Serendipitous discovery of (L)‐valine mediated in situ formation of two‐dimensional coordination polymer by tripodal ligand with transition metals

A new methodology for 2D coordination polymer formation has been reported by in situ amide bond cleavage of the ligand L at room temperature under a mild condition in the presence of aqueous pyridine. The ligand is formed by the coupling of (L)‐valine with benzene‐1,3,5‐tricarboxylic acid (btcH3). The three amide bonds present on the tripodal ligand, easily break and forms 2D coordination polymer with btc−3 as {[(btc)(py)3(H2O)(Co)1.5].(py)(H2O)2}n (1), {(btc)0.66(py)3(H2O)Ni}n (2), and {[(btc)(py)3Zn1.5](H2O)2}n (3). The tripodal ligand L has been characterized by 1H NMR, 13C NMR, IR, and mass spectra and their corresponding coordination polymers 1, 2, and 3, respectively, have been characterized by single‐crystal X‐ray diffraction and thermogravimetric analysis. The topology of pore and cavities, formed by stacking the consecutive layer of 2D coordination polymer depends upon the synthetic approach.