Herein, we report new porous coordination polymers (PCPs) via a facile synthetic approach called "in situ generation of functionality in the ligand". Upon a synthetic process of PCPs, a neutral (-CH2OH) or a cationic functionality (-CH2[4,4'-bipyridine](+)) was generated on a isophthalate ligand from a reactive haloalkane (-CH2Br) moiety, affording two new PCPs. The PCPs have two-dimensional layered structures with large potential solvent-accessible voids for CO2 adsorption.