Synthesis and Characterization of Neutral and Cationic Layered Materials Based on Heavier Group 14 Metals: BING-5, -6, -
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Synthesis and Characterization of Neutral and Cationic Layered Materials Based on Heavier Group 14 Metals: BING-5, -6, -9, -10 Dat T. Tran, Peter Y. Zavalij and Scott R. J. Oliver Department of Chemistry, State University of New York at Binghamton, Binghamton, NY 13902-6016, U.S.A.
ABSTRACT Our research involves the solvothermal synthesis and characterization of new 3D open-framework and low dimensional inorganic materials. We focus on heavier group 14 elements to prepare structures that are analogous to aluminosilicate zeolites, but the main emphasis is to obtain cationic materials, a feat not possible with silicon oxides. We have successfully synthesized a series of novel compounds with Pb as building block: a cationic layered lead fluoride material (BING-5, Pb3F5NO3); a neutral, layered lead phenylphosphonate pyridine (BING-6); and a layered lead metamethylphenylphosphonate (BING-9). A molecular solid, tetrafluorodipyridine-germanium (BING-10) was also obtained. These structures are characterized by a variety of solid state techniques, including: powder X-Ray diffraction (PXRD), thermogravimetric analysis (TGA), UV-Vis spectroscopy and NMR. Our BING-5 material can exchange its interlayer NO3− for a variety of other anions. It is also stable to 450°C, which is far superior to organic resins that are still the standard for anion-exchange.
INTRODUCTION Layered metal phosphonate materials have stimulated much research activity in the past decade. Clearfield and co-workers, for example, reported the synthesis of a neutral layered lead hydrogen-phenylphosphonate, Pb(HO3PC6H5)2 [1]. Also, Cabeza and coworkers reported a new lead(II) phenylphosphonate, Pb(O3PC6H5), in which its crystal structure was solved from powder X-ray diffraction data [2]. Many Ge-based structures have also recently been described. Cascales and co-workers reported a new anionic layered germanate Ge5O11H(C6N2H13), using dabconium cations (DABCO = 1,4diazabicyclo-[2,2,2]-octane) as a bulky structure-directing agent [3]. The material shows catalytic activity in Michael reactions. Our research is currently focused on the solvothermal synthesis of new layered and open-framework materials based on heavier group 14 elements. Thus far, we have used both cationic and anionic structure-directing agents (SDAs) for the formation of anionic, cationic and neutral germanium- [4], tin- [5-8] and lead-based compounds [9,10]. Our particular interest in these materials stems from their potential to yield chemically and thermally stable microporous zeotype materials. Zeotypes have materials properties for such potential applications as ion-exchange, chemical separation and catalysis. These new materials we denote as BING-n, where BING denotes State University of New York (SUNY) at Binghamton, and n denotes structure type. Our primary target is to prepare
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cationic layered materials or open-frameworks. We are also interested in these materials for their possible semiconducting and therefore chemoselective sensing properties.
EXPERIMENTAL DETAILS B
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