Teraaza- and hexaazacyclophanes have been synthesized via a one-step palladium catalyzed amination reaction. The chemical oxidation of cyclophanes leads to the formation of radical cations, the presence of which was manifested by the appearance of new bands in UV-Vis-NIR and IR spectra. Spins of radical cations can be magnetically coupled. The nutation pulsed-EPR technique (PEANUT experiment) enables us to determine the multiplicity of the systems for different oxidant/cyclophane ratios. Spins of cyclophanes oxidized to diradical dications interact ferromagnetically to form a pure triplet state.