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Syntheses of the B(8)-hydroxy- and B((8),(8)')-dihydroxy-derivatives of the bis(1,2-dicarbollido)-3-cobalt(1-)ate ion by its reductive acetoxylation and hydroxylation: molecular structure of [8,8'-mu-CH3C(O) (2) (1,2-C2B9H10) (2) -3-Co] (0) zwitterion determined by X-ray diffraction analysis
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SYSNO ASEP 0163326 Document Type J - Journal Article R&D Document Type Journal Article Subsidiary J Ostatní články Title Syntheses of the B(8)-hydroxy- and B((8),(8)')-dihydroxy-derivatives of the bis(1,2-dicarbollido)-3-cobalt(1-)ate ion by its reductive acetoxylation and hydroxylation: molecular structure of [8,8'-mu-CH3C(O) (2) (1,2-C2B9H10) (2) -3-Co] (0) zwitterion determined by X-ray diffraction analysis Author(s) Plešek, Jaromír (UACH-T)
Grüner, Bohumír (UACH-T) RID, SAI, ORCID
Báča, Jiří (UACH-T)
Fusek, Jiří (UACH-T)
Císařová, I. (CZ)Source Title Journal of Organometallic Chemistry. - : Elsevier - ISSN 0022-328X
Roč. 649, č. 2 (2002), s. 181-190Number of pages 10 s. Language eng - English Country GB - United Kingdom Keywords bis(1,2-dicarbollido)-3-cobalt(1-)ate ion ; carbaboranes ; metallacarboranes Subject RIV CA - Inorganic Chemistry R&D Projects GA104/99/1096 GA ČR - Czech Science Foundation (CSF) GA203/99/M037 GA ČR - Czech Science Foundation (CSF) CEZ AV0Z4032918 - UACH-T Annotation Preparative routes to 8-hydroxy-bis(1,2-dicarbollido)-3-cobalt(1-)ate (2) and 8,8-dihydroxy-bis(1,2-dicarbollido)-3-cobalt(1-)ate (3) ions are reported by the reductive acetoxylation of the parent bis(dicarbollido)cobaltate ion (1) followed by hydrolysis of the intermediates. The essential reagent is acetic anhydride, and strong acids are required as catalysts. For the hydroxyderivative ion 2 the simultaneous presence of acetic acid brings benefit, whereas it is detrimental for the formation of the dihydroxyderivative 3. Reaction intermediate leading to the dihydroxy derivative is the already reported [8,8'-mu-CH3C (O) (2) (1,2-C2B9H10) (2)-3-Co] (0) zwitterion. This compound was adequately characterised for the first time and its molecular structure as determined by X-ray diffraction analysis is presented. Both B-hydroxylated bis(dicarbollido)-ions can be alternatively obtained on the direct hydroxylation of the parent ion by hot 60-80 sulphuric acid. Optimised synthetic procedures and the main physicochemical properties (MS, TLC, HPLC, 1H- and 11B-NMR) of the species are presented. The probable reaction course of the reductive acetoxylation is discussed. Workplace Institute of Inorganic Chemistry Contact Jana Kroneislová, krone@iic.cas.cz, Tel.: 311 236 931 Year of Publishing 2003
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