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A HPLC-ICP-AES technique for the screening of [XW11NbO40]n− aqueous solutionsElectronic supplementary information (ESI) available: HPLC-ICP-AES, XRD, XRPD details. CCDC 1587891 and 1587892. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c7nj04702a
Erscheinungsjahr
2018-05
Quelle
Alma/SFX Local Collection
Beschreibungen/Notizen
The reaction of H
3
[PW
12
O
40
] with (NH
4
)[NbO(C
2
O
4
)
2
(H
2
O)
2
]·3H
2
O leads to the straightforward incorporation of Nb into a Keggin anion backbone resulting in [PW
11
NbO
40
]
4−
in nearly quantitative yield. Solution behavior of this monosubstituted anion as a function of pH was studied through
31
P 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 [PW
11
O
39
]
7−
. In aged solutions of [PW
11
NbO
40
]
4−
the formation of a mixture of [PNb
2
W
10
O
39
]
5−
isomers was detected. The HPLC-ICP-AES technique was applied for the study of [BW
11
O
39
]
9−
behavior in aqueous solutions at different pH values and for monitoring the [GeW
11
O
39
]
4−
reaction with the niobium oxalate complex. Despite the presence of the nucleophilic Nb&z.dbd;O group [PW
11
NbO
40
]
4−
does not coordinate Co
2+
in DMF or Ni
2+
in CH
3
CN, producing double [Co(DMF)
6
][PW
11
NbO
40
]·2.6DMF (
2
) and [Ni(CH
3
CN)
5.5
(H
2
O)
0.5
]
2
[PW
11
NbO
40
]·1.7CH
3
CN (
3
) salts instead.
In this research combined HPLC-ICP-AES technique was used to study formation of mixed [XW
11
O
40
]
n
−
(X = P, Ge, B) complexes.
Sprache
Englisch
Identifikatoren
ISSN: 1144-0546
eISSN: 1369-9261
DOI: 10.1039/c7nj04702a
Titel-ID: cdi_rsc_primary_c7nj04702a
Format
–
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