Two new coordination complexes, formulated as [Cd-2(3-NPA)(phen)(4)(H2O)(2)](2) (1) and [Zn(3-NPA)(phen)(H2O)](n) (2) (3-NPAH(2) = 3-nitrophthalic acid, phen = 1,10-phenanthroline) have been synthesized by hydrothermal reactions of the rigid neutral ligand phen with metal ions in the presence of 3-NPAH. X-ray analysis shows that complex 1 is a 0D dinuclear structure that is arranged to form a 3D supramolecular framework through hydrogen bonds and pi-pi stacking interactions. In polymer 2, the 3-NPA(2-) anions coordinate the Cd(II) ions in a tridentate mode to form a 1D infinite chain structure, which is connected by the hydrogen bonds and pi-pi stacking interactions resulting in a 3D supramolecular architecture. In addition, the two complexes were characterized by infrared spectroscopy, elemental analysis, luminescent properties, thermo gravimetric analysis, and powder X-ray diffraction (PXRD).