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Title: Synthesis and characterization of four new metal 5-phosphonoisophthalates discovered by high-throughput experimentation

A new ligand, 5-diethylphosphonoisophthalic acid ((HOOC){sub 2}C{sub 6}H{sub 3}-PO{sub 3}(C{sub 2}H{sub 5}){sub 2}, H{sub 2}Et{sub 2}L), for the hydrothermal synthesis of inorganic-organic hybrid compounds was prepared and characterized by NMR-spectroscopy. Its in situ hydrolysis leads to the corresponding 5-phosphonoisophthalic acid ((HOOC){sub 2}C{sub 6}H{sub 3}-PO{sub 3}H{sub 2}, H{sub 4}L). Applying high-throughput methods, different di- and trivalent metal salts for the synthesis of crystalline metal phosphonates based on H{sub 2}Et{sub 2}L have been screened. From the resulting discovery library, single-crystals of four new compounds, [Sm{sub 2}(H{sub 2}O){sub 4}(H(OOC){sub 2}C{sub 6}H{sub 3}-PO{sub 3}){sub 2}].2H{sub 2}O (1), [Cu{sub 3}(H{sub 2}O)(H(OOC){sub 2}C{sub 6}H{sub 3}-PO{sub 3}){sub 2}].2H{sub 2}O (2), Ca{sub 2}(H{sub 2}O)[H(OOC){sub 2}C{sub 6}H{sub 3}-PO{sub 3}H]{sub 2} (3), and Ba{sub 2}(H{sub 2}O){sub 3}(OOC){sub 2}C{sub 6}H{sub 3}-PO{sub 3} (4), have been isolated. The single-crystal structure determination of the title compounds shows H{sub 4}L to be a versatile ligand, exhibiting different types of coordination modes between the functional groups and the metal ions. A comparison of the structural features of the title compounds shows a varying degree of M-O-M connectivities. Thus, isolated metal-oxygen clusters (compounds 1 and 2), infinite M-O-M chains (compound 3), and infinite M-O-M layers (compound 4) are observed. The title compounds 1, 2, and 3more » were further characterized by IR-spectroscopy, TG-, EDX-, and elemental chemical analysis. - Graphical abstract: Applying high-throughput methods, the new ligand 5-diethylphosphonoisophtalic acid, (HOOC){sub 2}C{sub 6}H{sub 3}-PO{sub 3}(C{sub 2}H{sub 5}){sub 2} (H{sub 2}Et{sub 2}L), was reacted with several di- and trivalent metal salts under hydrothermal conditions. Single-crystals of four new inorganic-organic hybrid compounds were isolated from the discovery library. The single-crystal structure analysis shows a varying M-O-M connectivity.« less
Authors:
 [1] ;  [2]
  1. Institute of Inorganic Chemistry, Christian-Albrechts-University, Otto-Hahn-Platz 6/7, D 24098 Kiel (Germany)
  2. Institute of Inorganic Chemistry, Christian-Albrechts-University, Otto-Hahn-Platz 6/7, D 24098 Kiel (Germany), E-mail: stock@ac.uni-kiel.de
Publication Date:
OSTI Identifier:
21043733
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 180; Journal Issue: 11; Other Information: DOI: 10.1016/j.jssc.2007.08.026; PII: S0022-4596(07)00370-2; Copyright (c) 2007 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; BARIUM COMPLEXES; CALCIUM COMPLEXES; CHEMICAL ANALYSIS; COPPER COMPLEXES; CRYSTAL STRUCTURE; HYDROLYSIS; HYDROTHERMAL SYNTHESIS; INFRARED SPECTRA; LAYERS; LIGANDS; MONOCRYSTALS; PHOSPHONATES; PHTHALATES; SAMARIUM COMPLEXES; SPECTROSCOPY; WATER