J. Beckmann, S. L. Jänicke
FULL PAPER
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C 63.78, H 9.40, N 4.06. 5·bpe: Yield 30 mg (43%). C36H58N2O3Si3
(651.13): calcd. C 66.41, H 8.98, N 4.30; found C 66.35, H 9.19, N
4.27. 5·azpy: Yield 40 mg (57%). C34H56N4O3Si3 (653.09): calcd. C
62.53, H 8.64, N 8.58; found C 62.31, H 8.58, N 8.44. 5·bpa: Yield
40 mg (57%). C36H56Si3N2O3 (648.10): calcd. C 66.61, H 8.70, N
4.32; found C 66.12, H 8.71, N 4.19.
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X-ray Crystallography: Intensity data were collected with a Bruker
SMART 1000 CCD diffractometer with graphite-monochromated
Mo-Kα (0.7107 Å) radiation. Data were reduced using the program
SAINT.[17] The structures were solved by direct methods and differ-
ence Fourier synthesis using SHELXS-97 implemented in the pro-
gram WinGX 2002.[18] Full-matrix least-squares refinements on F2,
using all data, were carried out with anisotropic displacement pa-
rameters applied to all non-hydrogen atoms. Disorder of an isopro-
pyl group in 5·0.5H2O was resolved with split occupancies of 0.6
and 0.4 for C81 and C81Ј. The large residual electron density
(2.498 e·Å–3) might be indicative for disorder (of O12) or an unac-
counted solvent molecule; however, all attempts of modelling
failed. Hydrogen atoms attached to carbon atoms were included in
geometrically calculated positions using a riding model and were
refined isotropically. Hydrogen atoms attached to oxygen atoms
were located from the electron-density maps of 5·bpy·0.5H2O,
5·bpe, 5·azpy and 5·bpa and refined isotropically without restraints.
The absolute configuration of 5·azpy has been determined by the
refinement of the Flack parameter [0.00(8)]. Figures were created
using DIAMOND.[19] Further details are listed in Table 6. CCDC-
605353 (5·0.5H2O), -605354 (5·bpy·0.5H2O), -605355 (5·bpe),
-605356 (5·azpy) and -605357 (5·bpa) contain the supplementary
crystallographic data for this paper. These data can be obtained
free of charge from The Cambridge Crystallographic Data Centre
via www.ccdc.cam.ac.uk/data_request/cif.
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Acknowledgments
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[12] R. West, R. H. Baney, J. Am. Chem. Soc. 1959, 81, 6145–6148.
Mrs. Irene Brüdgam (Freie Universität Berlin) is gratefully ac-
knowledged for the X-ray data collection.
¯
[13] Crystal system: tetragonal, space group: P4, cell dimensions: a
= 11.3732(10), c = 11.1566(21) Å.
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[19] DIAMOND, V2.1d, Crystal Impact, K. Brandenburg & M.
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Received: April 27, 2006
Published Online: July 25, 2006
3358
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Eur. J. Inorg. Chem. 2006, 3351–3358