Two novel complexes, {Cu 2 [5-(NO 2 )sal] 2 (DMF) 4 } 2 (1) and{Co )sal] (H 2 O) 3 } 2 (2), have been prepared and characterized by elemental analysis, IR spectrum, and X-ray single-crystal diffraction. Complex 1 is a four nuclear Cu(II) complex and belongs to monoclinic system with space group C 2/c, a = 23.541 (2) Å, b = 14.8150(12) Å, c = 22.459(2) Å, β = 104.361(2) • , V = 7588.0(12) Å 3 , D c = 1.368 Mg/m 3 , Z = 4, F(000) = 3216, R 1 = 0.0826, wR 2 = 0.2212 [I>2σ (I)] Every Cu(II) atom is six-coordinated by three O atoms from two 5-(NO 2 )sal and two O atoms from two DMF and one bridged O atom. The distance of Cu···Cu are 4.5027(14), 5.817(2), and 5.526(2) Å. Complex 2 is a dinuclear Co(II) complex and belongs to monoclinic system with space group P 2 1 /c, a = 10.9003(9) Å, b = 13.6938(15) Å, c = 6.6781(5) Å, β = 91.223(1) • , V = 996.59(16) Å 3 , D c = 1.748 Mg/m 3 , Z = 2, F(000) = 596, R 1 = 0.1058, wR 2 = 0.3098 [I>2σ (I)] Every Co(II) atom is sixcoordinated by two O atoms from one 5-(NO 2 )sal and three O atoms from three coordinated water and one bridged O atom, and the distance of Co···Co is 3.191(3) Å. Two complexes have been screened for antibacterial activities by the agar-diffusion method and showed good effects against Escherichia coli, Staphylococcus aureus, and Bacillus subtilis. (5-(NO 2 )sal = 5-nitrosalicylate anion, DMF = N, N-dimethylformamide).