Synthesis of Molecular Vanadium(III) Phosphonates†
Sumit Khanra Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorMarc Kloth Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorHassanatu Mansaray
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorChristopher A. Muryn Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorFloriana Tuna Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorE. Carolina Sañudo Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorMadeleine Helliwell Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorEric J. L. McInnes Prof.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorRichard E. P. Winpenny Prof.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorSumit Khanra Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorMarc Kloth Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorHassanatu Mansaray
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorChristopher A. Muryn Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorFloriana Tuna Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorE. Carolina Sañudo Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorMadeleine Helliwell Dr.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorEric J. L. McInnes Prof.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorRichard E. P. Winpenny Prof.
School of Chemistry, University of Manchester, Oxford Road , Manchester, M13 9PL, UK, Fax: (+44) 161-275-4616
Search for more papers by this authorWe thank the EPSRC and the EC (NMP3-CT-2005-515767 “Magmanet”) for funding.
Graphical Abstract
Eine ganze Familie: Organophosphonatkomplexe des Vanadiums in hoher Oxidationsstufe sind verbreitet, ihre VIII-Analoga sind dagegen äußerst dünn gesäht. Aus VCl3 und Phosphonaten entsteht unter Solvothermalbedingungen eine ganze Familie entsprechender Vanadium(III)-phosphonate, darunter der schichtförmige Cluster {VIII12(VIVO)} im Bild (V grün, P violett, O rot, C schwarz). Erste Untersuchungen zum magnetischen Verhalten werden ebenfalls beschrieben.
Supporting Information
Supporting information for this article is available on the WWW under http://www.wiley-vch.de/contents/jc_2001/2007/z701115_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
- 1R. C. Finn, J. Zubieta, R. C. Haushalter, Prog. Inorg. Chem. 2003, 51, 421.
- 2G. Centi, F. Trifiro, J. R. Ebner, V. M. Franchetti, Chem. Rev. 1988, 88, 55.
- 3J. W. Johnson, A. J. Jacobsen, W. M. Butler, S. E. Rosenthal, J. F. Brod, J. T. Lewandowsky, J. Am. Chem. Soc. 1989, 111, 381.
- 4
- 4aJ. Salta, Q. Chen, J. Zubieta, Angew. Chem. 1994, 106, 781; Angew. Chem. Int. Ed. Engl. 1994, 33, 757;
- 4bG. Huan, A. J. Jacobsen, V. W. Day, Angew. Chem. 1991, 103, 426; Angew. Chem. Int. Ed. Engl. 1991, 30, 422.
- 5A. Müller, K. Hovemeier, R. Rohlfing, Angew. Chem. 1992, 104, 1214; Angew. Chem. Int. Ed. Engl. 1992, 31, 1192.
- 6
- 6aV. Soghomonian, R. C. Haushalter, J. Zubieta, Chem. Mater. 1995, 7, 1648;
- 6bV. Soghomonian, Q. Chen, R. C. Haushalter, J. Zubieta, Angew. Chem. 1993, 105, 601; Angew. Chem. Int. Ed. Engl. 1993, 32, 610;
- 6cZ. Yiping, A. Clearfield, R. C. Haushalter, Chem. Mater. 1995, 7, 1221.
- 7J. Salta, J. Zubieta, J. Cluster Sci. 1996, 7, 531.
- 8
- 8aR. H. Laye, M. Murrie, S. Ochsenbein, A. R. Bell, S. Teat, J. Raftery, H. U. Güdel, E. J. L. McInnes, Chem. Eur. J. 2003, 9, 6215;
- 8bI. S. Tidmarsh, R. H. Laye, P. R. Brearley, M. Shanmugam, E. C. Sañudo, L. Sorace, A. Caneschi, E. J. L. McInnes, Chem. Commun. 2006, 2560;
- 8cR. H. Laye, Q. Wei, P. V. Mason, M. Shanmugam, S. J. Teat, E. K. Brechin, D. Collison, E. J. L. McInnes, J. Am. Chem. Soc. 2006, 128, 9020.
- 9
- 9aE. I. Tolis, M. Helliwell, S. Langley, J. Raftery, R. E. P. Winpenny, Angew. Chem. 2003, 115, 3934;
10.1002/ange.200351764 Google ScholarAngew. Chem. Int. Ed. 2003, 42, 3804;
- 9bE. I. Tolis, L. P. Engelhardt, P. V. Mason, G. Rajaraman, K. Kindo, M. Luban, A. Matsuo, H. Nojiri, J. Raftery, C. Schröder, G. A. Timco, F. Tuna, W. Wernsdorfer, R. E. P. Winpenny, Chem. Eur. J. 2006, 12, 8961;
- 9cH-C. Yao, J-J. Wang, Y-S. Ma, O. Waldmann, W-X. Du, Y. Song, Y-Z. Li, L-M. Zheng, S. Decurtins, X-Q. Xin, Chem. Commun. 2006, 1745;
- 9dS. Konar, N. Bhuvanesh, A. Clearfield, J. Am. Chem. Soc. 2006, 128, 9604.
