Abstract: | A new thallium‐based supramolecular polymer [Tl(μ3–3‐HClb)(μ3–3‐Clb)]n ( 1 ), (3‐HClb = 3‐chloroperbenzoic acid), has been synthesized and structurally characterized by single crystal X‐ray crystallography. It has a two‐dimensional structure with linear thallophilic and covalent hydrogen‐bonding interactions. In order to evaluate the effects of concentration, ultrasonic irradiation and type of solvents on structure, morphology and thermal behavior of 1 , some experiments were designed, and eight samples of 1 were synthesized under different conditions. These samples were characterized by IR spectroscopy, thermogravimetric and differential thermal analyses, X‐ray powder diffraction and scanning electron microscopy. |