SCHEDULED MAINTENANCE
Use of Se4N4 and Se(NSO)2 in the preparation of palladium adducts of diselenium dinitride, Se2N2; crystal structure of [PPh4]2[Pd2Br6(Se2 N2)]
Abstract
Reaction of Se
4
N
4
with
[NBu
n
4
]
2
[Pd
2
Br
6
]
at 100 °C in CH
2
Cl
2
resulted in
[NBu
n
4
]
2
[Pd
2
Br
6
(Se
2
N
2
)] 1a in high yield (67%). In
contrast to the reaction of
[PPh
4
]
2
[Pd
2
Br
6
] with
S
4
N
4
, which generates a number of products, the
tetrabutylammonium salt generated only
[NBu
n
4
]
2
[Pd
2
Br
6
(S
2
N
2
)] 1b; comparison of the IR spectra
of 1a and 1b allows unambiguous identification of the
two bands due to E
2
N
2
vibrations. While reaction
of S(NSO)
2
with [Pt(PPh
3
)
3
] leads to a
mixture of [Pt(S
2
N
2
)(PPh
3
)
2
]
and [Pt(NSO)
2
(PPh
3
)
2
], only the latter
species forms in the analogous reaction of Se(NSO)
2
. Two
different results were also found in reactions with
[PPh
4
]
2
[Pd
2
Br
6
]; while
S(NSO)
2
appears surprisingly inert to this reagent,
Se(NSO)
2
reacts, when present in excess, to give the
unexpected product
[PPh
4
]
2
[Pd
2
Br
6
(Se
2
N
2
)] 1c. The crystal structure of the latter
confirms the presence of the adducted diselenium dinitride unit.
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