School of Chemistry, University of Manchester, Oxford Road, Manchester M13 9PL, UK.
Nat Chem. 2014 Nov;6(11):978-82. doi: 10.1038/nchem.2056. Epub 2014 Sep 21.
We describe the synthesis of a [2]catenane that consists of two triply entwined 114-membered rings, a molecular link. The woven scaffold is a hexameric circular helicate generated by the assembly of six tris(bipyridine) ligands with six iron(II) cations, with the size of the helicate promoted by the use of sulfate counterions. The structure of the ligand extension directs subsequent covalent capture of the catenane by ring-closing olefin metathesis. Confirmation of the Star of David topology (two rings, six crossings) is provided by NMR spectroscopy, mass spectrometry and X-ray crystallography. Extraction of the iron(II) ions with tetrasodium ethylenediaminetetraacetate affords the wholly organic molecular link. The self-assembly of interwoven circular frameworks of controlled size, and their subsequent closure by multiple directed covalent bond-forming reactions, provides a powerful strategy for the synthesis of molecular topologies of ever-increasing complexity.
我们描述了一种[2]索烃的合成，该索烃由两个三重交织的 114 元环组成，是一种分子连接物。编织支架是由六个三联吡啶配体与六个二价铁离子组装而成的六元环状螺旋体，螺旋体的尺寸通过使用硫酸盐抗衡离子来促进。配体延伸的结构指导随后通过闭环烯烃复分解反应进行索烃的共价捕获。通过 NMR 光谱、质谱和 X 射线晶体学证实了大卫之星拓扑结构（两个环，六个交叉点）。用四钠乙二胺四乙酸提取二价铁离子得到全有机分子连接物。通过交织的圆形框架的自组装，控制其大小，并通过多个定向的共价键形成反应进行后续的闭合，为合成越来越复杂的分子拓扑结构提供了一种强大的策略。
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