From tin(II) to tin(IV): Following solid‐liquid reactions by microscopy

Hans Reuter, Simona Schröder, Natalie Röwekamp-Krugley, Markus Imwalle
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Abstract

In order to study the formation of complexes independently from stoichiometry we developed a microscale experiment that allows us to monitor the reaction progress by light microscopy In the present study, the complex formation between SnF2 and 1,10‐phenanthroline (phen) with N,N‐dimethylformamide as solvent was investigated over a period of some weeks. By use of this setup, the formation of three different crystals has been observed, whose compositions and structures were determined by single crystal X‐ray diffraction: 3SnF2 · phen, 1, 2SnF2 · SnF4 · phen, 2, SnF4 · phen, 3. While the octahedral fluorine environment of the tin(IV) atoms of 2 and 3 is very regular, the coordinations of the tin(II) atoms in 1 and 2 is irregular. Assuming a non‐bonding 5s electron pair, classical 2c‐2e‐ and symmetrical and asymmetrical, hypervalent 3c‐4e‐bonds ‐ all based on the orthogonal p atomic orbitals of Sn – an approach to analyse and describe these coordinations in a simple comprehensive way is presented.
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从锡(II)到锡(IV):用显微镜跟踪固液反应
为了研究络合物的形成而不受化学计量学的影响,我们开发了一种微尺度实验,使我们能够通过光学显微镜监测反应的进展。通过使用这种装置,观察到了三种不同晶体的形成,并通过单晶 X 射线衍射确定了它们的成分和结构:2 和 3 中锡(IV)原子的八面体氟环境非常规则,而 1 和 2 中锡(II)原子的配位则不规则。假定存在非成键的 5s 电子对、经典的 2c-2e-、对称和不对称的高价 3c-4e-键--所有这些都基于锡的正交 p 原子轨道--本文提出了一种以简单全面的方式分析和描述这些配位的方法。
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