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Triorganotin(iv) cation-promoted dimethyl carbonate synthesis from CO2 and methanol: solution and solid-state characterization of an unexpected diorganotin(iv)-oxo clusterElectronic supplementary information (ESI) available: Supplementary data containing general NMR numbering of substituents, selected NMR spectra, molecular structure of 6 as well as selected crystallographic data of 4a, 6 and 7 may be found. CCDC 1590298, 1590299 and 1590300 numbers for compounds 6, 7 and 4a contain the suppleme
Two novel C , N -chelated organotin( iv ) complexes bearing weakly coordinating carborane moieties were prepared by the reaction of the corresponding C , N -chelated organotin( iv ) chloride ( i.e. L CN R 2 SnCl, R = n -Bu ( 1 ) and Ph ( 2 ); L CN = 2-( N , N -dimethylaminomethyl)phenyl)) with monoc...
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| Main Authors: | , , , , , |
|---|---|
| Format: | Article |
| Language: | English |
| Online Access: | Get full text |
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| Summary: | Two novel
C
,
N
-chelated organotin(
iv
) complexes bearing weakly coordinating carborane moieties were prepared by the reaction of the corresponding
C
,
N
-chelated organotin(
iv
) chloride (
i.e.
L
CN
R
2
SnCl, R =
n
-Bu (
1
) and Ph (
2
); L
CN
= 2-(
N
,
N
-dimethylaminomethyl)phenyl)) with monocarba-
closo
-dodecaborate silver salt (AgCB
11
H
12
; Ag·
3
). Both products of the metathesis, [L
CN
(
n
-Bu)
2
Sn]
+
[CB
11
H
12
]
−
(
4
) and [L
CN
Ph
2
Sn]
+
[CB
11
H
12
]
−
(
5
), respectively, were characterized by both multinuclear NMR spectroscopy and elemental analysis. The instability of
4
and
5
towards water is discussed. The solid-state structure of L
CN
(
n
-Bu)
2
SnOH·B(C
6
F
5
)
3
(
4a
) as a model compound with a Sn-O(H) B linkage is also reported. The evaluation of the catalytic activity of
4
and
5
was carried out within the direct synthesis of dimethyl carbonate (DMC) from methanol and CO
2
. While
5
was shown to be definitively inactive, presumably due to cleavage of the Sn-Ph bond, compound
4
exhibits a beneficial action, since it leads to an amount of DMC higher than the stoichiometry (
n
DMC
/
n
Sn(cat)
= 1.5). In addition, the solid state structures of [BnNMe
3
]
+
[CB
11
H
12
]
−
(
6
) and [(
n
-Bu)
20
Sn
10
O
2
(OMe)
6
(CO
3
)
2
]
2+
·
2
[CB
11
H
12
]
−
(
7
), isolated as single-crystals and resulting from the recombination of
4
under the reaction conditions (methanol/CO
2
), were established by sc-XRD analyses within the term of this work as well.
6
and
7
were also fully characterized by IR spectroscopy, multinuclear NMR in solution and elemental analysis.
Novel
C
,
N
-chelated organotin(
iv
) complexes bearing weakly coordinating carborane moieties were prepared and used as a catalyst precursor for the direct synthesis of dimethyl carbonate (DMC) from CO
2
and methanol. |
|---|---|
| ISSN: | 1144-0546 1369-9261 |
| DOI: | 10.1039/c7nj05058e |