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. 2020 Oct 21;142(44):18859–18865. doi: 10.1021/jacs.0c07977

Scheme 1. Synthesis of (FeII)5-Coordinated Pentafoil Knot Complex 2 and (FeII)6-Coordinated Star of David [2]Catenane Complex 3 from Ligand 1.

Scheme 1

Pentafoil knot 2 is isolated and used with a chloride anion bound in the central cavity. The Star of David [2]catenane 3 was treated with Na4EDTA to generate the demetalated link 4.

Reagents and conditions: (a) FeCl2, dimethyl sulfoxide, 60 °C, 24 h followed by excess saturated aqueous KPF6 solution; (b) Hoveyda-Grubbs second-generation catalyst (H2IMes)Cl2RuCH(o-OiPrC6H4), 1,2-dichloroethane/MeNO2 (1:1), 60 °C, 24 h followed by excess saturated aqueous KPF6 solution; (c) FeSO4·7H2O, ethylene glycol, 170 °C, 24 h followed by excess saturated KPF6 in methanol; (d) Na4EDTA (EDTA = ethylenediaminetetraacetic acid), H2O/MeCN (1:1), 80 °C, 4 h.