Research output: Contribution to journal › Article › peer-review
Synthesis, Stability, and Crystal Structure of the (NMe2H2)9 [(AsW9O33)2 (NbO)3 (H2 O)]·44H2O Complex. / Shmakova, A. A.; Abramov, P. A.; Sokolov, M. N.
In: Journal of Structural Chemistry, Vol. 60, No. 4, 01.04.2019, p. 623-629.Research output: Contribution to journal › Article › peer-review
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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 -
ID: 20165073