A novel heterometallic coordination polymer {[Cd2(NiL)2(Btca)4] · H2O} n (I) (H2L = 2,3-dioxo5,6,14,15-dibenzo-1,4,8,12-tetraazacyclo-pentadeca-7,13-dien, H2Btca = benzotriazole-5-carboxylic acid) was synthesized and structurally characterized by elemental analysis, IR spectroscopy, and single crystal X-ray diffraction (CIF file CCDC no. 1043065). Complex I exhibits a two-dimensional network structure formed by Cd2Ni2 units via the oxamide and benzotriazole-5-carboxylate bridges. It crystallizes in the monoclinic system, space group P21/c. The lattice parameters are: a = 1.24488(8), b = 2.75370(19), c = 1.49336(10) Å, β = 103.1070(10)° and V = 4.9859(6) Å3, Z = 4. The fluorescence properties of compound I are also discussed.