Synthesis and characterization of 2-phosphonoethanesulfonic acid and a barium-hydrogenphosphonatoethanesulfonate - BaH(O{sub 3}P-C{sub 2}H{sub 4}-SO{sub 3})

Journal Article · Sat Mar 15 04:00:00 EDT 2008 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2007.12.003· OSTI ID:21043913

Sonnauer, Andreas ^[1]; Stock, Norbert ^[1]

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1. Institute of Inorganic Chemistry, Christian-Albrechts-University, Otto-Hahn-Platz 6/7, D 24118 Kiel (Germany)

Following the strategy of using polyfunctional phosphonic acids for the synthesis of new metal phosphonates, the organic linker molecule 2-phosphonoethanesulfonic acid, H{sub 2}O{sub 3}P-C{sub 2}H{sub 4}-SO{sub 3}H (1) (H{sub 3}L), was synthesized and characterized in detail. The acid was used in a high-throughput (HT) investigation of the system BaCl{sub 2}/H{sub 3}L/NaOH/H{sub 2}O. The HT experiments comprising 48 individual hydrothermal reactions were performed to systematically investigate the influence of pH of the starting mixture as well as the molar ratio Ba{sup 2+}: H{sub 3}L. Only two reaction products were observed: small amounts of BaCO{sub 3} under basic conditions and BaH(O{sub 3}P-C{sub 2}H{sub 4}-SO{sub 3}) (2). For compounds 1 and 2 the crystal structures were determined from single-crystal X-ray diffraction data (H{sub 2}O{sub 3}P-C{sub 2}H{sub 4}-SO{sub 3}H: trigonal, P3{sub 2}, a=814.58(1), c=861.20(2) pm, Z=3, R1=0.0254, wR{sub 2}=0.0758 for I>2{sigma}(I); BaH(O{sub 3}P-C{sub 2}H{sub 4}-SO{sub 3}): orthorhombic, Ibam, a=953.39(19), b=855.55(17), c=867.82(17) pm, Z=4, R1=0.0162, wR{sub 2}=0.0417 for I>2{sigma}(I)). The structure of H{sub 3}L (1) is stabilized exclusively by strong hydrogen bonds. Compound 2 is built up by chains of edge sharing BaO{sub 8} polyhedra. These chains are connected to a three-dimensional network by the -CH{sub 2}CH{sub 2}- linker of the ligand. Thermogravimetric investigation of compound 2, as well as IR spectra of 1 and 2 are presented. - Graphical abstract: The synthesis of the ligand H{sub 2}O{sub 3}P-C{sub 2}H{sub 4}-SO{sub 3}H and its use in the systematic investigation in the system BaCl{sub 2}/H{sub 2}O{sub 3}P-C{sub 2}H{sub 4}-SO{sub 3}H/NaOH/H{sub 2}O led to the new barium phosphonatosulfonate BaH(O{sub 3}P-C{sub 2}H{sub 4}-SO{sub 3}H)

• OSTI ID: 21043913
• Journal Information: Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Journal Issue: 3 Vol. 181; ISSN 0022-4596; ISSN JSSCBI
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
BARIUM CARBONATES
BARIUM CHLORIDES
BARIUM COMPOUNDS
BARIUM IONS
ETHYLENE
INFRARED SPECTRA
LIGANDS
MONOCRYSTALS
ORTHORHOMBIC LATTICES
PHOSPHONATES
PHOSPHONIC ACIDS
SODIUM HYDROXIDES
SULFONIC ACIDS
SYNTHESIS
THERMAL GRAVIMETRIC ANALYSIS
X-RAY DIFFRACTION