under a nitrogen atmosphere. The required amount of co-catalyst
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prescribed temperature was reached, the reactor was pressurized
to the desired pressure. After the reaction mixture was stirred for
the desired period of time, the reaction was stopped and about
1 mL of the reaction solution was collected, quenched by the
addition of 10% aqueous hydrogen chloride and then analyzed by
gas chromatography (GC).
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X-Ray crystallographic studies
Single-crystal X-ray studies for compounds 12 and 5a were carried
out on a Rigaku R-AXIS Rapid IP diffractometer, while the
single-crystal X-ray study for complex 14a was carried out on a
Brucker P4 diffractometer, with graphite-monochromated MoKa
˚
radiation (l = 0.71073 A) at 296(2) K. Cell parameters were
obtained by global refinement of the positions of all collected
reflections. Intensities were corrected for Lorentz and polarization
effects and empirical absorption. The structures were solved by
direct methods and refined by full-matrix least-squares on F2. All
non-hydrogen atoms were refined anisotropically. All hydrogen
atoms were placed in calculated positions. Structure solution and
refinement were performed by using the SHELXL-97 package.28
Crystal data and processing parameters for 12, 5a and 14a are
summarized in Table 6. Due to the quality of the crystals obtained,
the R-factor of structures 12 and 14a are relatively high, however,
the character of structures could be researched.
Acknowledgements
This work was supported by NSFC No. 20674089. We are grateful
to Mr Abiodun Omokehinde Eseola for the English improvement.
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