TY - JOUR

T1 - Synthesis, Stability, and Crystal Structure of the (NMe2H2)9 [(AsW9O33)2 (NbO)3 (H2 O)]·44H2O Complex

AU - Shmakova, A. A.

AU - Abramov, P. A.

AU - Sokolov, M. N.

PY - 2019/4/1

Y1 - 2019/4/1

N2 - 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.

AB - 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.

KW - arsenic

KW - crystal structure

KW - niobium

KW - polyoxometalate

KW - OXIDATION

KW - CATALYSIS

KW - NB

KW - HETEROPOLYANIONS

KW - POLYOXOANIONS

KW - DERIVATIVES

UR - http://www.scopus.com/inward/record.url?scp=85065419173&partnerID=8YFLogxK

U2 - 10.1134/S0022476619040139

DO - 10.1134/S0022476619040139

M3 - Article

AN - SCOPUS:85065419173

VL - 60

SP - 623

EP - 629

JO - Journal of Structural Chemistry

JF - Journal of Structural Chemistry

SN - 0022-4766

IS - 4

ER -