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Hydrothermal reactions of manganese (II)/cadmium(II) salts with 1,2,4-trimellitic acid (H3tma) and 2,2′:6′,2-terpyridine (tpy) result in two novel complexes formulated with [M(Htma)(tpy)]·H2O (M = Mn(1) and Cd(2)). X-ray diffraction structural analyses of two complexes reveal they are isomorphic except for the different center metal ions and crystallize in the monoclinic crystal system of P(2)/n space group. The metal ion lies in a six-coordinated distorted octahedral environment coordinated with three Htma2− anions and one tpy ligand. There is an infinite two-dimensional rhombic network based on the metallic dimmers and Htma2− anions with the tpy ligands in void. Furthermore, the tpy ligands from the adjacent network weakly interact each other by π⋯π packing interactions into 3D supramolecular structure. The fluorescence properties could be assigned to the π – π* transition of organic ligands.