Unusual Coordination Behavior of Pn-Ligand Complexes with Tl+†
Stefan Welsch
Institut für Anorganische Chemie, Universität Regensburg, 93040 Regensburg, Germany, Fax: (+49) 941-943-4439
Search for more papers by this authorLaurence J. Gregoriades Dr.
Institut für Chemie, Humboldt-Universität zu Berlin, 10099 Berlin, Germany
Search for more papers by this authorMarek Sierka Dr.
Institut für Chemie, Humboldt-Universität zu Berlin, 10099 Berlin, Germany
Search for more papers by this authorManfred Zabel Dr.
Institut für Anorganische Chemie, Universität Regensburg, 93040 Regensburg, Germany, Fax: (+49) 941-943-4439
Search for more papers by this authorAlexander V. Virovets Dr.
Nikolaev Institute of Inorganic Chemistry, Siberian Division of RAS, Acad. Lavrentyev str. 3, 630090 Novosibirsk, Russia
Search for more papers by this authorManfred Scheer Prof. Dr.
Institut für Anorganische Chemie, Universität Regensburg, 93040 Regensburg, Germany, Fax: (+49) 941-943-4439
Search for more papers by this authorStefan Welsch
Institut für Anorganische Chemie, Universität Regensburg, 93040 Regensburg, Germany, Fax: (+49) 941-943-4439
Search for more papers by this authorLaurence J. Gregoriades Dr.
Institut für Chemie, Humboldt-Universität zu Berlin, 10099 Berlin, Germany
Search for more papers by this authorMarek Sierka Dr.
Institut für Chemie, Humboldt-Universität zu Berlin, 10099 Berlin, Germany
Search for more papers by this authorManfred Zabel Dr.
Institut für Anorganische Chemie, Universität Regensburg, 93040 Regensburg, Germany, Fax: (+49) 941-943-4439
Search for more papers by this authorAlexander V. Virovets Dr.
Nikolaev Institute of Inorganic Chemistry, Siberian Division of RAS, Acad. Lavrentyev str. 3, 630090 Novosibirsk, Russia
Search for more papers by this authorManfred Scheer Prof. Dr.
Institut für Anorganische Chemie, Universität Regensburg, 93040 Regensburg, Germany, Fax: (+49) 941-943-4439
Search for more papers by this authorThis work was supported by the Deutsche Forschungsgemeinschaft and the Fonds der Chemischen Industrie. The authors would like to thank Prof. Dr. W. Kunz and Dr. R. Neueder for their support with the VPO measurements, Prof. Dr. E. Brunner and Dipl.-Phys. C. Gröger for the solid-state NMR measurements, and Cand.-Chem. T. Rödl for technical assistance.
Graphical Abstract
Pentaphosphaferrocene coordinates as a π ligand to the large monocation Tl+. In addition, one of the phosphorus atoms of each cyclo-P5 moiety coordinates to a neighboring Tl+ ion to give a one-dimensional polymer. Even at low temperatures, fast rotation of the P5 rings is observed in solution and in the solid state.
Supporting Information
Supporting information for this article is available on the WWW under http://www.wiley-vch.de/contents/jc_2002/2007/z704015_s.pdf or from the author.
Please note: The publisher is not responsible for the content or functionality of any supporting information supplied by the authors. Any queries (other than missing content) should be directed to the corresponding author for the article.
References
- 1Recent review articles:
- 1aW. Huang, H.-B. Zhu, S.-H. Gou, Coord. Chem. Rev. 2006, 250, 414–423;
- 1bN. C. Gianneschi, M. S. Masar III, C. A. Mirkin, Acc. Chem. Res. 2005, 38, 825–837;
- 1cM. Ruben, J. Rojo, F. J. Romero-Salguero, L. H. Uppadine, J.-M. Lehn, Angew. Chem. 2004, 116, 3728–3747;
10.1002/ange.200300636 Google ScholarAngew. Chem. Int. Ed. 2004, 43, 3644–3662;
- 1dL. Carlucci, G. Ciani, D. M. Proserpio, Coord. Chem. Rev. 2003, 246, 247–289;
- 1eG. F. Swiegers, T. J. Malefetse, Coord. Chem. Rev. 2002, 225, 91–121.
- 2aO. J. Scherer, T. Brück, Angew. Chem. 1987, 99, 59; Angew. Chem. Int. Ed. Engl. 1987, 26, 59;
- 2bO. J. Scherer, T. Brück, G. Wolmershäuser, Chem. Ber. 1988, 121, 935–938.
