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Heteropolymolybdates of AsIII, SbIII, BiIII, SeIV, and TeIV Functionalized by Amino Acids

2002; Wiley; Volume: 41; Issue: 21 Linguagem: Inglês

10.1002/1521-3773(20021104)41

ISSN

1521-3773

Autores

Ulrich Kortz, Masha G. Savelieff, F.Y.A. Ghali, L.M. Khalil, S.A. Maalouf, Dima I. Sinno,

Tópico(s)

Organometallic Compounds Synthesis and Characterization

Resumo

Angewandte Chemie International EditionVolume 41, Issue 21 p. 4070-4073 Communication Heteropolymolybdates of AsIII, SbIII, BiIII, SeIV, and TeIV Functionalized by Amino Acids† Ulrich Kortz Prof., Ulrich Kortz Prof. [email protected] Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461 Current Adress: School of Engineering and Science International University Bremen Campus Ring 1, 28759 Bremem (Germany) Fax: (+49) 421-200-3103Search for more papers by this authorMasha G. Savelieff, Masha G. Savelieff Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461Search for more papers by this authorFida Y. Abou Ghali, Fida Y. Abou Ghali Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461Search for more papers by this authorLina M. Khalil, Lina M. Khalil Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461Search for more papers by this authorSamer A. Maalouf, Samer A. Maalouf Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461Search for more papers by this authorDima I. Sinno, Dima I. Sinno Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461Search for more papers by this author Ulrich Kortz Prof., Ulrich Kortz Prof. [email protected] Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461 Current Adress: School of Engineering and Science International University Bremen Campus Ring 1, 28759 Bremem (Germany) Fax: (+49) 421-200-3103Search for more papers by this authorMasha G. Savelieff, Masha G. Savelieff Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461Search for more papers by this authorFida Y. Abou Ghali, Fida Y. Abou Ghali Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461Search for more papers by this authorLina M. Khalil, Lina M. Khalil Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461Search for more papers by this authorSamer A. Maalouf, Samer A. Maalouf Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461Search for more papers by this authorDima I. Sinno, Dima I. Sinno Department of Chemistry American University of Beirut, P.O. Box: 11-0236 Riad El Solh Beirut 1107 2020 (Lebanon) Fax: (+961) 1-744461Search for more papers by this author First published: 31 October 2002 https://doi.org/10.1002/1521-3773(20021104)41:21 3.0.CO;2-3Citations: 274 † U.K. thanks the American University of Beirut for research support through a URB grant. U.K. also highly appreciates that the Georgetown University Chemistry Department (USA) allowed him unlimited access to the single-crystal X-ray diffractometer. Figure 1–4 were generated by Diamond Version 2.1b (copyright Crystal Impact GbR). Read the full textAboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onEmailFacebookTwitterLinkedInRedditWechat Graphical Abstract Taming the uncontrollable: The novel heteropolymolybdates, such as the [SeIVMo6O21(O2CCH2NH3)3]2− ion shown, functionalized by amino acids, can be derivatized at two different positions in a controlled manner. In addition, further functionalization of the clusters through the amino groups is possible, thus the 18 new compounds are ideal candidates for pharmaceutical applications. Supporting Information Supporting information for this article is available on the WWW under http://www.wiley-vch.de/contents/jc_2002/2002/z19132_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 1 Polyoxometalate Chemistry: From Topology via Self-Assembly to Applications (Ed ), Kluwer, Dordrecht, 2001. 2Special issue on Polyoxometalates Chem. Rev. 1998, 98, 1–390. 