부산대학교 도서관

The preparation of five different compounds, [La2(H2pmd)3(H2O)12] (1: 1D), [La2(H2pmd)(pmd)(H2O)2] (2: 3D), [La(H3pmd)(H2pmd)(H2O)] (3: 3D), [La2(H2pmd)3(H2O)2] (4: 3D), and [La2(H2pmd)(pmd)(H2O)4] (5: 3D), as crystalline materials fromthereaction of 1,4-phenylenebis(methylene)diphosphonic acid (H4pmd) with lanthanum chloride is reported. Two different, fast, andeconomically viable synthetic approaches were employed with theirvarious parameters being probed and, when possible, optimized to increaseyields and purity: microwave-assisted synthesis (MWAS, in ca. 1 min)and a benchprocedure using standard ambient conditions(one-pot, ca. 10 min). Compounds 1and 2were isolated as phase-pure crystalline materials. Compounds 3and 4were characterized by single-crystalX-ray diffraction from mixtures, and compound 5was identifiedby powder X-ray diffraction studies (also from a physical mixturewith 2). Structural details for all compounds were investigatedby using in tandem X-ray diffraction (single-crystal and powder),electron microscopy (SEM and EDS), and FT-IR spectroscopy. Topologicalstudies were also performed for all 3D networks. The conversion ofcompound 1(1D) into 3D networks was investigated usinghydrothermal, microwave, and one-pot methods: 1was totallyconverted into phase-pure 2via the hydrothermal methodand one-pot method. [ABSTRACT FROM AUTHOR]