Результаты исследований: Научные публикации в периодических изданиях › статья › Рецензирование
A HPLC-ICP-AES technique for the screening of [XW11NbO40]: N - Aqueous solutions. / Shmakova, Alexandra A.; Akhmetova, Maria M.; Volchek, Victoria V. и др.
в: New Journal of Chemistry, Том 42, № 10, 21.05.2018, стр. 7940-7948.Результаты исследований: Научные публикации в периодических изданиях › статья › Рецензирование
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TY - JOUR
T1 - A HPLC-ICP-AES technique for the screening of [XW11NbO40]: N - Aqueous solutions
AU - Shmakova, Alexandra A.
AU - Akhmetova, Maria M.
AU - Volchek, Victoria V.
AU - Romanova, Tamara E.
AU - Korolkov, Ilya
AU - Sheven, Dmitri G.
AU - Adonin, Sergey A.
AU - Abramov, Pavel A.
AU - Sokolov, Maxim N.
N1 - Publisher Copyright: © 2018 The Royal Society of Chemistry and the Centre National de la Recherche Scientifique.
PY - 2018/5/21
Y1 - 2018/5/21
N2 - The reaction of H3[PW12O40] with (NH4)[NbO(C2O4)2(H2O)2]·3H2O leads to the straightforward incorporation of Nb into a Keggin anion backbone resulting in [PW11NbO40]4- in nearly quantitative yield. Solution behavior of this monosubstituted anion as a function of pH was studied through 31P NMR and HPLC-ICP-AES techniques (a combination of chromatography and ICP-AES). Increasing of the pH leads to the elimination of Nb from the structure with the formation of mixed Nb/W Lindqvist-type anions and monolacunary [PW11O39]7-. In aged solutions of [PW11NbO40]4- the formation of a mixture of [PNb2W10O39]5- isomers was detected. The HPLC-ICP-AES technique was applied for the study of [BW11O39]9- behavior in aqueous solutions at different pH values and for monitoring the [GeW11O39]4- reaction with the niobium oxalate complex. Despite the presence of the nucleophilic NbO group [PW11NbO40]4- does not coordinate Co2+ in DMF or Ni2+ in CH3CN, producing double [Co(DMF)6][PW11NbO40]·2.6DMF (2) and [Ni(CH3CN)5.5(H2O)0.5]2[PW11NbO40]·1.7CH3CN (3) salts instead.
AB - The reaction of H3[PW12O40] with (NH4)[NbO(C2O4)2(H2O)2]·3H2O leads to the straightforward incorporation of Nb into a Keggin anion backbone resulting in [PW11NbO40]4- in nearly quantitative yield. Solution behavior of this monosubstituted anion as a function of pH was studied through 31P NMR and HPLC-ICP-AES techniques (a combination of chromatography and ICP-AES). Increasing of the pH leads to the elimination of Nb from the structure with the formation of mixed Nb/W Lindqvist-type anions and monolacunary [PW11O39]7-. In aged solutions of [PW11NbO40]4- the formation of a mixture of [PNb2W10O39]5- isomers was detected. The HPLC-ICP-AES technique was applied for the study of [BW11O39]9- behavior in aqueous solutions at different pH values and for monitoring the [GeW11O39]4- reaction with the niobium oxalate complex. Despite the presence of the nucleophilic NbO group [PW11NbO40]4- does not coordinate Co2+ in DMF or Ni2+ in CH3CN, producing double [Co(DMF)6][PW11NbO40]·2.6DMF (2) and [Ni(CH3CN)5.5(H2O)0.5]2[PW11NbO40]·1.7CH3CN (3) salts instead.
KW - CAPILLARY-ELECTROPHORESIS
KW - POLYOXOMETALATE CLUSTERS
KW - EMISSION-SPECTROMETRY
KW - LIQUID-CHROMATOGRAPHY
KW - GAMMA-CYCLODEXTRIN
KW - CRYSTAL-STRUCTURES
KW - KEGGIN
KW - NMR
KW - POLYOXOANIONS
KW - COORDINATION
UR - http://www.scopus.com/inward/record.url?scp=85047013152&partnerID=8YFLogxK
U2 - 10.1039/c7nj04702a
DO - 10.1039/c7nj04702a
M3 - Article
AN - SCOPUS:85047013152
VL - 42
SP - 7940
EP - 7948
JO - New Journal of Chemistry
JF - New Journal of Chemistry
SN - 1144-0546
IS - 10
ER -
ID: 13468726