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The cation radical salt of dimethylthiotetrathiafulvalene bisannulated tetraoxatetrathiatetracosane with linear pentaiodide and triiodide counterions was prepared by electrocrystallization. Within the crystal, linear I5 - and I3 - form a cage-like network, in which isolated cation radicals are located. The formation of linear I5 - was also confirmed by the optical spectra.

Charge-transfer complexes of bis(methylthio)tetrathiafulvalene (DMT-TTF) bisannulated macrocycles with 2,3,5,6-tetrafluoro-7,7,8,8-tetracyanoquinodimethane (F4-TCNQ) were prepared. The crystal structural analysis revealed an intramolecular dimer structure with the π-π overlap of DMT-TTF units. The magnitude of intramolecular π-π overlap depends on the ring size of macrocycles.

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