The solid‐state conversion of a 3D lead(II) coordination polymer, [Pb(1,4‐BDC)(H2O)]n (1) microstructures (1,4‐H2BDC = 1,4‐benzenedicarboxylic acid) with PbO7 coordination sphere, was synthesized by a sonochemical process to a 3D [Pb(1,4‐BDC)]n (2) coordination polymer with nanoparticle morphology and the same coordination environment was observed upon thermal treatment and dehydration. The color of this compound did not change during the process. This process is irreversible and compound 2 cannot absorb water again. Adsorption and desorption of water in these lead(II) coordination polymers were studied by IR spectroscopy, thermo gravimetric and differential thermal analyses (TG‐DTA), X‐ray powder diffraction (XRD), and scanning electron microscopy (SEM).

A new potassium-based coordination polymer [K (μ 7 -HTar)] n (1), (H 2 Tar = (+)tartaric acid), has been synthesized and structurally characterized by single crystal X-ray crystallography. It has a three-dimensional structure with zigzag K···K metallophilic interactions. Also widespread hydrogen bonding network in three-dimensional structure of 1 was observed. In order to evaluation the effects of concentration, ultrasonic irradiation and type of the solvents on morphology and thermal behavior of 1, some experiments were designed and six samples of 1 were synthesized under different conditions. These samples were characterized by IR spectroscopy, thermo gravimetric and differential thermal analyses (TG-DTA), X-ray powder diffraction (XRD) and Scanning Electron Microscopy (SEM).

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