Ayari Jihed, Göb Christian R, Oppel Iris M, Lutter Michael, Hiller Wolf, Jurkschat Klaus
Fakultät für Chemie und Chemische Biologie, Technische Universität Dortmund, Otto-Hahn-Straße 6, 44227, Dortmund, Germany.
Institut für Anorganische Chemie, RWTH Aachen, 52056, Aachen, Germany.
Angew Chem Int Ed Engl. 2020 Dec 21;59(52):23892-23898. doi: 10.1002/anie.202012248. Epub 2020 Oct 19.
The syntheses of the novel silicon-bridged tris(tetraorganotin) compounds MeSi(CH SnPh R) (2, R=Ph; 5, R=Me SiCH ) and their halogen-substituted derivatives MeSi(CH SnPh I ) (3, n=1; 4, n=2) and MeSi(CH SnI R) (6, R=Me SiCH ) are reported. The reaction of compound 4 with di-t-butyltin oxide (t-Bu SnO) gives the oktokaideka-nuclear (18-nuclear) molecular diorganotin oxide [MeSi(CH SnPhO) ] (7) while the reaction of 6 with sodium hydroxide, NaOH, provides the trikonta-nuclear (30-nuclear) molecular diorganotin oxide [MeSi(CH SnRO) ] (8, R=Me SiCH ). Both 7 and 8 show belt-like ladder-type macrocyclic structures and are by far the biggest molecular diorganotin oxides reported to date. The compounds have been characterized by elemental analyses, electrospray mass spectrometry (ESI-MS), NMR spectroscopy, H DOSY NMR spectroscopy (7), IR spectroscopy (7, 8), and single-crystal X-ray diffraction analysis (2, 7, 8).
报道了新型硅桥连三(四有机锡)化合物MeSi(CH₂SnPh₃)₃(2, R = Ph; 5, R = Me₃SiCH₂)及其卤代衍生物MeSi(CH₂SnPh₂I)ₙ(3, n = 1; 4, n = 2)和MeSi(CH₂SnIR₂)(6, R = Me₃SiCH₂)的合成。化合物4与二叔丁基氧化锡(t-Bu₂SnO)反应生成十八核分子二有机锡氧化物[MeSi(CH₂SnPhO)₃]₂(7),而6与氢氧化钠(NaOH)反应得到三十核分子二有机锡氧化物[MeSi(CH₂SnRO)₃]₁₀(8, R = Me₃SiCH₂)。7和8均呈现带状梯型大环结构,是迄今为止报道的最大的分子二有机锡氧化物。这些化合物通过元素分析、电喷雾质谱(ESI-MS)、核磁共振光谱、¹H DOSY核磁共振光谱(7)、红外光谱(7, 8)以及单晶X射线衍射分析(2, 7, 8)进行了表征。