- 3
- 3aL. Y. Goh, C. K. Chu, R. C. S. Wong, T. W. Hambley, J. Chem. Soc. Dalton Trans. 1989, 1951–1956;
- 3bO. J. Scherer, H. Sitzmann, G. Wolmershäuser, J. Organomet. Chem. 1984, 268, C 9-C12.
- 4
- 4aJ. Bai, E. Leiner, M. Scheer, Angew. Chem. 2002, 114, 820–823;
Angew. Chem. Int. Ed. 2002, 41, 783–786;
10.1002/1521-3773(20020301)41:5<783::AID-ANIE783>3.0.CO;2-J CAS PubMed Web of Science® Google Scholar
- 4bM. Scheer, L. Gregoriades, J. Bai, M. Sierka, G. Brunklaus, H. Eckert, Chem. Eur. J. 2005, 11, 2163–2169;
- 4cM. Scheer, L. J. Gregoriades, M. Zabel, M. Sierka, L. Zhang, H. Eckert, Eur. J. Inorg. Chem. 2007, 2775–2782.
- 5J. Bai, A. V. Virovets, M. Scheer, Angew. Chem. 2002, 114, 1808–1811;
Angew. Chem. Int. Ed. 2002, 41, 1737–1740.
10.1002/1521-3773(20020517)41:10<1737::AID-ANIE1737>3.0.CO;2-4 CAS PubMed Web of Science® Google Scholar
- 6
- 6aJ. Bai, A. V. Virovets, M. Scheer, Science 2003, 300, 781–783;
- 6bM. Scheer, J. Bai, B. P. Johnson, R. Merkle, A. V. Virovets, C. E. Anson, Eur. J. Inorg. Chem. 2005, 4023–4026.
- 7M. Scheer, L. J. Gregoriades, A. V. Virovets, W. Kunz, R. Neueder, I. Krossing, Angew. Chem. 2006, 118, 5818–5822; Angew. Chem. Int. Ed. 2006, 45, 5689–5693.
- 8I. Krossing, Chem. Eur. J. 2001, 7, 490–502.
10.1002/1521-3765(20010119)7:2<490::AID-CHEM490>3.0.CO;2-I CAS PubMed Web of Science® Google Scholar
- 9M. Scheer, L. J. Gregoriades, M. Zabel, J. Bai, I. Krossing, G. Brunklaus, H. Eckert, Chem. Eur. J. 2007, .
- 10For an early review see: H. Schmidbaur, Angew. Chem. 1985, 97, 893–904; Angew. Chem. Int. Ed. Engl. 1985, 24, 893–904.
- 11
- 11aY. Sarazin, D. L. Hughes, N. Kaltsoyannis, J. A. Wright, M. Bochmann, J. Am. Chem. Soc. 2007, 129, 881–894;
- 11bY. Sarazin, N. Kaltsoyannis, J. A. Wright, M. Bochmann, Organometallics 2007, 26, 1811–1815.
- 12H. Schmidbaur, W. Bublak, J. Riede, G. Müller, Angew. Chem. 1985, 97, 402–403; Angew. Chem. Int. Ed. Engl. 1985, 24, 414–415.
- 13
- 13aS. H. Strauss, M. D. Noirot, O. P. Anderson, Inorg. Chem. 1986, 25, 3850–3851;
- 13bM. D. Noirot, O. P. Anderson, S. H. Strauss, Inorg. Chem. 1987, 26, 2216–2223;
- 13cA. M. Bandman, C. B. Knobler, M. F. Hawthorne, Inorg. Chem. 1988, 27, 2399–2400;
- 13dH. Schmidbaur, W. Bublak, B. Huber, J. Hofmann, G. Müller, Chem. Ber. 1989, 122, 265–270;
- 13eW. Frank, G. Korrell, G. J. Reiß, Z. Anorg. Allg. Chem. 1995, 621, 765–770;
- 13fW. Frank, G. Korrell, G. J. Reiß, J. Organomet. Chem. 1996, 506, 293–300;
- 13gR. S. Mathur, T. Drovetskaya, C. A. Reed, Acta Crystallogr. Sect. C 1997, 53, 881–883.
- 14M. Gonsior, I. Krossing, N. Mitzel, Z. Anorg. Allg. Chem. 2002, 628, 1821–1830.
