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An 17O NMR Study of Hydrolyzed Nb(V) in Weakly Acidic and Basic Aqueous Solution.


ABSTRACT: Time-dependent 17O NMR spectra of basified decaniobate (Nb10O286-) solutions displayed intense resonances assigned to the well-known protonated hexaniobate anion (Nb6O198-) and two other species identified as heptaniobate (Nb7O229-) and protonated tetracosaniobate (Nb24O7224-) anions. The decaniobate ion showed no sign of protonation from pH 6 - 10, in contrast with the hexaniobate ion which was protonated at doubly-bridging oxygen sites at pH 10-13. Most (> 90%) of the heptaniobate formed 1 h after basification was transformed into other species after 3 weeks. Tetracosaniobate was formed reversibly from decaniobate, but only when KOH, NaOH and [(CH3)4N]OH were employed; none was observed after basification with [(n-C4H9)4N]OH. Moreover, far more tetracosaniobate was formed from KOH than from [(CH3)4N]OH. This effect was attributed to a tetracosaniobate cation binding site that binds K+ more readily than (CH3)4N+ but is too small to accommodate (n-C4H9)4N+.

SUBMITTER: Klemperer WG 

PROVIDER: S-EPMC3622484 | biostudies-literature | 2013 Apr

REPOSITORIES: biostudies-literature

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An <sup>17</sup>O NMR Study of Hydrolyzed Nb(V) in Weakly Acidic and Basic Aqueous Solution.

Klemperer Walter G WG   Marek Keith A KA  

European journal of inorganic chemistry 20130401 10-11


Time-dependent <sup>17</sup>O NMR spectra of basified decaniobate (Nb<sub>10</sub>O<sub>28</sub><sup>6-</sup>) solutions displayed intense resonances assigned to the well-known protonated hexaniobate anion (Nb<sub>6</sub>O<sub>19</sub><sup>8-</sup>) and two other species identified as heptaniobate (Nb<sub>7</sub>O<sub>22</sub><sup>9-</sup>) and protonated tetracosaniobate (Nb<sub>24</sub>O<sub>72</sub><sup>24-</sup>) anions. The decaniobate ion showed no sign of protonation from pH 6 - 10, in co  ...[more]

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