Orthaber, Andreas ORCID: 0000-0001-5403-9902, Seidel, Christiane, Belaj, Ferdinand, Albering, Joerg H., Pietschnig, Rudolf ORCID: 0000-0003-0551-3633 and Ruschewitz, Uwe ORCID: 0000-0002-6511-6894 (2010). Optimized Synthesis of Tetrafluoroterephthalic Acid: A Versatile Linking Ligand for the Construction of New Coordination Polymers and Metal-Organic Frameworks. Inorg. Chem., 49 (20). S. 9350 - 9358. WASHINGTON: AMER CHEMICAL SOC. ISSN 1520-510X

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Abstract

Pure 2,3,5,6-tetrafluoroterephthalic acid (H(2)tfBDC) is obtained in high yields (95%) by reacting 1,2,4,5-tetrafluorobenzene with a surplus (>2 equiv) of n-butyllithium in tetrahydrofuran (THF) and subsequent carbonation with CO2 without any extensive purification procedure. A single crystal X-ray structure analysis of H2tfBDC (1) confirms former data obtained for a deuterated sample (P (1) over bar, Z = 1). Recrystallization from water/acetone leads to single crystals of H(2)tfBDC center dot 2H(2)O (2, P2(1)/c, Z. 2), where an extensive hydrogen bonding network is found. By reacting H2tfBDC with an aqueous ammonia solution, single crystals of (NH4)(2)tfBDC (3, C2/m, Z. 2) are obtained. 3 is thermally stable up to 250 degrees C and shows an enhanced solubility in water compared to H(2)tfBDC. Monosubstituted 2,3,5,6-tetrafluorobenzoic acid (H(2)tfBC, 4) is obtained by reacting 1,2,4,5-tetrafluorobenzene with stoichiometric amounts (1 equiv) of n-butyllithium in THF. Its crystal structure (Fdd2, Z = 16) shows dimeric units as characteristic structural feature.

Item Type: Journal Article
Creators:
CreatorsEmailORCIDORCID Put Code
Orthaber, AndreasUNSPECIFIEDorcid.org/0000-0001-5403-9902UNSPECIFIED
Seidel, ChristianeUNSPECIFIEDUNSPECIFIEDUNSPECIFIED
Belaj, FerdinandUNSPECIFIEDUNSPECIFIEDUNSPECIFIED
Albering, Joerg H.UNSPECIFIEDUNSPECIFIEDUNSPECIFIED
Pietschnig, RudolfUNSPECIFIEDorcid.org/0000-0003-0551-3633UNSPECIFIED
Ruschewitz, UweUNSPECIFIEDorcid.org/0000-0002-6511-6894UNSPECIFIED
URN: urn:nbn:de:hbz:38-494187
DOI: 10.1021/ic1009829
Journal or Publication Title: Inorg. Chem.
Volume: 49
Number: 20
Page Range: S. 9350 - 9358
Date: 2010
Publisher: AMER CHEMICAL SOC
Place of Publication: WASHINGTON
ISSN: 1520-510X
Language: English
Faculty: Unspecified
Divisions: Unspecified
Subjects: no entry
Uncontrolled Keywords:
KeywordsLanguage
CRYSTAL-STRUCTURE; INDUSTRIAL APPLICATIONS; HYDROGEN STORAGE; DESIGN; TEMPERATURE; DIFFRACTION; REFINEMENT; ADSORPTIONMultiple languages
Chemistry, Inorganic & NuclearMultiple languages
URI: http://kups.ub.uni-koeln.de/id/eprint/49418

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