4.6 Article

Crystal structures and evaluated of structural transformations of three novel Lead(II) halide/pseudohalide coordination polymers: Effect of sonochemical synthesis conditions on morphology and particle size

Journal

JOURNAL OF SOLID STATE CHEMISTRY
Volume 302, Issue -, Pages -

Publisher

ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.jssc.2021.122390

Keywords

Supramolecular network; Ultrasonic technique; Crystal-to-crystal transformations; Mechanochemical method

Funding

  1. Tarbiat Modares University

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A thermal gradient method was used to synthesize three novel lead mixed-ligand coordination polymers, which were structurally characterized by single crystal X-ray diffraction and their thermal behavior was identified by thermogravimetric analysis. Compounds 2 and 3 were also prepared by an ultrasonic process and characterized by IR spectroscopy, powder X-ray diffraction, and scanning electron microscopy. The particle size and morphology of compounds 2 and 3 were examined by changing the initial concentration of reagents, time, and ultrasonic power.
A thermal gradient method (branched tube) was applied to synthesize three novel lead (II) mixed-ligand coordination polymers, [Pb(NNO) (HNNO) (I-3)](n) (1), [Pb(NNO) (SCN)](n) (2) and [Pb(PNO) (I)](n) (3), (HPNO = picolinic acid N-oxide and HNNO = nicotinic acid N-oxide) which were structurally characterized by single crystal X-ray diffraction. The thermal behavior of 1, 2 and 3 was identified by thermogravimetric analysis. Compounds 2 and 3 were also prepared by an ultrasonic process and their characterizations were carried out by IR spectroscopy, powder X-ray diffraction and scanning electron microscopy. Mechanochemical transformations of compounds 3 and [Pb(PNO) (SCN)] (4) were investigated by replacement of their anions. The particle size and morphology of compounds 2 and 3 were examined by changing the initial concentration of reagents, time and ultrasonic power.

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