A new compound {[Bi(trans-DAM)(cis-DAM)(H2O)]NO3·H2O}n 1 derived from bismuth and the flexible ligand N,N’-diacetic acid imidazolium chloride (H2DAMCl) was obtained by hydrothermal synthesis and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic P21/c space group with a = 9.2298(18), b = 13.339(3), c = 17.090(3) , β = 105.38(2)o, V = 2028.7(7) 3, Z = 4, C14H18N5O13Bi, Mr = 673.31, Dc = 2.204 g/cm3, F(000) = 1296, μ = 8.772 mm-1, the final R = 0.0472 and wR = 0.1441 for 4129 observed reflections (I > 2σ(I)). In 1, the carboxylic groups from DAM- ligands adopt a cheating mode to link bismuth ions to form a 2D sheet network. These sheets are further connected by hydrogen bonding interactions to give an interesting 3D supramolecular framework. 2D correlation analysis of IR of 1 with thermal and magnetic perturbation was introduced to ascertain the characteristic adsorption of the groups overlapped in the 1D IR spectrum. Additionally, compound 1 exhibits fluorescent emission at room temperature. A new compound {[Bi (trans-DAM) (cis-DAM) (H2O)] NO3 · H2O} n1 derived from bismuth and the flexible ligand N, N’-diacetic acid imidazolium chloride (H2DAMCl) was obtained by hydrothermal synthesis Compound 1 crystallizes in the monoclinic P21 / c space group with a = 9.2298 (18), b = 13.339 (3), c = 17.090 ), V = 2028.7 (7) 3, Z = 4, C14H18N5O13Bi, Mr = 673.31, Dc = 2.204 g / cm3, F (000) = 1296, μ = 8.772 mm-1, final R = 0.0472 and wR = 0.1441 for 4129 observed reflections (I> 2σ (I)). In 1, the carboxylic groups from DAM-ligands adopt a cheating mode to link bismuth ions to form a 2D sheet network. These sheets are further connected by hydrogen bonding interactions to give an interesting 3D supramolecular framework. 2D correlation analysis of IR of 1 with thermal and magnetic perturbation was introduced to ascertain the characteristic adsorption of the groups overlapped in the 1D IR spectrum. Additionally, comp ound 1 exhibited fluorescent emission at room temperature.