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Metal-organic frameworks (MOFs) have exhibited excellent properties in many areas such as luminescence, catalysis, magnetism, and gas storage.Using the bridging ligand 1,3,5-benzene tricarboxylate acid (H3BTC) and the second terminal molecular 1,10-phenanthroline (phen) as coligand, a series of novel three-demensional metal-organic frameworks with different metal centers based on the same structure denoted as [M5(μ3-OH)(BTC)3(phen)4]·5H2O (M=Zn, Mn).These single crystals have been synthesized under mild solvothermal condition and structurally characterized by means of single-crystal X-ray diffraction and X-ray powder diffraction.The pH value is the essential key to control the structure type.Further characterization was carried on with the aid of UV-vis spectra, IR spectra and TG analyses.UV-vis spectra shows the absorption band in visible region and high thermal stability can be achieved own to the existence of terminal ligand phen.The SBUs in the above strucures include binuclear and trinuclear clusters.Detailed structural information indicated that MOFs with different metal center exhibit slight shifts in both bond length and bond angle.