Scorpionates bearing nitro substituents: mono-, bis- and tris-(3-nitro-pyrazol-1-yl)borate ligands and their copper(i) complexesCCDC reference numbers 776890-776893. For crystallographic data in CIF or other electronic format see DOI: 10.1039/c0dt00474j
Two scorpionates sodium trihydro(3-nitro-pyrazol-1-yl)borate (Na[H 3 B(3-(NO 2 )pz)]) and sodium hydrotris(3-nitro-pyrazol-1-yl)borate (Na[HB(3-(NO 2 )pz) 3 ]), featuring electron withdrawing substituents, have been synthesized in high yield starting from 3(5)-nitropyrazole and sodium borohydride. T...
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| Main Authors | , , , , , , |
|---|---|
| Format | Journal Article |
| Language | English |
| Published |
21.09.2010
|
| Online Access | Get full text |
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| Summary: | Two scorpionates sodium trihydro(3-nitro-pyrazol-1-yl)borate (Na[H
3
B(3-(NO
2
)pz)]) and sodium hydrotris(3-nitro-pyrazol-1-yl)borate (Na[HB(3-(NO
2
)pz)
3
]), featuring electron withdrawing substituents, have been synthesized in high yield starting from 3(5)-nitropyrazole and sodium borohydride. The treatment of CuX (X = (CH
3
CN)
4
PF
6
, Cl or I) with Na[H
3
B(3-(NO
2
)pz)], Na[HB(3-(NO
2
)pz)
3
] or the related bis(pyrazolyl)borate Na[H
2
B(3-(NO
2
)pz)
2
] in the presence of triphenylphosphine or
tert
-butyl isocyanide afforded the corresponding (azolyl)borate supported copper(
i
) triphenylphosphine or
tert
-butyl isocyanide adducts. These compounds have been characterized by elemental analyses, FT-IR, ESI-MS and multinuclear NMR spectroscopy. X-Ray crystal structures of [H
3
B(3-(NO
2
)pz)]Cu[P(C
6
H
5
)
3
]
2
, [H
2
B(3-(NO
2
)pz)]Cu(CN
t
-Bu)
2
, and [HB(3-(NO
2
)pz)
3
]Cu[P(C
6
H
5
)
3
], as well as that of the {[HB(3-(NO
2
)pz)
3
]Na}
4
are also reported. The latter displays a particularly interesting tetrameric structure with each tris(pyrazolyl)borate adopting an unusual inverted configuration and serves as a bridging ligand for three different sodium ions.
Weakly coordinating scorpionates based on nitro-pyrazoles have been synthesized. |
|---|---|
| Bibliography: | 776890-776893 For crystallographic data in CIF or other electronic format see DOI CCDC reference numbers 10.1039/c0dt00474j |
| ISSN: | 1477-9226 1477-9234 |
| DOI: | 10.1039/c0dt00474j |