Abstract: | Four transition metal coordination compounds, {[Co(PPDA)(H2O)2]}n (1), {[Ni(HPPDA)2]}n (2), {[Cd(PPDA)(H2O)]?H2O}n (3), and {Zn(HPPDA)2(H2O)4}n (4), were synthesized by assembling transition metal salts with a semirigid ligand 4-(pyridin-3-yloxy)-phthalic acid (H2PPDA) under hydrothermal conditions. The compounds have been characterized by elemental analyses, IR spectra, TGA, powder X-ray diffraction, and single-crystal X-ray crystallography. Compound 1 exhibits a three-connected 2-D layered structure, 2 shows a (3,6)-connected 2-D layered structure, 3 displays a (3,6)-connected 2-D layered framework based on binuclear units, and 4 is a mononuclear structure, connected to generate a 3-D supramolecular architecture by hydrogen bonds. Compound 2 is thermally stable up to 300 °C. The magnetic properties of 1 and photoluminescent properties of 3 and 4 have been explored. |