F. Zhang et al. / Journal of Organometallic Chemistry 613 (2000) 68–76
75
4. Supplementary material
parameters were refined to R1=0.0440, wR2=0.0965.
Goodness-of-fit indicator was 0.876. All calculations
were performed using SHELX86 and SHELX93 [25].
Crystallographic data (excluding structure factors)
for the structures reported in this paper have been
deposited with the Cambridge Crystallographic Data
Centre as supplementary publication no. CCDC
141918/CCDC 141919. 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@ccdc.cam.ac.uk or www:
http://www.ccdc.cam.ac.uk).
3.8. X-ray structural determination of 4
Crystallographic data are collected in Table 3. Sin-
gle crystals of complex 4 suitable for X-ray diffrac-
tion were grown from
a saturated solution in
CH2Cl2–hexane (1:3, v/v) in fridge (0–4°C). A yellow
crystal of dimensions 0.25×0.16×0.12 mm sealed in
a glass capillary was used. Data were collected on a
Siemens P4 four-circle diffractometer with a graphite
monochromator using Mo–Ka radiation. A total of
6211 reflections were measured in ꢀ−2q scan mode.
The structure was solved by direct methods and
refined by full-matrix least-squares methods on F2.
Hydrogen atoms were located by combination of dif-
ference Fourier map and HYDROGEN program. A to-
tal of 1943 independent data [I\2|(I)] with 237
variable parameters were refined to R1=0.0427,
wR2=0.0763. Goodness-of-fit indicator was 1.026. All
calculations were performed using SHELX86 and
SHELX93 [25].
Acknowledgements
This work was supported by the National Natural
Science Foundation of China (nos. 29734143 and
29672013) and the Sinopec.
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