A 2D barium complex formulated as [Ba(C6H4NO3)(Cl)(H2O)]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
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, α= 106.432(2)°, β= 100.644(2)°, γ= 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 R22(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.