The newly synthesized complex (2) of copper(I) chloride with di n hexyl 2,2´ biquinoline 4,4´ dicarboxylate (L) was spectroscopically and electrochemically characterized. The X ray diffraction study showed that the crystals of complex 2 consist of the dinuclear moieties [L 2 Cu I 2 (μ Cl) 2 ] containing Cu 2 (μ Cl) 2 clusters. Spectrophotometric studies and ESI mass spec trometric measurements showed that after the dissolution of complex 2 in acetonitrile (AN) and N methyl 2 pyrrolidone (NMP), the solution contained not only the dinuclear complexes [L 2 Cu I 2 (μ Cl) 2 ] but also [L 2 Cu I ]Cl, [LCu I Cl(Sol)], and [Cu I Cl(Sol)] (Sol is the solvent). The electrochemical data also confirm the conclusion that bridged dinuclear chloride complex 2 dissociates both in NMP and AN to form the tetrahedral bis biquinoline complex [L 2 Cu I ]Cl. In solutions of complex 2 in alcohols and N,N dimethylformamide (DMF), only [L 2 Cu I ]Cl and [Cu I Cl(Sol)] are present. In EtOH, AN, and DMF, [Cu I Cl(Sol)] undergoes disproportionation to [Cu II Cl(Sol)] and Cu 0 .