Tubular polyoxoanion [(SeMoO)(CO)] and its transformations
Self-assembly reactions in the Na 2 MoO 4 /SeO 2 /H 2 C 2 O 4 system lead to the formation of a tubular [(SeMo 6 O 21 ) 2 (C 2 O 4 ) 3 ] 10− hybrid polyanion, isolated and characterized by single crystal X-ray diffraction (SCXRD) as Na 9 H[(SeMo 6 O 21 ) 2 (C 2 O 4 ) 3 ]·NaNO 3 ·20.6H 2 O ( SeMo6-1...
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| Published in | New journal of chemistry Vol. 45; no. 15; pp. 6745 - 6752 |
|---|---|
| Main Authors | , , , , , , , |
| Format | Journal Article |
| Published |
21.04.2021
|
| Online Access | Get full text |
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| Summary: | Self-assembly reactions in the Na
2
MoO
4
/SeO
2
/H
2
C
2
O
4
system lead to the formation of a tubular [(SeMo
6
O
21
)
2
(C
2
O
4
)
3
]
10−
hybrid polyanion, isolated and characterized by single crystal X-ray diffraction (SCXRD) as Na
9
H[(SeMo
6
O
21
)
2
(C
2
O
4
)
3
]·NaNO
3
·20.6H
2
O (
SeMo6-1
). Dehydration of this compound leads to the formation of Na
10
[(SeMo
6
O
21
)
2
(C
2
O
4
)
3
]·0.5NaNO
3
·8H
2
O (
SeMo6-2
). The electrochemical behavior of
SeMo6-2
as a component of the paste electrode was studied by CV in CH
3
CN solution. A concentrated aqueous solution of
SeMo6-2
was studied using
77
Se and
95
Mo NMR techniques, which show extensive degradation of the complex. Addition of TBABr to the concentrated solution leads to a precipitate consisting of TBA salts of [Mo
6
O
19
]
2−
and [β-Mo
8
O
26
Na
2
(NO
3
)
2
]
2−
anions. The latter was characterized by SCXRD as (TBA)
3
[β-Mo
8
O
26
Na
2
(NO
3
)]·CH
3
CN (
Mo8-Na
). This transformation shows the presence of [β-Mo
8
O
26
]
4−
and [Mo
6
O
19
]
2−
in the aqueous solution of
SeMo6-2
. The study of (NBu
4
)
4
[β-Mo
8
O
26
] and (NBu
4
)
2
[Mo
6
O
19
] solutions in CH
3
CN by HPLC shows equilibration between [β-Mo
8
O
26
]
4−
and [Mo
6
O
19
]
2−
.
Tubular [(SeMo
6
O
21
)
2
(C
2
O
4
)
3
]
10−
polyoxoanion can be assembled from Na
2
MoO
4
/SeO
2
/H
2
C
2
O
4
system. TBABr precipitates complexes of [Mo
6
O
19
]
2−
and [β-Mo
8
O
26
Na
2
(NO
3
)]
3−
from its aqueous solution. Speciation of [β-Mo
8
O
26
]
4−
and [Mo
6
O
19
]
2−
has been studied. |
|---|---|
| Bibliography: | 2056268-2056270 For ESI and crystallographic data in CIF or other electronic format see DOI 10.1039/d1nj00421b Electronic supplementary information (ESI) available: Crystal packing. CCDC |
| ISSN: | 1144-0546 1369-9261 |
| DOI: | 10.1039/d1nj00421b |