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Regioselective synthesis and characterization of monovanadium‐substituted β‐octamolybdate [VMo 7 O 26 ] 5−
Author(s) -
Krivosudský Lukáš,
Roller Alexander,
Rompel Annette
Publication year - 2019
Publication title -
acta crystallographica section c
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.304
H-Index - 17
ISSN - 2053-2296
DOI - 10.1107/s205322961900620x
Subject(s) - polyoxometalate , chemistry , crystallography , cluster (spacecraft) , ion , hydrogen peroxide , dissolution , selectivity , catalysis , organic chemistry , computer science , programming language
The monovanadium‐substituted polyoxometalate anion [VMo 7 O 26 ] 5− , exhibiting a β‐octamolybdate archetype structure, was selectively prepared as pentapotassium [hexaikosaoxido(heptamolybdenumvanadium)]ate hexahydrate, K 5 [VMo 7 O 26 ]·6H 2 O ( VMo 7 ), by oxidation of a reduced vanadomolybdate solution with hydrogen peroxide in a fast one‐pot approach. X‐ray structure analysis revealed that the V atom occupies a single position in the cluster that differs from the other positions by the presence of one doubly‐bonded O atom instead of two terminal oxide ligands in all other positions. The composition and structure of VMo 7 was also confirmed by elemental analyses and IR spectroscopy. The selectivity of the synthesis was inspected by a 51 V NMR investigation which showed that this species bound about 95% of V V in the crystallization solution. Upon dissolution of VMo 7 in aqueous solution, the [VMo 7 O 26 ] 5− anion is substantially decomposed, mostly into [VMo 5 O 19 ] 3− , α‐[VMo 7 O 26 ] 4− and [V 2 Mo 4 O 19 ] 4− , depending on the pH.