A 2D barium complex formulated as [Ba(C 6 H 4 NO 3 )(Cl)(H 2 O)] n was successfully synthesized by gel diffusion technique using hydrosilica gel medium at room temperature. Single crystal X-ray diffraction studies confirm that the complex is triclinic with space group P 1 and exhibits a 2D framework by the interconnection of oxobridge and chlorobridge in alternative layers. The unit cell dimensions are a = 5.7737(2) Å, b = 6.8503(2) Å, c = 11.5378(4) Å, ␣ = 106.432(2) • ,  = 100.644(2) • , ␥ = 93.049(2) • . The crystal structure is further stabilized by a 3D one through a pair of N-H • • • O intermolecular hydrogen bonds to form R 2 2 (8) ring motifs. Each barium cation is nine coordinated to form distorted tricapped trigonal prism geometry. The gel grown crystals were characterized by several physico-chemical techniques including elemental analysis, FT-IR, UV-Visible spectral studies, powder X-ray diffraction and thermogravimetry.