The complex [Cu(m-NBA)(2,2'-bipy)(H2O)(2)]center dot m-NBA center dot H2O was obtained by self-assembly of m-nitrobenzoic acid. 2,2'-bipyridine and copper(II). The crystal structure of the complex has been determined by X-ray diffraction single crystal Structure analysis. The crystal belongs to monoclinic system, space group P2(1)/n. The cell parameters are: a=0.705 65(9) nm, b=2.901 2(4) nm, c=1.271 52(2) nm; beta=92.895(2)degrees, and V=2.599 8(6) nm(3), D-c= 1.551 g.cm(-3), Z=4, mu(Mo K alpha)=9.09 cm(-1), F(000)=1 244, R-1=0.0407, omega R-2=0.085 5[I>2 sigma(I)]. The crystal structure shows that the copper M ion is coordinated with two nitrogen atoms from one 2,2'-bipyridine Molecule, one oxygen atom from one m-nitrobenzoic acid Molecule and and two oxygen atoms from two water molecules, forming a distorted coordination square-pyramid. The cyclic voltametric behavior of the complex was also studied. CCDC: 687131.