- 15The crystal structure analyses were performed on a STOE-IPDS diffractometer using MoKα radiation (λ=0.71073 Å). The structures were solved with the programs SIR-97[20] (4) and SHELXS-97[21a] (5); full-matrix-least-squares refinement on F 2 in SHELXL-97[21b] was performed with anisotropic displacements for heavy atoms in 4 and for all non-H atoms in 5. As the two counteranions [Al{OC(CF3)3}4]− of 4 were disordered, numerous restraints (SADI) had to be used to order the atoms in appropriate positions,[22] which lead to somewhat elevated wR2 values. For 5, a twinning refinement using the merohedral twin law (0 −1 0; −1 0 0; 0 0 −1) was applied. The relative weighting of the two components was refined to 42.1(1) and 57.9(1) %. Hydrogen atoms were located in idealized positions and refined isotropically according to the riding model. 4: C121H72Al2F72Mo12O32P12Tl2, Mr=5391.41, crystal dimensions 0.40×0.24×0.20 mm3, orthorhombic, space group Pbca (No. 61), a=35.998(2), b=20.9594(11), c=43.1881(19) Å, V=32 585(3) Å3, Z=8, T=123(1) K, ρcalcd=2.169 g cm−3, μ=3.135 mm−1, 66 420 reflections collected, 15 153 unique reflections (Rint=0.1488), 1120 parameters, R1=0.0732, wR2=0.1504. 5: C46H45AlF36Fe3O4P15Tl, Mr=2209.27, crystal dimensions 0.30×0.10×0.10 mm3, trigonal, space group P31c (No. 159), a=19.401(3), b=19.401(3), c=11.367(2) Å, V=3705.3(10) Å3, Z=2, T=100(1) K, ρcalcd=1.980 g cm−3, μ=3.211 mm−1, 26 508 reflections collected, 5181 unique reflections (Rint=0.0304), 325 parameters, R1=0.0284, wR2=0.0761. CCDC-658370 (4) and CCDC-658371 (5) 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.
- 16I. R. Shapiro, D. M. Jenkins, J. C. Thomas, M. W. Day, J. C. Peters, Chem. Commun. 2001, 2152–2153.
- 17J. F. Hinton, Magn. Reson. Chem. 1987, 25, 659–669.
- 18O. J. Scherer, T. Brück, G. Wolmershäuser, Chem. Ber. 1989, 122, 2049–2054.
- 19A. R. Fox, R. J. Wright, E. Rivard, P. P. Power, Angew. Chem. 2005, 117, 7907–7911;
10.1002/ange.200502865 Google ScholarAngew. Chem. Int. Ed. 2005, 44, 7729–7733.
- 20A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna, J. Appl. Crystallogr. 1999, 32, 115–119.
- 21aG. M. Sheldrick, SHELXS-97, Universität Göttingen, 1997;
- 21bG. M. Sheldrick, SHELXL-97, Universität Göttingen, 1997.
- 22I. Krossing, A. Reisinger, Coord. Chem. Rev. 2006, 250, 2721–2744.
- 23A. Klamt, G. Schüürmann, J. Chem. Soc. Perkin Trans. 2 1993, 799–805.
- 24
- 24aR. Ahlrichs, M. Bär, M. Häser, H. Horn, C. Kölmel, Chem. Phys. Lett. 1989, 162, 165–169;
- 24bO. Treutler, R. Ahlrichs, J. Chem. Phys. 1995, 102, 346–354.
- 25
- 25aA. D. Becke, Phys. Rev. A 1988, 38, 3098–3100;
- 25bS. H. Vosko, L. Wilk, M. Nusair, Can. J. Phys. 1980, 58, 1200–1211;
- 25cJ. P. Perdew, Phys. Rev. B 1986, 33, 8822–8824; erratum: J. P. Perdew, Phys. Rev. B 1986, 34, 7406.
- 26F. Weigend, R. Ahlrichs, Phys. Chem. Chem. Phys. 2005, 7, 3297–3305.
- 27
- 27aK. Eichkorn, O. Treutler, H. Öhm, M. Häser, R. Ahlrichs, Chem. Phys. Lett. 1995, 242, 652;
- 27bM. Sierka, A. Hogekamp, R. Ahlrichs, J. Chem. Phys. 2003, 118, 9136–9148.
- 28F. Weigend, Phys. Chem. Chem. Phys. 2006, 8, 1057–1065.
- 29B. Metz, M. Schweizer, H. Stoll, M. Dolg, W. Liu, Theor. Chem. Acc. 2000, 104, 22–28.