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Organoantimony(iii) compounds containing (imino)aryl ligands of the type 2-(RN&z.dbd;CH)C6H4 (R = 2′,4′,6′-Me3C6H2, 2′,6′-iPr2C6H3): bromides and chalcogenidesElectronic supplementary information (ESI) available: X-ray crystallographic data in CIF format for 4, 5, 6·CHCl3, 7, 9·CH2Cl2, 10 and 11·0.25CH3OH; figures representing the optical isomers as well as the supramolecular architectures in the crystals of these compounds; NMR spectra; representations of calculated vs. determined structures of
The reaction of 2-(RN&z.dbd;CH)C 6 H 4 MgBr [R = 2′,4′,6′-Me 3 C 6 H 2 (R 1 ), 2′,6′- i Pr 2 C 6 H 3 (R 2 )] [prepared from 2-(R 1 N&z.dbd;CH)C 6 H 4 Br ( 1 ) or 2-(R 2 N&z.dbd;CH)C 6 H 4 Br ( 2 ) and Mg] with SbCl 3 in a 2 : 1 and 1 : 1 molar ratio followed by treatment with an aqueous...
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| Main Authors: | , , , , , , |
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| Format: | Article |
| Language: | English |
| Online Access: | Get full text |
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| Summary: | The reaction of 2-(RN&z.dbd;CH)C
6
H
4
MgBr [R = 2′,4′,6′-Me
3
C
6
H
2
(R
1
), 2′,6′-
i
Pr
2
C
6
H
3
(R
2
)] [prepared from 2-(R
1
N&z.dbd;CH)C
6
H
4
Br (
1
) or 2-(R
2
N&z.dbd;CH)C
6
H
4
Br (
2
) and Mg] with SbCl
3
in a 2 : 1 and 1 : 1 molar ratio followed by treatment with an aqueous KBr solution gave [2-(R
1
N&z.dbd;CH)C
6
H
4
]
2
SbBr (
3
) and [2-(R
2
N&z.dbd;CH)C
6
H
4
]
2
SbBr (
4
) as well as [2-(R
1
N&z.dbd;CH)C
6
H
4
]SbBr
2
(
6
) and [2-(R
2
N&z.dbd;CH)C
6
H
4
]SbBr
2
(
7
). Treatment of
4
with Na
2
S·9H
2
O provided the dinuclear [{2-(R
2
N&z.dbd;CH)C
6
H
4
}
2
Sb]
2
S (
5
). Heterocyclic species,
i.e.
the oxide
cyclo
-[{2-(R
2
N&z.dbd;CH)C
6
H
4
}SbO]
3
(
8
) and the sulfides
cyclo
-[{2-(R
1
N&z.dbd;CH)C
6
H
4
}SbS]
2
(
9
) and
cyclo
-[{2-(R
2
N&z.dbd;CH)C
6
H
4
}SbS]
2
(
10
), were obtained by reacting dibromides
6
and
7
with KOH and Na
2
S·9H
2
O, respectively, in a water-toluene solvent mixture. The sulfide
10
reacted with [W(CO)
5
(thf)] to yield the heterometallic complex
cyclo
-[{2-(R
2
N&z.dbd;CH)C
6
H
4
}SbS]
2
[W(CO)
5
] (
11
). The compounds were characterised by multinuclear NMR spectroscopy in solution, mass spectrometry and IR spectroscopy in the solid state. The molecular structures of
4
,
5
,
6
·CHCl
3
,
7
,
9
·CH
2
Cl
2
,
10
and
11
·0.25CH
3
OH were established by single-crystal X-ray diffraction. Theoretical calculations using DFT methods were carried out on bromide
7
and the geometrical isomers of its dimer association as well as the geometrical isomers of sulfide
10
and its monomer.
The title compounds and the complex shown in the joined picture were prepared and characterized. |
|---|---|
| ISSN: | 1477-9226 1477-9234 |
| DOI: | 10.1039/c2dt32494f |