A novel heterometallic coordination polymer {[Cd 2 (NiL) 2 (Btca) 4 ] ⋅ H 2 O} n (I) (H 2 L = 2,3 dioxo 5,6,14,15 dibenzo 1,4,8,12 tetraazacyclo pentadeca 7,13 dien, H 2 Btca = 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 Cd 2 Ni 2 units via the oxamide and benzotriazole 5 carboxylate bridges. It crystallizes in the mon oclinic system, space group P2 1 /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) Å 3 , Z = 4. The fluorescence properties of compound I are also discussed.