Synthesis of phosphinochalcogenoic amidato complexes of divalent
transition metals and their thermolysis to metal selenide and telluride
phases
Abstract
Protolysis of the transition-metal diamides
[M{N(SiMe
3
)
2
}
2
(thf)
n
] (M = Cr, Mn, Fe or Co) with 2
equivalents of phosphinochalcogenoic amides
Bu
t
2
P(E)NHR (E = Se or Te,
R = Pr
i
or cyclo-C
6
H
11
)
gave a series of thermally stable metal–selenium and
–tellurium complexes
[M{Bu
t
2
P(E)NR}
2
]. The complex
[Ni{Bu
t
2
P(Se)NR}
2
] was
obtained from Li[Bu
t
2
(Se)NR] and
[NiCl
2
(PMe
3
)
2
]. The compounds sublime
readily under reduced pressure and are suitable for the gas-phase
deposition of metal chalcogenide films. The selenium precursors lead to
MSe (M = Cr, Mn, Fe or Ni), while tellurium complexes
afford MTe
2
(M = Fe, Mn or Co). By contrast,
[Co{Bu
t
2
P(Se)NR}
2
] gives
Co
3
Se
4
, while
[Ni{Bu
t
2
P(Se)NR}
2
] generates
NiSe or Ni
6
Se
5
, depending on the deposition
conditions.
)
n
] (M = Cr, Mn, Fe or Co) with 2
equivalents of phosphinochalcogenoic amides
Bu
t
2
P(E)NHR (E = Se or Te,
R = Pr
i
or cyclo-C
6
H
11
)
gave a series of thermally stable metal–selenium and
–tellurium complexes
[M{Bu
t
2
P(E)NR}
2
]. The complex
[Ni{Bu
t
2
P(Se)NR}
2
] was
obtained from Li[Bu
t
2
(Se)NR] and
[NiCl
2
(PMe
3
)
2
]. The compounds sublime
readily under reduced pressure and are suitable for the gas-phase
deposition of metal chalcogenide films. The selenium precursors lead to
MSe (M = Cr, Mn, Fe or Ni), while tellurium complexes
afford MTe
2
(M = Fe, Mn or Co). By contrast,
[Co{Bu
t
2
P(Se)NR}
2
] gives
Co
3
Se
4
, while
[Ni{Bu
t
2
P(Se)NR}
2
] generates
NiSe or Ni
6
Se
5
, depending on the deposition
conditions.
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