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Tetramercaptotetrathiacalix[4]arene ( LH 4  ) can be used as a coordination platform to bind four Cu I  ions at the thiolate and thioether S atoms. Donor ligands such as phosphanes can stabilize the resulting  [LCu 4 ]  units, which then remain monomeric ( [(Ph 3 PCu) 4 L] ). In the absence of donor ligands, they aggregate, providing a hexamer ( [LCu 4 ] 6  ) in high yields, with a hollow‐sphere structure formed by an unprecedented Cu 24 S 48  cage that is surrounded by the organic framework of the calixarene chalices. Preliminary NMR experiments with regard to the host‐guest chemistry in solution showed that the compound represents a polytopic host for acetonitrile and methane.

angewandte chemie international edition

Mercaptothiacalixarenes Steer 24 Copper(I) Centers to form a Hollow‐Sphere Structure Featuring Cu 2 S 2  Motifs with Exceptionally Short Cu⋅⋅⋅Cu Distances