ABSTRACT 2,2′-Butanediyl-bisisoquinolinium diiodide (DIQC4I2) was synthesized by reaction of isoquinoline with 1,4-diiodobutane. This salt was further reacted with TCNQ and TCNQ− to obtain the charge transfer complex DIQC4⋅TCNQ3. This charge transfer complex was characterized by elemental analysis, infrared, electronic, and mass spectrometry. The crystal structure of DIQC4⋅TCNQ3 is triclinic with a = 8.1478(11), b = 10.2302(13), c = 15.041(2)Å, α = 80.987(10), β = 81.335(10), γ = 70.402(10), Z = 1, and space group P¯1. The donors and acceptors are packed in segregated columns. The IR spectrum shows a very strong absorption envelope in the range of 4000 to 1000 cm−1 resulting from the electronic conduction band. The electrical conductivity of DIQC4⋅TCNQ3 is 2.4 × 10−2 S/cm at room temperature with activation energy 0.20 eV, typical of semiconductor behavior.