A new bis(pyrazolecarboxylate) ligand, 1,3-phenylenebis-(1H-pyrazole-5-carboxylic acid) (H 2 PBPC) has been synthesized to study the structure and intriguing properties of the resultant coordination polymers synthesized under solvothermal conditions. The reaction of H 2 PBPC with Cu(ClO 4 ) 2 in the presence of NaOH at two different temperatures (80 and 120°C) resulted in two coordination polymers, namely, [{Cu 2 Na(H 2 OPBPC)}] ϱ (1) and [{Cu 4 Na 2 (H 2 OPBPC) 2 }] ϱ (2), which display 2D corrugated sheet and 3D staircase architectures, respectively; in these structures, the aromatic C-H bond flanked by the pyrazolecarboxylate moieties was oxidized to form a C-O bond. When 2,2Ј-bipyridine (2,2Ј-bpy)[a] 5874 was used instead of NaOH, [{Cu 2 (2,2Ј-bpy) 2 (H 2 PBPC)}-(H 2 O)] ϱ (3) formed, and such C-H bond activation was not observed. Interestingly, one of the coordination polymers, namely, 1, displayed catecholase and phosphatase activity. Variable-temperature magnetic susceptibility data in the range 2-300 K showed that there is antiferromagnetic coupling between the metal centers of 1 and 2 that is mediated through the phenoxo and pyrazole bridges, whereas 3 revealed dominant ferromagnetic interactions between the bis-(pyrazolato)-bridged Cu II centers owing to its very unusual Cu-N-N-Cu torsion angles of 75.28 and 69.52°.