.0c02920
Anna Hanft ₁ , Malte Jürgensen ₁ , Laura Wolz ₁ , Krzysztof Radacki ₁ , Crispin Lichtenberg ₁

Affiliation

The formation of salicylaldimine derivatives via ring contraction as byproducts in 2-aminotropone syntheses has been investigated. Salicylaldiminate (SAI) complexes of the alkali metals Li–K have been synthesized and transformed into heterobimetallic complexes. Important findings include an unusual double heterocubane structure of the homometallic sodium SAI, an unprecedented ligand-induced E/Z isomerization of the aldimine functional group in the homometallic potassium SAI, and the first example of a structurally authenticated mixed-metal SAI based on s-block central atoms. Rapid equilibria have been shown to play a crucial role in the solution phase chemistry of mixed-metal SAIs. Analytical techniques applied in this work include (heteronuclear) NMR spectroscopy, VT- and DOSY NMR spectroscopy, high-resolution mass spectrometry, single-crystal X-ray diffraction analysis, and DFT calculations.

中文翻译：

水杨醛亚胺：通过环收缩形成和合成单金属和异双金属碱金属杂种。

已经研究了通过2-甲基萘酮合成中的副产物环收缩形成的水杨醛亚胺衍生物。已经合成了碱金属Li–K的水杨醛二酰亚胺（SAI）配合物，并将其转变为异双金属配合物。重要发现包括同金属钠SAI的非同寻常的双重异源结构，一种前所未有的配体诱导的E / Z均金属钾SAI中醛亚胺官能团的异构化，以及基于s嵌段中心原子的结构鉴定混合金属SAI的第一个例子。快速平衡已显示在混合金属SAI的溶液相化学中起着至关重要的作用。在这项工作中应用的分析技术包括（异核）NMR光谱，VT-和DOSY NMR光谱，高分辨率质谱，单晶X射线衍射分析和DFT计算。

更新日期：2020-12-07

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