One-three-dimensional metal-organic frameworks Mg 1.5 (C 12 H 6 O 4 ) 1.5 (C 3 H 7 NO) 2 (MgNDC) has been synthesized solvothermally and characterized by single crystal XRD, powder XRD, FT-IR spectra. The low-temperature molar heat capacities of MgNDC were measured by temperature modulated differential scanning calorimetry (TMDSC) over the temperature range from 205 to 470 K for the first time. No phase transition or thermal anomaly was observed in the experimental temperature range. The thermodynamic parameters of MgNDC such as entropy and enthalpy relative to reference temperature of 298.15 K were derived based on the above molar heat capacities data. Moreover, the thermal stability and decomposition of MgNDC was further investigated through thermogravimetry (TG)-mass spectrometer (MS). Three stages of mass loss were observed in the TG curve. TG-MS curve indicated that the oxidative degradation products of MgNDC are mainly H 2 O, CO 2 , NO, and NO 2 .