Hydrothermal reactions of N,N′-di-3-pyridyladipoamide (L) with 1,2,4,5-benzenetetracarboxylic acid (1,2,4,5-H 2 btec) in water without and with NaOH afforded [Co(L)(1,2,4,5btec) 0.5 ] n , 1, and [Co(L)(1,2,4,5-btec) 0.5 (H 2 O) 2 ] n , 2, respectively, while immersion of 1 into water at room temperature gave {[Co(L) 0.5 (1,2,4,5-btec) 0.5 (H 2 O) 4 ]•2H 2 O} n , 3, which have been structurally characterized. Complexes 1−3 display a 2-fold interpenetrated 3D framework, a unique 2D layer, and a 1D chain, respectively. While complexes 1 and 2 adopt the same point symbol of (4.6 4 .8) 2 (4 2 .6 2 .8 2 ) for nets, they differ in the vertex symbols that are [4.