Abstract Depolymerisation of a copper(II)/pyrrolidine-based 2D -polymer 2 by 4,4′-bipyridyl [molar ratio: 2 (CuL2) : 1 (Bipy)] and recrystallisation of the reaction product leads to two visually distinguishable crystal charges, composed of dark green octahedra meso-4 and light green rod-shaped crystals racem-5. Separation of the conglomerate of the morphologically different crystals is accomplished by pick out. The structure of the dinuelear complex racem-5 has been established unambigously by X-ray structure analysis. EPR and susceptibility measurements of mixtures of complex meso-4 and racem-5 indicate that there is no interaction between the two copper(II) centres.