Crystal structure determinations
11 W. Doman´ska and J. Pikies, VIIth Polish Symposium of the Heteroor-
ganic Section of the Polish Chemical Society, Ło´dz´, Poland, 25.11.2004,
abstract P – 5.
Diffraction data were collected at 100 K (13·toluene) and 120 K
(other compounds) on a KUMA KM4CCD diffractometer, Ox-
ford Diffraction Ltd. Numerical absorption correction based on
the multi-faceted crystal shape with empirical scaling was applied
(CrysAlis RED, Oxford Diffraction22). Details of crystal data,
data collection and refinement are summarized in Table 2 (supple-
mentary materials). The structures were solved by direct methods
using the SHELX-97 program package23,24 and refined with full-
matrix least-squares on F2. All atoms, excluding hydrogen, were
refined with anisotropic displacement ellipsoids. Hydrogen atoms
were positioned geometrically and refined as riding on their heavy
atoms.
12 W. Doman´ska, J. Chojnacki and J. Pikies, Acta Cryst., 2005, E61,
m1114.
13 W. Doman´ska-Babul, K. Baranowska, R. Grubba, E. Matern and J.
Pikies, Polyhedron, 2007, 26, 2491.
14 E. Matern, J. Pikies and G. Fritz, Z. Anorg. Allg. Chem., 2000, 626,
2136.
15 J. Chatt, R. Mason and D. W. Meek, J. Am. Chem. Soc., 1975, 97, 3826.
16 M. L Clarke, G. L. Holliday, A. M. Z. Slavin and J. D. Wollins, J. Chem.
Soc. Dalton Trans., 2002, 1093.
17 F. B. Ogilvie, J. M. Jenkins and J. G. Verkade, J. Am. Chem. Soc., 1970,
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19 H. Krautscheid, E. Matern, J. Olkowska-Oetzel, J. Pikies and G. Fritz,
Z. Anorg. Allg. Chem., 2001, 627, 1505.
20 H. Goesmann, E. Matern, J. Olkowska-Oetzel, J. Pikies and G. Fritz,
Z. Anorg. Allg. Chem., 2001, 627, 1181.
The toluene molecules were left isotropic for 4·toluene and
13·toluene. In the later case the solvent was refined as disordered
over two positions. In both cases C–C bond lengths in toluene
were restrained to have physically acceptable values.
21 Oxford Diffraction, CrysAlis CCD and CrysAlis RED. Version 1.171.
Oxford Diffraction Ltd, Abingdon, Oxfordshire, England, 2005.
22 G. M. Sheldrick, SHELXS97. Program for crystal structure solution,
University of Go¨ttingen, Germany, 1997.
23 G. M. Sheldrick, SHELXL97. Program for crystal structure refinement,
Acknowledgements
University of Go¨ttingen, Germany, 1997.
24 H. Krautscheid, E. Matern, G. Fritz and J. Pikies, Z. Anorg. Allg.
Chem., 1998, 624, 501.
25 H. Krautscheid, E. Matern, J. Pikies and G. Fritz, Z. Anorg. Allg.
Chem., 2000, 626, 2133.
W. D.-B. and J. P. thank the Polish State Committee of Scientific
Research (project No. 1 T09A 148 30) for financial support.
26 A. G. Orpen and N. G. Connelly, Organometallics, 1990, 9, 1206.
27 W. Doman´ska-Babul, J. Chojnacki and J. Pikies, Phosphorus, Sulfur,
Silicon, Relat. Elem., accepted.
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