1322
H.-R. Liu et al. / Journal of Organometallic Chemistry 690 (2005) 1314–1323
50 ml of dry toluene were added and the resulting sol-
vent was then saturated at a monomer relative pressure
of 1 bar, which was maintained throughout the polymer-
ization reactions. Then, the co-catalyst was added in the
proper Al/Ni ratio via a glass syringe. At this time, the
solutions were brought to the desired temperatures
and allowed to equilibrate for 15 min. After this, the
corresponding amount of a toluene solution of the Ni
catalyst was added to the polymerization reactors. The
polymerizations were terminated after several minutes
for ethylene and 1 h for propylene by quenching the
mixture with 150 ml of a 2% HCl/methanol solution.
The obtained polymers were then filtered, washed sev-
eral times with 50 ml portions of methanol and dried
in a vacuum oven at 50 ꢀC for 3 days.
32771/99 and POCTI/QUI/42015/2001 and Grants
SFRH/BPD/3522/2000 and PRAXIS XXI/BD/19638/
99, respectively, to H-R.L. and to S.I.C.), FSE and
FEDER. We are grateful to DST, India, and GRICES,
Portugal, for grants under Indo-Portuguese Collabora-
tion for this investigation. We appreciate the support
by Borealis in the polymerization equipment.
References and Notes
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Crystal structures were obtained using a MACH3
Nonius diffractometer equipped with Mo radiation
˚
(k = 0.71069 A) for complex 4 and a TURBO CAD4
˚
with a Cu rotating anode (k = 1.54180 A) in compound
3. All data were corrected for Lorentz, polarization and
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In both structures all non-hydrogen atoms were re-
fined anisotropically and the hydrogen atoms were in-
serted in idealized positions riding in the parent C atom.
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and 4 are summarized in Table 5. As can be seen, the
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5. Supplementary material
Crystallographic data for the structural analyses have
been deposited with the Cambridge Crystallographic
Data Centre, CCDC, Nos. 239956 and 239957 for the li-
gand 3 and the complex 4, respectively. Copies of this
information may be obtained free of charge from: The
Director, CCDC, 12 Union Road, Cambridge CB2
1EZ UK (Fax: +44-1223-336033; E-mail: deposit@
[17] R. van Asselt, C.J. Elsevier, W.J.J. Smeets, A.L. Spek, R.
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[21] AspenTech, Aspen Engineering SuiteTM 10.2.
[22] In entries LNi3–LNi7 different polymerization times were used
sometimes slightly higher and sometimes slightly lower than those
used in the other runs reported (usually around 6/7 min). This
occurred because either a very high concentration of polymer in
the solution inside the reactor or a very low one was expected for
higher or lower catalyst concentrations in the feed, respectively.
Acknowledgements
This work was funded by Fundac¸a˜o Luso-Americana
para o Desenvolvimento (Projet 122/2000), Fundac¸a˜o
ˆ
para a Ciencia e Tecnologia (Projects POCTI/QUI/