A new compound, [H2N(CH3)2]2[Zn(btec)].H2O(1, H4 btec = 1,2,4,5-benzenetetracarboxylic acid) has been solvothermally synthesized and structurally characterized by singlecrystal X-ray diffraction. The crystal structure is of monoclinic, space group P21/c with a = 9.5741(3), b = 14.5044(4), c = 13.7329(5) , β = 100.582(4)°, V = 1874.61(10) 3, C14H20N2O9 Zn, Mr = 425.7, Z = 4, Dc = 1.387 g/cm3, μ = 1.349 mm-1, F(000) = 776, R = 0.0560 and w R = 0.1684 for 2834 observed reflections(I > 2σ(I)). Compound 1 based on μ4-btec and tetrahedral building unit features a three-dimensional(3D) anionic framework with mixed connected nou topology. The luminescent property and thermogravimetric analysis of compound 1 are investigated. A new compound, [H2N (CH3) 2] 2 [Zn (btec)]. H20 (1, H4 btec = 1,2,4,5-benzenetetracarboxylic acid) has been solvothermally synthesized and structurally characterized by singlecrystal X-ray diffraction . The crystal structure is of monoclinic, space group P21 / c with a = 9.5741 (3), b = 14.5044 (4), c = 13.7329 5, β = 100.582 (4) °, V = 1874.61 (10) 3, C14H20N2O9 Zn, Mr = 425.7, Z = 4, Dc = 1.387 g / cm3, μ = 1.349 mm-1, F (000) = 776, R = 0.0560 and w R = 0.1684 for 2834 observed reflections (I> 2σ (I)). Compound 1 based on μ4-btec and tetrahedral building unit features a three-dimensional (3D) anionic framework with mixed connected nou topology. The luminescent property and thermogravimetric analysis of compound 1 are investigated.