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The synthesis and structure of a macrocyclic dinickel complex incorporating a hypercoordinated sulfenium(II) cation are reported. The novel complex [Ni2L3(Cl)]2+ was obtained from a reaction of the per‐hydroxyethylated N6S2 macrocycle H2L2 with NiCl2(H2O)6 in the presence of air, and isolated as its ClO4 or BPh4 salt. The structure reveals a three‐coordinate sulfenium cation that is stabilized by...
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