Low-temperature hydrothermal technique was employed for the synthesis of highly porous and crystalline MIL-101(Cr) metal-organic frameworks series. The resulting as-synthesized MOFs were characterized by Fourier transform infrared (FTIR) spectroscopy, powdered X-ray diffraction (XRD), scanning electron microscopy (SEM), nitrogen adsorption-desorption analysis, thermogravimetric analysis (TGA), photoluminescence (PL) spectroscopy, and ultraviolet-visible (UV-vis) diffuse reflectance spectroscopy. The photocatalytic activity of the MOFs was evaluated for degradation of phenanthrene (PHE) under visible light irradiation. Among the MOFs, MIL-101@160 has the highest Brunner Emmett-Teller (BET) specific surface area and corresponding pore volume of 2,592.2 m2g-1 and 1.09 cm3g-1, respectively. Furthermore, it has shown higher photocatalytic degradation of the PHE than other samples with 98% degradation efficiency achieved within 150 minutes.