The synthesis of 1, 2, 9, 16, 17, 24-hexathia [2.1. 2.1]-4, 6, 8, 11, 13, 15, 19, 21, 23, 26, 28, 30-dodecamethyl-metacyclophane by direct sulphuration of mesitylene, the first report of a single-step synthesis of an aromatic macrocycle with alternating sulphide and disulphide linkages, is reported. Structure determination of this compound was achieved by mass spectrometry, and by reductive degradation to 3, 3'-dithio-dimesitylsulphide and ...