Communication
Pb22− as Ligand in [Ph4P]2[{W(CO)5}4Pb2]
Peter Rutsch Dipl.-Chem.,
Gottfried Huttner Prof. Dr.,
Peter Rutsch Dipl.-Chem.
Anorganisch-chemisches Institut der Universität Heidelberg Im Neuenheimer Feld 270, 69120 Heidelberg (Germany) Fax: (+49) 6221-545-707
Search for more papers by this authorGottfried Huttner Prof. Dr.
Anorganisch-chemisches Institut der Universität Heidelberg Im Neuenheimer Feld 270, 69120 Heidelberg (Germany) Fax: (+49) 6221-545-707
Search for more papers by this authorPeter Rutsch Dipl.-Chem.,
Gottfried Huttner Prof. Dr.,
Peter Rutsch Dipl.-Chem.
Anorganisch-chemisches Institut der Universität Heidelberg Im Neuenheimer Feld 270, 69120 Heidelberg (Germany) Fax: (+49) 6221-545-707
Search for more papers by this authorGottfried Huttner Prof. Dr.
Anorganisch-chemisches Institut der Universität Heidelberg Im Neuenheimer Feld 270, 69120 Heidelberg (Germany) Fax: (+49) 6221-545-707
Search for more papers by this authorFirst published: 13 October 2000
Citations: 11
This work was supported by the Fonds der Chemischen Industrie and by the Deutsche Forschungsgemeinschaft (SFB 247).
Abstract
References
- 1
K. P. Huber, G. Herzberg in Molecular Spectra and Molecular Structure, IV. Constants of Diatomic Molecules, Vol. 4, Van Nostrand Reinhold Company, New York, 1979.
10.1007/978-1-4757-0961-2 Google Scholar
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- 4 The bond dissociation energy of Pb22− is not known. The experimentally determined sequence of dissociation energies of Pb2 (8 valence electrons, 0.8 eV), PbBi (9 valence electrons, 1.4 eV), and BiBi (10 valence electrons, 2.0 eV) suggests that Pb22− with 10 valence electrons should be comparably stable. For details on the properties of diatomic molecules see ref. [1].
- 5 At lower temperatures the crystals of [(Ph4P)+]2-1 decompose with retention of their habitus to give an X-ray amorphous powder (for the structure of [(Ph4P)+]2-1 see ref. [6]).
- 6 Crystal structure data: The X-ray structure analysis was carried out on a Nonius-Kappa-CCD diffractometer with MoKα radiation (λMo=0.71074 Å). Data collection and reduction was performed with the Nonius Software COLLECT.[11] The SHELXTL-PLUS software package was used for the structure solution and refinement. The structures were solved by direct methods with SHELXS-86 and refined with SHELXL-93.[12] The program XPMA was used for the graphical workup of the data.[13] The figure was generated with WINRAY-32.[14] The refinement was carried out anisotropically against F 2, hydrogen atoms were included in calculated positions. Structure data for 1: space group P1¯, a=12.343(3), b=12.806(3), c=24.605(5) Å, α=96.69(3), β=96.94(3), γ=110.85(3)°, V=3554×106 pm3, ρcalcd=2.232 g cm−3, 2θmax=61.8°, Z=2, 41 927 measured reflections, 21 593 independent reflections, of which 12 537 were observed (I>2σ(I)), 868 refined parameters, R=0.051, Rw=0.113, residual electron density ≤4.39×10−6 e pm−3. (An overview of more than 250 X-ray crystallographically determined Pb−Pb distances is found in the database of the Cambridge Crystallographic Data Centre (status 1999): F. H. Allen, J. E. Davis, J. J. Galloy, O. Johnson, O. Kennard, C. F. Macrae, E. M. Mitchell, G. F. Mitchell, J. M. Smith, D. G. Watson, J. Chem. Inf. Comput. Sci. 1991, 31, 187–204.) Crystallographic data (excluding structure factors) for the structure reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication no. CCDC-141592. Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax: (+44) 1223-336-033; e-mail: [email protected]).
- 7 The distances to Pb1, which bears the terminal W(CO)5 group, are all slightly longer than the Wb−Pb2 distances to the non-terminally coordinated Pb center (see Figure 1).
- 8 P. Kircher, G. Huttner, K. Heinze, J. Organomet. Chem. 1998, 562, 217–227.
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- 10 E. Lindner, H. Behrens, S. Birkle, J. Organomet. Chem. 1968, 15, 165–175.
- 11 COLLECT, software for data collection, Nonius, 1998; http://www.nonius.com.
- 12a G. M. Sheldrick, SHELXS-86, Program for Crystal Structure Solution, Universität Göttingen, 1986;
- 12b G. M. Sheldrick, SHELXL-93, Program for Crystal Structure Refinement, Universität Göttingen, 1993; http://www.shelx.uni-ac.gwdg.de/shelx/index.html;
- 12c International Tables for X-Ray Crystallography, Vol. 4, Kynoch, Birmingham, 1974.
- 13 L. Zsolnai, G. Huttner, XPMA, Universität Heidelberg, 1998; http://www.rzuser.uni-heidelberg.de/~v54/xpm.html.
- 14 R.Soltek, G. Huttner, WINRAY-32, Universität Heidelberg, 1998; http://www.rzuser.uni-heidelberg.de/~v54.
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