Reactions of M(Ⅱ) acetate(M = Cu,Ni) with disodium 4,4’-biphenyldisulfonate(BPDS) and 2,2’-bipyridine(2,2’-bipy) yielded three new metal sulfonates formulated as {[Cu2(2,2’-bipy)2(H2O)(C2O4)(BPDS)]·2H2O}n 1,[Cu(2,2’-Bipy)(H2O)3](BPDS)·2H2O 2 and [Ni(2,2’-Bipy)(H2O)4](BPDS)·2.5H2O 3.These three compounds were characterized by elemental analyses,FT-IR spectra,TG-DTA analyses and single-crystal X-ray diffraction analyses.Compound 1 belongs to the monoclinic system,space group P21/c with a = 17.7942(2),b = 10.1369(10),c = 19.8681(3) ,β = 104.323(10)°,V = 3472.20(7) 3,Mr = 893.82,Z = 4,F(000) = 1824,μ(CuKα) = 3.295 mm-1,R = 0.0427 and wR = 0.1278.Compound 2 is of orthorhombic system,space group Pca21 with a = 20.1016(7),b = 7.2460(2),c = 17.4802(6) ,V = 2546.10(14) 3,Mr = 622.11,Z = 4,F(000) = 1284,μ(CuKα) = 3.314 mm-1,R = 0.0415 and wR = 0.1291.Compound 3 belongs to the monoclinic system,space group C2/c with a = 15.9204(5),b = 11.7511(4),c = 15.2559(4) ,β = 98.886(3)°,V = 2819.85(15) 3,Mr = 1288.60,Z = 2,F(000) = 1340,μ(CuKα) = 2.957 mm-1,R = 0.0515 and wR = 0.1454.Compound 1 is composed of one-dimensional helical chains of [Cu2(2,2’-bipy)2(H2O)(C2O4)]2+ fragments bridged alternately by 4,4’-biphenyldisulfonate ligands,along the c axis of the unit cell.In compound 2,4,4’-biphenyldisulfonate anions are arranged in a zigzag mode and interact with the lattice waters via hydrogen bonds resulting in the formation of infinite chains.Adjacent chains are linked by lattice waters to form 2D extended sheets.The complex cations are located in the interlayer regions and interact with the sheets through hydrogen bonds.In compound 3,the Ni center resides at a crystallographic inversion center and adopts a distorted octahedral coordination sphere.The complex cations interact with 4,4’-biphenyldisulfonate anions via O-H…O hydrogen bonds,creating 2D extended grid structures.The lattice waters are located in the interlayer regions. Reactions of M (Ⅱ) acetate (M = Cu, Ni) with disodium 4,4’-biphenyldisulfonate (BPDS) and 2,2’-bipyridine (2,2’-bipy) yielded three new metal sulfonates formulated as { (2,2’-bipy) 2 (H2O) (C2O4) (BPDS)] 2H2O} n1 [Cu These three compounds were characterized by elemental analyzes, FT-IR spectra, TG-DTA analyzes and single-crystal X-ray analysis. Compound 1 (2,2’-Bipy) belongs to the monoclinic system, space group P21 / c with a = 17.7942 (2), b = 10.1369 (10), c = 19.8681 (3) β, β = 104.323 (10) °, V = 3472.20 , Mr = 893.82, Z = 4, F (000) = 1824, μ (CuKα) = 3.295 mm -1, R = 0.0427 and wR = 0.1278.Compound 2 is of orthorhombic system, space group Pca 21 with a = 20.1016 , b = 7.2460 (2), c = 17.4802 (6) , V = 2546.10 (14) 3, Mr = 622.11, Z = 4, F (000) = 1284 and μ (CuKα) = 3.314 mm -1 , R = 0.0415 and wR = 0.1291.Compound 3 belongs to the monoclinic system, space group C2 / c with a = 15.9204 (5), b = 11.7511 (4), c = 15.2559 (15) 3, Mr = 1288.60, Z = 2, F (000) = 1340, μ (CuKα) = 2.957 mm-1, R = 0.0515 and wR = 0.1454.Compound 1 is composed of one-dimensional helical chains of [Cu2 (2,2’-bipy) 2 (H2O) (C2 O4)] 2+ fragments bridged alternately by 4,4’-biphenyldisulfonate ligands along the c axis of the unit cell. In compound 2,4,4-biphenyldisulfonate anions are arranged in a zigzag mode and interact with the lattice waters via hydrogen bonds resulting in the formation of infinite chains. Adjacent chains are linked by lattice waters to form 2D extended sheets. The complex cations are located in the interlayer regions and interact with the sheets through hydrogen bonds. In compound 3, the Ni center resides at a crystallographic inversion center and adapts a distorted octahedral coordination sphere. The complex cations interact with 4,4’-biphenyldisulfonate anions via OH ... O hydrogen bonds, creating 2D extended grid structures. The lattice waters are located in the interlayer regions.