We synthesized a new diacetylene monomer with urethane groups in the middle of the substituents and tetrathiafulvalene (TTF) moieties at both ends (BT). BT was found to form the CT complex with tetrafluorotetracyanoquinodimethane (F(4)TCNQ) to be (BT)(F(4)TCNQ)(2). BT could be polymerized in the solid state to give irregular conjugated structure by UV irradiation although the solid-state polymerization of the CT complex was not confirmed. Morphology of their cast films was observed by AFM. The films of (BT)(F(4)TCNQ)(2) before and after UV irradiation showed semiconducting temperature dependence with activation energies of 0.19 and 0.16 eV, respectively, and the electrical conductivities at room temperature were found to be more than 10(-5) Scm(-1).