Two novel divalent transition metal disulfonates were synthesized and characterized by X-ray single crystal diffraction. [Ni (cyclam) (1, 5 nds)] . 1/3 H2O (1) crystallized in space group P2 (1)/c with unit cell parameters a = 8.583 (5), b = 10.533 (6), c = 12.946 (7) Angstrom, and beta = 0.433(9)degrees The Ni2+ center is coordinated by the cyclam ligand and two sulfonate groups. The interactions between [ Ni (cyclam)](2+) and the sulfonates are further enhanced by multiple hydrogen bonds of type O2S-(OH)-H-...-N [Co(cyclam)(H2O)(2)] (1, 5nds) (.) 2H(2)O (2) crystallized in space group P1 with unit cell parameters a = 8.738(5), b = 9. 324(5)degrees c = 10.118(5)A, a = 81.382 (8), beta = 64.868 (8), and gamma = 62.999 (8)degrees. The sulfonate groups do not have any direct contact with the Co2+ center, instead, they form second sphere coordination with Ni2+, via hydrogen bonds and extend the structure into a 3-D network.