Synthesis, Stability, and Crystal Structure of the (NMe2H2)9 [(AsW9O33)2 (NbO)3 (H2 O)]·44H2O Complex

A. A. Shmakova, P. A. Abramov, M. N. Sokolov

Research output: Contribution to journalArticlepeer-review

1 Citation (Scopus)

Abstract

Citrate complexes of niobium(V) formed in the interaction of [Nb 6 O 19 ] 8− hexaniobate with citric acid are used for transferring the {NbO} 3+ niobium group to the pseudo-trilacunary [α-B-As III W 9 O 33 ] 9− anion with the formation of sandwich-type [(AsW 9 O 33 ) 2 (NbO) 3 (H 2 O)] 9− complexes. Slow evaporation of the reaction mixture in the presence of dimethylammonium chloride yields crystalline product (NMe 2 H 2 ) 9 [(AsW 9 O 33 ) 2 (NbO) 3 (H 2 O)]·44H 2 O (1) whose structure is determined by single crystal XRD. When the (NBu 4 ) + salt (obtained by the exchange reaction between 1 and tetrabutylammonium bromide) of [(AsW 9 O 33 ) 2 (NbO) 3 (H 2 O)] 9− is dissolved in DMF, As 3+ is oxidized to As 5+ with the formation of a mixture of the Keggin-type [AsW 11 NbO 40 ] 4− and [AsW 10 Nb 2 O 40 ] 5− anions. In an aqueous solution 1 is oxidized by hydrogen peroxide with the formation of a mixture of Keggin anions with different numbers of niobium atoms in the structure.

Original languageEnglish
Pages (from-to)623-629
Number of pages7
JournalJournal of Structural Chemistry
Volume60
Issue number4
DOIs
Publication statusPublished - 1 Apr 2019

Keywords

  • arsenic
  • crystal structure
  • niobium
  • polyoxometalate
  • OXIDATION
  • CATALYSIS
  • NB
  • HETEROPOLYANIONS
  • POLYOXOANIONS
  • DERIVATIVES

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