- 10
- 10aS. Maheswaran, G. Chastanet, S. J. Teat, T. Mallah, R. Sessoli, W. Wernsdorfer, R. E. P. Winpenny, Angew. Chem. 2005, 117, 5172;
10.1002/ange.200501265 Google ScholarAngew. Chem. Int. Ed. 2005, 44, 5044;
- 10bE. K. Brechin, R. A. Coxall, A. Parkin, S. Parsons, P. A. Tasker, R. E. P. Winpenny, Angew. Chem. 2001, 113, 2772;
10.1002/1521-3757(20010716)113:14<2772::AID-ANGE2772>3.0.CO;2-P Google ScholarAngew. Chem. Int. Ed. 2001, 40, 2700;10.1002/1521-3773(20010716)40:14<2700::AID-ANIE2700>3.0.CO;2-C CAS PubMed Web of Science® Google Scholar
- 10cM. Shanmugam, G. Chastanet, T. Mallah, R. Sessoli, S. J. Teat, G. A. Timco, R. E. P. Winpenny, Chem. Eur. J. 2006, 12, 877;
- 10dM. Shanmugam, M. Shanmugam, G. Chastanet, R. Sessoli, T. Mallah, W. Wernsdorfer, R. E. P. Winpenny, J. Mater. Chem. 2006, 26, 2576.
- 11R. A. Coxall, S. G. Harris, D. K. Henderson, S. Parsons, P. A. Tasker, R. E. P. Winpenny, Dalton Trans. 2000, 2349.
- 12
- 12aR. Sessoli, H.-L. Tsai, A. R. Schake, S. Wang, J. B. Vincent, K. Folting, D. Gatteschi, G. Christou, D. N. Hendrickson, J. Am. Chem. Soc. 1993, 115, 1804;
- 12bR. Sessoli, D. Gatteschi, A. Caneschi, M. A. Novak, Nature 1993, 365, 141.
- 13Crystal data for 1⋅1.75 MeCN⋅0.25 H2O: C99.5H85.75N5.75O15.25P4V4, Mr=1933.63, 0.11×0.11×0.06 mm3, green plate, triclinic, space group P
, a=18.652(4), b=20.154(2), c=26.782(5) Å, α=72.45(3), β=85.23(3), γ=82.78(3)°, V=9512(3) Å3, Z=4, T=150(2) K, λ(synchroton)=0.69040 Å, ρcalcd=1.35 g cm−3, 74 340 reflections collected, 33 461 unique (Rint=0.0604), R(F)=0.0647 and wR2=0.1840 using 26 920 reflections with I>2 σ(I). Crystal data for 2⋅3 MeCN: C65H98N10O19P6V5Cl2, Mr=1834.95, 0.23×0.15×0.08 mm3, green block, monoclinic, space group Cc, a=26.149(5), b=13.331(3), c=49.308(10) Å, β=97.84(3)°, V=17 028(6) Å3, Z=8, T=150(2) K, ρcalcd=1.432 g cm−3, λ(synchroton)=0.69040 Å, 65 309 reflections collected, 29 674 unique (Rint=0.0615), R(F)=0.0444 and wR2=0.1106 using 27 284 reflections with I>2 σ(I). Crystal data for 3⋅2 MeCN: C70H136N2O34P4V6, Mr=1979.33, 0.35×0.15×0.03 mm3, green block, triclinic, space group P
, a=11.968(2), b=15.409(3), c=15.761(3) Å, α=69.32(3), β=69.96(3), γ=77.72(3)°, V=17 028(6) Å3, Z=1, T=100(2) K, ρcalcd=1.294 g cm−3, λ(synchroton)=0.17073 Å, 25 127 reflections collected, 12 935 unique (Rint=0.0349), R(F)=0.0493 and wR2=0.1428 using 9748 reflections with I>2 σ(I). Crystal data for 4: C77H144O39P3V9, Mr=2245.29, 0.23×0.11×0.04 mm3, green block, monoclinic, space group P21/n, a=26.4735(18), b=15.6272(11), c=28.8611(19) Å, β=110.381(10)°, V=11 192.6(13) Å3, Z=4, T=100(2) K, ρcalcd=1.332 g cm−3, λ(synchroton)=0.78480 Å, 76 831 reflections collected, 19 704 unique (Rint=0.1078), R(F)=0.0685 and wR2=0.1693 using 12 032 reflections with I>2 σ(I). Crystal data for 5⋅3 EtOH: C82H168V13O57P8Cl2, Mr=3047.04, 0.1×0.1×0.1 mm3, green block, monoclinic, space group P21/m, a=13.559(5), b=28.725(13), c=18.759(3) Å, β=110.238(9)o, V=6855(4) Å3, Z=2, T=150(2) K, ρcalcd=1.476 g cm−3, λ(synchroton)=0.69070 Å, 6503 reflections collected, 6503 unique (Rint=0.000), R(F)=0.1256, wR2=0.3107 using 4435 reflections with I>2 σ(I). CCDC 639860–CCDC 639864 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.
- 14G. M. Sheldrick, SHELX-97, Program for X-ray Crystal Structure Solution and Refinement; Göttingen University: Göttingen, Germany, 1997.
Citing Literature
This is the
German version
of Angewandte Chemie.
Note for articles published since 1962:
Do not cite this version alone.
Take me to the International Edition version with citable page numbers, DOI, and citation export.
We apologize for the inconvenience.
