2
608
F. Majoumo-Mbe et al. / Journal of Organometallic Chemistry 693 (2008) 2603–2609
C
84
H
96
N
4
Ni
2
P
4
: M = 1403.00. Anal. Calc. for C84
H
96
N
4
Ni
2
P
4
ꢄ 4OEt
2
to a vacuum line, and a measured amount (10 ml or 40 ml) of iso-
butene was transferred under vacuum to the reactor (by a similar
procedure as for propene but at ꢀ30 °C). After the reaction was fin-
ished the excess of isobutene was released in a well-ventilated
hood. The products were separated similar to the procedure de-
scribed for 1-hexene: a 1:1 mixture of methylene chloride and
HCl (10 wt% in water) was added to the Schlenk tube. After neu-
tralization of the catalytic mixture, the contents of the Schlenk
tube were transferred to a separating funnel. The organic fraction
(
1699.49): C, 70.7; H, 8.0; N, 3.3. Found: C, 70.0; H, 9.4; N, 3.2%.
3.2. Reaction of complex 1 with ethene
In a glove box a high-pressure reactor (100 ml) was charged
ꢀ
3
with complex 1 (10 mg, 7.13 ꢁ 10 mmol), the desired amount
of MAO according to the Ni:Al ratio, and 10 ml of solvent. Then
the reactor was connected to a high-pressure line and filled with
ethene (99.999%) at 20 atm. To maintain a constant pressure of
4
was separated and dried with MgSO . After filtration the mixture
2
0 atm a solenoid valve was used. Hence, when the pressure in
was analyzed by NMR and GCMS.
the reactor was reduced it was refilled constantly. After a specific
amount of time, the reactor (kept at ꢀ30 °C) was opened in a
well-ventilated hood, the raw content was weighed, and the
amount of products was calculated as the difference between the
mass of raw content and the sum of the masses of the catalyst,
MAO, and the solvent. The raw product was maintained at
4
. Supplementary material
CCDC 652339 contains the supplementary crystallographic data
ꢀ
4
30 °C to keep the C fraction liquid and filtered. From the result-
ing liquid samples for NMR and GCMS were taken. The solid mate-
rial obtained at room temperature was washed with a 1:1 mixture
of methanol and HCl (10 wt% solution), filtered again, washed with
acetone, and dried under vacuum.
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(
(
(
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1
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(
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(
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(
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[
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3
.4. Reaction of complex 1 with 1-hexene and 1,5-hexadiene
(
(
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ꢀ3
glove box with catalyst 1 (10 mg, 7.13 ꢁ 10 mmol), the desired
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(
(
(
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(
[
1
:1 mixture of methylene chloride and HCl (10 wt% in water)
was added to the Schlenk tube. After neutralization of the catalytic
mixture with solid NaHCO , the content of the Schlenk tube was
transferred to a separating funnel. The organic fraction was sepa-
rated and dried with MgSO . After filtration the vessel was con-
nected to flash evaporator, and methylene chloride was
(
(
(
(
c) X. Tang, Y. Cui, W.-H. Sun, Z. Miao, S. Yan, Polym. Int. 53 (2004) 2155;
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3
4
(f) Y. Chen, G. Wu, G.C. Bazan, Angew. Chem., Int. Ed. 44 (2005) 1108;
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(
2
(
a
removed by vacuum. The resulting residue was analyzed by NMR
and GCMS.
(i) H.Y. Kwon, S.Y. Lee, B.Y. Lee, D.M. Shin, Y.K. Chung, J. Chem. Soc., Dalton
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(
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k) J.N.L. Dennett, A.L. Gillon, K. Heslop, D.J. Hyett, J.S. Fleming, C.E. Lloyd-
3.5. Reaction of complex 1 with isobutene
(
The reactions were carried out in a high-pressure stainless steel
Jones, A.G. Orpen, P.G. Pringle, D.F. Wass, J.N. Scutt, R.H. Weatherhead,
Organometallics 23 (2004) 6077;
reactor (100 ml) charged in a glove box with complex 1 (10 mg,
(
l) C. Mueller, L.J. Ackerman, J.N.H. Reek, P.C.J. Kamer, P.W.N.M. van Leeuwen,
ꢀ
3
7
.13 ꢁ 10 mmol), the desired amount of MAO according to the
J. Am. Chem. Soc. 126 (2004) 14960;
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Ni:Al ratio, and 10 ml of solvent. Then, the reactor was connected