NEW JOURNAL OF CHEMISTRY, vol.38, no.7, pp.3187-3192, 2014 (SCI-Expanded)
Reversible anion-exchange of nonporous 3D lead(m) coordination polymers with ligand 2,5-bis(4-pyridyl)-3,4diaza-2,4-hexadiene (4-bpdh), from [Pb(4-bpdh)(mu.-NCS)(2)](n)-, (1) to intermediate 3D [Pb(4-bpdh)(mu-NCS)(NO3)](n),-, (2) and then porous 3D coordination polymers of [Pb(4-bpdh)(NO3)(2)(H2O)](n), (3) and [Pb(4-bpdh)(NO3)(2)](n), (4) by solid state anion-replacement processes under mechanochemical reactions, have been studied. The reversible solid state structural transformations of compound 1 to compound 2 and then 3 and 4 by anion-replacement have been verified by PXRD and IR spectroscopy. Pb5O4SO4, Pb-2(SO4)O and PbO nanoparticles were obtained by thermal decomposition of compounds 1, 2 and 3, 4 at 600 degrees C under an air atmosphere, respectively. These nanoparticles were characterized by powder X-ray diffraction (PXRD) and scanning electron microscopy (SEM).