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Niobium uptake by a [PWO] macrocyclic polyanion
Reactions of inorganic macrocyclic polytungstate cavitands K 28 Li 5 H 7 [P 8 W 48 O 184 ]·92H 2 O or Li 17 (NH 4 ) 21 H 2 [P 8 W 48 O 184 ]·85H 2 O with (NH 4 )[NbO(C 2 O 4 ) 2 (H 2 O) 2 ]·3H 2 O (Nb-Ox) in aqueous solution lead to incorporation of up to five {NbO(H 2 O)} 3+ units into the {P 8 W 4...
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| Published in: | New journal of chemistry 2019-07, Vol.43 (25), p.9943-9952 |
|---|---|
| Main Authors: | , , , , , , , |
| Format: | Article |
| Language: | English |
| Online Access: | Get full text |
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| Summary: | Reactions of inorganic macrocyclic polytungstate cavitands K
28
Li
5
H
7
[P
8
W
48
O
184
]·92H
2
O or Li
17
(NH
4
)
21
H
2
[P
8
W
48
O
184
]·85H
2
O with (NH
4
)[NbO(C
2
O
4
)
2
(H
2
O)
2
]·3H
2
O (Nb-Ox) in aqueous solution lead to incorporation of up to five {NbO(H
2
O)}
3+
units into the {P
8
W
48
} cavity. The most stable species contain four {NbO(H
2
O)}
3+
units. The uptake of {NbO(H
2
O)}
3+
was determined by corroborative methods including single crystal XRD, inductively coupled plasma atomic emission spectroscopy (ICP-AES),
31
P and
13
C nuclear magnetic resonance (NMR), C-H-N elemental analysis (EA) and thermal gravimetric analysis (TGA). Solution speciation of the Nb-encapsulating macrocycles was studied by HPLC-ICP-AES and small angle X-ray scattering (SAXS).
Incorporation of Nb into the [P
8
W
48
O
184
]
40−
anionic macrocyclic cavitand leads to formation of new Nb-W POMs. Inclusion of up to five {NbO(H
2
O)}
3+
groups was observed. Solution speciation of the Nb-encapsulating macrocycles was studied by HPLC-ICP-AES and SAXS. |
|---|---|
| ISSN: | 1144-0546 1369-9261 |
| DOI: | 10.1039/c9nj01907c |