Parallels in Cation and Anion Coordination: A New Class of Cascade Complexes†
Md. Alamgir Hossain Dr.
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorJosé M. Llinares Dr.
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorSusan Mason Dr.
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorPaula Morehouse
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorDouglas Powell Dr.
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorKristin Bowman-James Prof.
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorMd. Alamgir Hossain Dr.
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorJosé M. Llinares Dr.
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorSusan Mason Dr.
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorPaula Morehouse
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorDouglas Powell Dr.
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorKristin Bowman-James Prof.
Department of Chemistry University of Kansas Lawrence, KS 66045 (USA) Fax: (+1) 785-864-5396
Search for more papers by this authorThis research was sponsored by the Environmental Management Science Program, Offices of Science and Environmental Management, U.S. Department of Energy under Grant DE-FG-96ER62307.
Graphical Abstract
Supporting Information
Supporting information for this article is available on the WWW under http://www.wiley-vch.de/contents/jc_2002/2002/z18101_s.pdf or from the author.
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References
- 1 B. Dietrich, J. Guilhem, J.-M. Lehn, C. Pascard, E. Sonveaux, Helv. Chim. Acta 1984, 67, 91–104.
- 2 Nomenclature: M=m-xylyl, P=p-xylyl, and Fu=furan spacers; E=ethyl links within the tren unit between amine groups; A=amine; cryp=cryptand.
- 3
- 3a S. Mason, T. Clifford, L. Seib, K. Kuczera, K. Bowman-James, J. Am. Chem. Soc. 1998, 120, 8899–8900;
- 3b T. Clifford, A. Danby, J. M. Llinares, S. Mason, N. W. Alcock, D. Powell, J. A. Aguilar, E. García-España, K. Bowman-James, Inorg. Chem. 2001, 40, 4710–4720.
- 4 T. Clifford, S. Mason, J. M. Llinares, K. Bowman-James, J. Am. Chem. Soc. 2000, 122, 1814–1815.
- 5 J. A. Aguilar, T. Clifford, A. Danby, J. M. Llinares, S. Mason, E. García-España, K. Bowman-James, Supramol. Chem. 2001, 13, 405–417.
- 6
- 6a J.-M. Lehn, S. H. Pine, E. I. Watanabe, A. K. Willard, J. Am. Chem. Soc. 1977, 99, 6766–6768;
- 6b J.-M. Lehn, Pure Appl. Chem. 1980, 52, 2441–2459.
- 7
- 7a J. Jazwinski, J.-M. Lehn, D. Lilienbaum, R. Ziessel, J. Guilheim, C. Pascard, J. Chem. Soc. Chem. Commun. 1987, 1691–1692;
- 7b D. McDowell, J. Nelson, Tetrahedron Lett. 1988, 29, 385–386;
- 7c D. Chen, A. E. Martell, Tetrahedron 1991, 47, 6895–6902.
- 8
V. Amendola, E. Bastianello, L. Fabbrizzi, C. Mangano, P. Pallavicini, A. Perotti, A. M. Lanfredi, F. Ugozzoli, Angew. Chem. 2000, 112, 3039–3042;
10.1002/1521-3757(20000818)112:16<3039::AID-ANGE3039>3.0.CO;2-Q Google ScholarAngew. Chem. Int. Ed. 2000, 39, 2917–2920.10.1002/1521-3773(20000818)39:16<2917::AID-ANIE2917>3.0.CO;2-0 CAS PubMed Web of Science® Google Scholar
- 9
X-ray data for 1: A crystal of dimensions 0.64×0.42×0.21 mm was selected for structural analysis. Crystal data: Mr=1161.31; triclinic space group, P
, a=9.8302(11), b=15.9973(19), c=17.417(2) Å, α=84.404(3), β=89.959(3), γ=77.098(2)°, V=2656.5(5) Å3, Z=2, ρcalcd=1.452 g cm−1, F(000)=1232. A total of 12 226 observed reflections (I>2σ(I)) were collected. The refinement converged at R1(F, observed data)=0.0443, and wR2 (F2, all data)=0.1189, and GOF=0.974. Diffraction data were collected using a Bruker SMART APEX CCD area detector mounted on a Bruker D8 goniometer using graphite-monochromated MoKα radiation (λ=0.71073 Å) at 100(2) K.[8] Intensity data were measured as a series of ω and θ oscillation frames each of 0.3° for times of 5 s per frame. The detector was operated in a 512×512 mode and was positioned 5.04 cm from the sample. Coverage of unique data was close to 99.4 % complete to 26.00° in θ. Cell parameters were determined from a least-squares fit of 9504 peaks in the range 2.40<θ<30.58°. Virtually no decay was observed, based on data obtained for a number of peaks monitored at both the beginning and end of data collection. The data were corrected for absorption by the semi-empirical method.[9] Lorentz and polarization corrections were applied. The data were merged to form a set of 15 608 independent data with Rint=0.0248. The space group was determined by statistical tests, and the structure was solved by direct methods and refined by full-matrix least-squares methods on F 2.[10] Hydrogen atom positions were initially determined by geometry and refined by a riding model. Non-hydrogen atoms were refined with anisotropic displacement parameters. CCDC-172118 (1) and CCDC-172119 (2) contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/conts/retrieving.html (or from the Cambridge Crystallographic Data Centre, 12, Union Road, Cambridge CB2 1EZ, UK; fax: (+44) 1223-336-033; or [email protected]).
- 10 Data collection: SMART Software Reference Manual, Bruker-AXS, 6300 Enterprise Dr., Madison, WI 53719-1173, USA, 1994. Data reduction: SAINT Software Reference Manual, Bruker-AXS, 6300 Enterprise Dr., Madison, WI 53719-1173, USA, 1995.
- 11 G. M. Sheldrick, SADABS. Program for Empirical Absorption Correction of Area Detector Data, University of Göttingen, Göttingen (Germany), 1996.
- 12 G. M. Sheldrick, SHELXTL Version 5 Reference Manual, Bruker AXS 5465 E. Cheryl Parkway, Madison, WI 53711-5373, USA, 1994, using International Tables for Crystallography, Vol. C, Kluwer, Boston, 1995, Tab. 6.1.1.4, 4.2.6.8, and 4.2.4.2.
- 13 N. Alcock in Bonding and Structure, Ellis Horwood, West Sussex, England, 1990, p. 316.
- 14 Synthesis, characterization, and structural results for 2 are given in the Supporting Information.
- 15 Protonation constants for PEAcryp have been reported as log K1=9.6(1), log K2=9.00(4), log K3=8.62(8), log K4=7.3(1), log K5=6.7(1), and log K6=6.52(9) using Et4NClO4 as the electrolyte: F. Arnaud-New, S. Fuangswasdi, B. Maubert, J. Nelson, V. McKee, Inorg. Chem. 2000, 39, 573–579.
- 16 R. J. Motekaitis, A. E. Martell, J.-M. Lehn, E.-I. Watanabe, Inorg. Chem. 1982, 21, 4253–4257.
- 17 P. Gans, A. Sabatini, A. Vacca, J. Chem. Soc. Dalton Trans. 1985, 1195–1200.