Synthesis, Crystal Structure, and Reactivity of the Strong Methylating Agent Me2B12Cl12†
Version of Record online: 6 APR 2010
Copyright © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Angewandte Chemie International Edition
Volume 49, Issue 20, pages 3536–3538, May 3, 2010
How to Cite
Bolli, C., Derendorf, J., Keßler, M., Knapp, C., Scherer, H., Schulz, C. and Warneke, J. (2010), Synthesis, Crystal Structure, and Reactivity of the Strong Methylating Agent Me2B12Cl12. Angew. Chem. Int. Ed., 49: 3536–3538. doi: 10.1002/anie.200906627
We are grateful to the Deutsche Forschungsgemeinschaft and the Universität Freiburg for financial support and Prof. Ingo Krossing for support and helpful discussions.
- Issue online: 28 APR 2010
- Version of Record online: 6 APR 2010
- Manuscript Received: 24 NOV 2009
- Deutsche Forschungsgemeinschaft
- Universität Freiburg
- 6Single-crystal X-ray structure determinations were carried out on a Rigaku R-AXIS Spider image-plate diffractometer using MoKα radiation (0.71073 Å). The crystals were selected at −30 °C and mounted onto a cryo loop using fluorinated oil and frozen in the cold nitrogen stream of the goniometer. The structures were solved by direct methods. Subsequent least-squares refinement on F 2 located the positions of the remaining atoms in the electron density maps. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in calculated positions using a riding model and were refined isotropically in blocks. (G. M. Sheldrick, SHELX-97 Programs for Crystal Structure Analysis, Universität Göttingen, 1997). The data were corrected for absorption (semi-empirical from equivalents). C2H6B12Cl12: Mr=585.19, orthorhombic, Pbca, a=1244.3(3), b=1193.0(2), c=1354.6(3) pm, V=2.0108(7) nm3, Z=4, μ=1.640 mm−1, T=100(2) K, 29 985 reflections measured, 1768 independent (Rint=0.1176), R1=0.0393 (I>2σ(I)), wR2=0.0797 (all data). C9H24B12Cl12S2: Mr=751.54, trigonal, Rm, a=b=1082.9(3), c=2486.0(5) pm, V=2.5247(11) nm3, Z=3, μ=1.117 mm−1, T=120(2) K, 16 043 reflections measured, 754 independent (Rint=0.0460), R1=0.0299 (I>2σ(I)), wR2=0.1073 (all data). CCDC 755209 and CCDC 755210 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.
- 8M. Keßler, C. Knapp, V. Sagawe, H. Scherer, R. Uzun, unpublished results.
- 15J. Warneke, T. Dülcks, D. Gabel, C. Knapp, unpublished results.