A novel Ca(II) complex material was prepared by reaction of O-nitrobenzaldehyde-3-amino-benzenesulfonic acid with Ca(ClO4)(2), and characterized by X-ray single crystal diffraction method. The analytical results shows that the Ca(II) complex was crystallized in the monoclinic system, space group P2(1)/c, with a = 17.515(10) angstrom, b = 7.019(4) angstrom, c = 13.853(8) angstrom, beta = 104.855(10) degrees, V = 1646.3(17) angstrom(3), Z = 2. The geometry of Ca(II) is a slightly distorted dodecahedrall geometry. In the crystal packing, the complex molecules form layered structure by the pi-pi packing interaction, and the molecules form a one-dimensional chain structure by hydrogen bonds.