SCHEDULED MAINTENANCE
Syntheses and crystal structures of bi- and tri-metallic complexes
containing a trioxoosmium(VIII)
moiety
Abstract
Interaction of
cis-[Pt(dppm)
2
(O
3
SCF
3
)
2
] [dppm = bis(diphenylphosphino)methane],
cis-[Pt(Bupy)(O
3
SCF
3
)
2
]
(Bupy = 4-tert-butylpyridine),
[Ir(CO)(PPh
3
)
2
(O
3
SCF
3
)], and
[Rh(cod)(OH
2
)(OTs)] (cod = cycloocta-1,5-diene,
OTs = tosylate) with
[NBu
n
4
][NOsO
3
] afforded bimetallic
nitrido-bridged complexes
cis-[Pt(dppm)(NOsO
3
)
2
] 3,
trans-[Pt(Bupy)
2
(NOsO
3
)
2
] 4,
[Ir(CO)(PPh
3
)
2
(NOsO
3
)] 5 and
[{Rh(cod)(NOsO
3
)}
2
] 6, respectively.
Complex 4 crystallises in the P![[1 with combining macron]](https://www.rsc.org/images/entities/char_0031_0304.gif)
space group with
a = 7.936(1),
b = 10.758(2),
c = 7.738(1) Å,
α = 100.02(1), β = 99.75(1),
γ = 101.75(1)°,
U = 622.5(2) Å
3
for
Z = 1. The Pt–N (Os), Os–N and the
mean Os–O distances are 1.958(7), 1.681(7) and 1.724 Å,
respectively. Complex 5 crystallises in the
P2
1
/n space group with
a = 10.124(1),
b = 15.564(2),
c = 22.623(3) Å,
β = 100.08(2)°,
U = 3509.7(7) Å
3
for
Z = 4. The Ir–N, Os–N and the mean
Os–O distances are 1.998(7), 1.710(7) and 1.718 Å,
respectively. Treatment of [Au(PPh
3
)(NOsO
3
)] 1
with Ph
3
P![[double bond, length as m-dash]](https://www.rsc.org/images/entities/char_e001.gif)
NPh gave the N-phosphinimine
complex
[Au(PPh
3
){N(PPh
3
)Ph}][NOsO
3
] 7. Complex 7 crystallises in the
P2
1
/n space group with
a = 8.780(1),
b = 20.781(2),
c = 20.711(5) Å,
β = 91.23(1)°,
U = 3788.0(9) Å
3
for
Z = 4. The Au–N distance is 2.091(8)
Å and the C–N–P angle in the phosphinimine is
127.0(7)°. Reaction of 1 with Bupy led to substitution of Bupy for
[NOsO
3
] and formation of
[Au(PPh
3
)(Bupy)][NOsO
3
] 8. Reaction of
[Pt(dppf)(O
3
SCF
3
)Cl]
[dppf = 1,1′-bis(diphenylphosphino)ferrocene] with
[NBu
n
4
][NOsO
3
] afforded the trimetallic
complex [Pt(dppf)(NOsO
3
)Cl] 11. Complex 11
crystallizes in the P2
1
/c space group with
a = 20.058(2),
b = 14.899(1),
c = 23.949(2) Å,
β = 114.57(2)°,
U = 6508(1) Å
3
for
Z = 8. The mean Pt–N, Os–N and
Os–O distances are 2.06, 1.66 and 1.67 Å, respectively.
space group with
a = 7.936(1),
b = 10.758(2),
c = 7.738(1) Å,
α = 100.02(1), β = 99.75(1),
γ = 101.75(1)°,
U = 622.5(2) Å
3
for
Z = 1. The Pt–N (Os), Os–N and the
mean Os–O distances are 1.958(7), 1.681(7) and 1.724 Å,
respectively. Complex 5 crystallises in the
P2
1
/n space group with
a = 10.124(1),
b = 15.564(2),
c = 22.623(3) Å,
β = 100.08(2)°,
U = 3509.7(7) Å
3
for
Z = 4. The Ir–N, Os–N and the mean
Os–O distances are 1.998(7), 1.710(7) and 1.718 Å,
respectively. Treatment of [Au(PPh
3
)(NOsO
3
)] 1
with Ph
3
PNPh gave the N-phosphinimine
complex
[Au(PPh
3
){N(PPh
3
)Ph}][NOsO
3
] 7. Complex 7 crystallises in the
P2
1
/n space group with
a = 8.780(1),
b = 20.781(2),
c = 20.711(5) Å,
β = 91.23(1)°,
U = 3788.0(9) Å
3
for
Z = 4. The Au–N distance is 2.091(8)
Å and the C–N–P angle in the phosphinimine is
127.0(7)°. Reaction of 1 with Bupy led to substitution of Bupy for
[NOsO
3
] and formation of
[Au(PPh
3
)(Bupy)][NOsO
3
] 8. Reaction of
[Pt(dppf)(O
3
SCF
3
)Cl]
[dppf = 1,1′-bis(diphenylphosphino)ferrocene] with
[NBu
n
4
][NOsO
3
] afforded the trimetallic
complex [Pt(dppf)(NOsO
3
)Cl] 11. Complex 11
crystallizes in the P2
1
/c space group with
a = 20.058(2),
b = 14.899(1),
c = 23.949(2) Å,
β = 114.57(2)°,
U = 6508(1) Å
3
for
Z = 8. The mean Pt–N, Os–N and
Os–O distances are 2.06, 1.66 and 1.67 Å, respectively.
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