M. Kemmer et al. / Journal of Organometallic Chemistry 608 (2000) 63–70
69
Table 13
Crystallographic data for compound 1, {[Bu2Sn(O2CCF3)2]2O}2
4. Supplementary material
Crystallographic data for compound 1 have been
deposited with the Cambridge Crystallographic Data
Centre, CCDC No. 141898. Copies of this information
may be obtained free of charge from The Director,
CCDC, 12 Union Road, Cambridge CB2 1EZ, UK
Formula
C40H72F12O10Sn4
1415.7
Triclinic
Formula weight
Crystal system
Space group
(
P1
Unit cell dimensions
,
a (A)
12.041(2)
14.423(4)
10.182(2)
106.98(2)
101.87(1)
111.84(2)
1468.1(8)
1
0.2×0.4×0.7
1.601
700
7140
6791
(fax:
+44-1223-336033;
e-mail:
deposit@ccdc.
,
b (A)
cam.ac.uk or www: http://www.ccdc.cam.ac.uk).
,
c (A)
h (°)
i (°)
k (°)
Acknowledgements
3
,
V (A )
Z
Crystal size (mm3)
We thank Eng I. Verbruggen for recording the NMR
spectra and Dr G. Laus and M. Desmet for the mass
spectra. We are grateful to H.J. Kolker, Dr J. Verweij,
Professor Dr G. Stoter, Dr J.H.M. Schellens, Labora-
tory of Experimental Chemotherapy and Pharmacol-
ogy, Department of Medical Oncology, Rotterdam
Cancer Institute, NL-3008 AE, Rotterdam, The
Netherlands, for performing the in vitro tests. This
research was supported by the Belgian Fonds voor
Kollektief Fundamenteel Onderzoek (F.K.F.O. grant
no. 2.0094.94, R.W., M.B.), the Belgian Nationale Lo-
terij (grant no. 9.0006.93, R.W., M.B.), and the Fund
for Scientific Research Flanders (Belgium, grants nos.
G.0192.98, R.W., M.B. and G.0074.00, M.G.), the
Ministe`re de l’Education Nationale du Luxembourg
(grants nos. BFR93/051, BPU96/130, BPU97/138,
BPU98/071 (M.K.) and the Action Vaincre le Cancer
du Luxembourg (M.K.) and the Australian Research
Council (E.R.T.T.). J.C.M. is a Postdoctoral Fellow of
the Fund for Scientific Research Flanders (Belgium)
(FWO).
Dcalc (g cm−3
F(000)
)
No. of data collected
No. of unique data
No. of reflections with I53.0|(I)
R
4136
0.067
0.069
0.59
Rw
−3
,
Residual zmax (e A
)
on F [37]. The Sn and O atoms were refined with
anisotropic displacement parameters, C and F atoms
were refined isotropically, and hydrogen atoms were
included in the model at their calculated positions
,
(C–H 0.95 A). The atoms comprising the molecule are
subject to high thermal motion. Attempts to collect
data at reduced temperatures were unsuccessful as the
crystals fragmented, a frequent experience encountered
for fluorinated samples of the type reported here. Two
positions were resolved for the F atoms comprising
each CF3 group. These were refined with site occupancy
factors of 0.6 and 0.4 (primed atoms) determined from
the refinement. The carbon atoms were refined so that
References
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,
C–C bond distances were constrained to 1.50 A. The
geometric parameters determined for the light atom
positions are thus unreliable, however, the molecular
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a weighting scheme of the form 1/[|2(F)+0.00002ꢀFꢀ2].
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13 and the crystallographic numbering scheme em-
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