Four new coordination polymers have been synthesized based on a mixed-ligand strategy, viz., ], SSICG-3; and [Zn 2 (ATRZ) 2 (NIPA)], SSICG-4 (4-ABPT = 3,5-di(pyridine-4-yl)-4H-1,2,4-triazol-4-amine, H 2 NIPA = 5-nitroisophthalic acid, and ATRZ = 3-amino-1,2,4-triazole, SSICG stands for the Solid State and Inorganic Chemistry Group at IIT Patna). The copper compounds are one-dimensional, whereas the nickel and zinc compounds are two-dimensional layer compounds. SSICG-3 possesses 4,4-net topology with a Schlafi symbol 4 4 .6 2 , whereas SSICG-4 exhibits a 3,3-net (fes) topology with a Schlafi symbol 4.8 2 . SSICG-1 and SSICG-3 have active metal sites due to the presence of replaceable coordinated water molecules and exhibits efficient catalytic activity for one-pot CO 2 cycloadditions. The conversions of SSICG-1 and SSICG-3 for CO 2 cycloaddition are 87 and 95% (turnover numbers (TON) of 174 and 190), respectively. The kinetic studies, substrate scope, recyclability, catalyst amount, and temperature dependence studies of the CO 2 cycloaddition reaction are discussed. These structurally diverse coordination polymers could contribute to broadening the scope of mixed-ligand coordination polymers for their applications in heterogeneous catalysis.