A complex { [Ln2( H2-DHBDC)3( H2O)4]( H2O)2}n[H2-DHBDC = 2,5-dihydroxy terephthalic acid] of Lanthanide rare earth ions and 2,5-dihydroxy terephthalic acid organic ligand was synthesized by solvothermal method. The structure and properties of the complex were analyzed and characterized by single crystal X-ray diffraction( SCXRD),elemental analysis( EA),fourier transform infrared spectrum( FTIR), thermal gravimetric analysis( TG) and fluorescence spectrum( FS),respectively. The results show that the crystal structure belongs to triclinic,space group P-1 with a = 1.0640( 8) nm,b = 1. 1239( 9) nm,c = 1. 5232( 12) nm,α = 99. 351( 11) °,β = 99. 511( 11) °,γ =92. 482( 12) °,V = 1768( 2) nm3,and Z = 2. The Tb3 +is in geometry of distorted trigondodecahedron built by eight oxygen atoms. The adjacent metal ions are connected by the 2,5-dihydroxy terephthalic acid forming a kind of three-dimension channel structure. Luminescence measuremet shows that the complex has fluorescent property.