Synthesis and stability studies of derivatives of the 2-sulfanyl-closo-decaborate anion [2-B^sub 10^H^sub 9^SH]^sup 2-

Synthesis and stability studies of derivatives of the 2-sulfanyl-closo-decaborate anion [2-B^sub 10^H^sub 9^SH]^sup 2-

By acylation of [2-B10H9SH]2− (1) with trifluoroacetic anhydride was synthesized the anion [B10H9SCOCF3]2− (2). The alkaline and acid hydrolysis of the [B10H9S(CH2COOEt)2]− anion leading to the formation of [B10H9S(CH2COOH)2]− (3) gave evidence of high stability of sulfonium derivatives. While in ph...

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Bibliographic Details
Published in:Inorganica Chimica Acta Vol. 477; p. 277
Main Authors: Kubasov, AS, Matveev, EYu, Turyshev, ES, Polyakova, IN, Nichugovskiy, AI, Zhizhin, K Yu, Kuznetsov, NT
Format: Journal Article
Language:English
Published: Amsterdam Elsevier Science Ltd 24-05-2018
Subjects:
Acylation
Anhydrides
Anions
Bonding strength
Boron
Cesium
Chemical elements
Chemical synthesis
Crystal structure
Derivatives
Hydrogen bonds
Hydrolysis
Infrared radiation
Infrared spectroscopy
NMR
Nuclear magnetic resonance
Stability
Thioesters
X-ray diffraction
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Summary:By acylation of [2-B10H9SH]2− (1) with trifluoroacetic anhydride was synthesized the anion [B10H9SCOCF3]2− (2). The alkaline and acid hydrolysis of the [B10H9S(CH2COOEt)2]− anion leading to the formation of [B10H9S(CH2COOH)2]− (3) gave evidence of high stability of sulfonium derivatives. While in phosphate buffer at pH = 5 the semi-hydrolysis time of thioesters [B10H9SCOCH3]2−, [B10H9SCOCF3]2− (2), and [B10H9SCOC6H5]2− were 600, 17 and 168 h. The substituted closo-decaborates were characterized by IR and NMR (1H, 11B, 13C) spectroscopy. The crystal structures of (Bu4N)3[B10H9(CH2COO)2H]2 (3) and Cs5(Bu4N)[B10H9SC(O)CF3]3 (2a) were determined by X-ray diffraction. In structure 3, anions were associated via strong O-H...O hydrogen bonds into centrosymmetric hexacharged tetramers. In structure 2a, anions formed the environment of all cesium cations and chelated one of them due to Cs-O and Cs-HB bonds.
ISSN:0020-1693
1873-3255