Synthesis and Characterization of [(OH)TeNb5O18](6-) in Water Solution, Comparison with [Nb6O19](8-)
| Autor: | Pavel A. Abramov, Tatiana P. Zemerova, Artem A. Zhdanov, Nikolay B. Kompankov, Cristian Vicent, Maxim N. Sokolov, Alfiya R. Tsygankova, Nikolay K. Moroz |
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| Rok vydání: | 2016 |
| Předmět: |
Single product
010405 organic chemistry Chemistry Electrospray ionization Analytical chemistry Crystal structure 010402 general chemistry 01 natural sciences 0104 chemical sciences Inorganic Chemistry chemistry.chemical_compound Capillary electrophoresis BORATE BUFFER Polyoxometalate Physical chemistry Redistribution (chemistry) Methanol Physical and Theoretical Chemistry |
| Zdroj: | Inorganic chemistry. 55(4) |
| ISSN: | 1520-510X |
| Popis: | Reaction of [Nb6O19](8-) with H6TeO6 in water gives telluropentaniobate [(OH)TeNb5O18](6-) (1) as single product, which was isolated as Na(+) and mixed Na(+)/K(+) salts. Crystal structures were determined for Na6[(OH)TeNb5O18]·15H2O (Na6-1) and K6Na[Nb(5.5){Te(OH)}(0.5)O(18.5)]·26H2O (K6Na-1). Formation of 1 was monitored with electrospray ionization mass spectrometry (ESI-MS) and (125)Te NMR techniques. Capillary electrophoresis was used to calculate electrophoretic mobilities and radii of the anionic species in solutions of [(OH)TeNb5O18](6-) and [Nb6O19](8-) in borate buffer. No condensation or degradation products were detected. Reactions of 1 with {Cp*Rh}(2+) sources gives 1:1 and 2:1 hybrid polyoxometalate, which are present in solution as a mixture of isomers, as detected by (125)Te NMR. The isomerism is related to various possibilities of coordination of {Cp*Rh}(2+) to different {M3O3} faces, relative to the unique Te atom. According to ESI-MS experiments in water and methanol, rapid redistribution of the organometallic fragments between the 1:1 and 2:1 complexes takes place. The 1:1 complexes are more stable in water, while 2:1 complexes dominate in methanol. X-ray structural analysis of the crystals isolated from 2:1 reaction mixture allowed identification of Na3[{Cp*Rh}2TeNb5O19]·24H2O (Cp*2Rh2-1) with two {Cp*Rh}(2+) fragments capping the opposing faces of the Lindqvist anion. |
| Databáze: | OpenAIRE |
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