3 Polyoxometalates: from Platonic Solids to Anti Retroviral Activity (Ed ), Kluwer, Dordrecht, 1994. 4M. T. Pope, A. Müller, Angew. Chem. 1991, 103, 56–70; Angew. Chem. Int. Ed. Engl. 1991, 30, 34–48. 5M. T. Pope, Heteropoly and Isopoly Oxometalates, Springer, Berlin, 1983. 6P. Gouzerh, A. Proust, Chem. Rev. 1998, 98, 77–111, and references therein. 7 7a“Vanadium Compounds: Chemistry, Biochemistry, and Therapeutic Applications”: ACS Symp. Ser. 1998, 711; 7bA. Müller, S. Sarkar, S. Q. N. Shah, H. Bögge, M. Schmidtmann, S. Sarkar, P. Kögerler, B. Hauptfleisch, A. X. Trautwein, V. Schünemann, Angew. Chem. 1999, 111, 3435–3439; Angew. Chem. Int. Ed. 1999, 38, 3238–3241; 7cA. Müller, S. Polarz, S. K. Das, E. Krickemeyer, H. Bögge, M. Schmidtmann, B. Hauptfleisch, Angew. Chem. 1999, 111, 3439–3443; Angew. Chem. Int. Ed. 1999, 38, 3241–3245; 7dX. Wei, M. H. Dickman, M. T. Pope, Inorg. Chem. 1997, 36, 130–131; 7eK. Wassermann, H.-J. Lunk, R. Palm, J. Fuchs, N. Steinfeldt, R. Stoesser, M. T. Pope, Inorg. Chem. 1996, 35, 3273–3279. 8D. C. Crans, M.-T. Mohammad, O. P. Anderson, M. M. Miller, Inorg. Chem. 1994, 33, 5586–5590. 9M. Fritzsche, K. Elvingson, D. Rehder, L. Pettersson, Acta Chem. Scand. 1997, 51, 483–491. 10M. Inoue, T. Yamase, Bull. Chem. Soc. Jpn. 1995, 68, 3055–3063. 11M. Cindrić, N. Strukan, M. Devçić, B. Kamenar, Inorg. Chem. Commun. 1999, 2, 558-560. 12A. Müller, S. K. Das, C. Kuhlmann, H. Bögge, M. Schmidtmann, E. Diemann, E. Krickemeyer, J. Hormes, H. Modrow, M. Schindler, Chem. Commun. 2001, 655–656. 13M. Sadakane, M. H. Dickman, M. T. Pope, Inorg. Chem. 2001, 40, 2715–2719. 14C. H. Ng, C. W. Lim, S. G. Teoh, H.-K. Fun, A. Usman, S. W. Ng, Inorg. Chem. 2002, 41, 2–3. 15T. Yamase, M. Inoue, H. Naruke, K. Fukaya, Chem. Lett. 1999, 7, 563–564. 16U. Kortz, N. K. Al-Kassem, M. G. Savelieff, N. A. Al Kadi, M. Sadakane, Inorg. Chem. 2001, 40, 4742–4749. 17U. Kortz, M. G. Savelieff, B. S. Bassil, M. H. Dickman, Angew. Chem. 2001, 113, 3488–3491; Angew. Chem. Int. Ed. 2001, 40, 3384–3386. 18U. Kortz, M. G. Savelieff, B. S. Bassil, B. Keita, L. Nadjo, Inorg. Chem. 2002, 41, 783–789. 19K. Y. Matsumoto, Bull. Chem. Soc. Jpn. 1979, 52, 3284–3291. 20U. Kortz, M. T. Pope, Inorg. Chem. 1995, 34, 2160–2163. 21U. Kortz, Inorg. Chem. 2000, 39, 625–626. 22The synthetic details, elemental analyses, and IR spectral data for all the compounds are available in the Supporting Information. 23X-ray structural analyses: Bruker SMART CCD, Mo anode, graphite monochromator, λ=0.71073 Å, refinement (SHELXS-97, SHELXL-97),[25] absorption correction (SADABS),[25] hydrogen-atom positions calculated. K2[SeIVMo6O21(O2CCH2NH3)3]⋅8 H2O: 0.24×0.18×0.08 mm3, orthorhombic, space group Pnma, Z=4, T=167(2) K, a=14.0414(14), b=20.724(2), c=12.2628(12) Å, V=3568.3(6) Å3, 2θmax=56.6°, ρcalcd=2.638 Mg m−3, μ=3.417 mm−1, min/max transmission 0.553/0.779, 38 537 reflections collected, 4537 independent reflections (Rint=0.041), 4290 observed reflections with I>2σ(I), 144 parameters, max residual electron density 1.41 e Å−3, R1=0.048, wR2=0.109; K, Se, Mo refined anisotropically. K(H3N(CH2)2COOH)[SeIVMo6O21(O2C(CH2)2NH3)3]⋅2.5 H2O: 0.20×0.16×0.14 mm3, monoclinic, space group P21/c, Z=4, T=173(2) K, a=10.5238(16), b=20.342(3), c=17.224(3) Å, β=97.626(2), V=3654.6(9) Å3, 2θmax=56.7°, ρcalcd=2.592 Mg m−3, μ=3.220 mm−1, min/max transmission 0.555/0.685, 40 850 reflections collected, 8922 independent reflections (Rint=0.067), 6696 observed reflections with I>2σ(I), 265 parameters, max residual electron density 2.755 e Å−3, R1=0.079, wR2=0.177; K, Se, Mo refined anisotropically. K2[SeIVMo6O21(O2C(CH2)3NH3)3]⋅KCl⋅10 H2O: 0.20×0.14×0.10 mm3, monoclinic, space group P21/n, Z=4, T=173(2) K, a=12.3206(12), b=22.059(2), c=17.3546(16) Å, β=106.130(2), V=4530.9(7) Å3, 2θmax=56.6°, ρcalcd=2.364 Mg m−3, μ=2.856 mm−1, min/max transmission 0.634/0.756, 51 123 reflections collected, 11 056 independent reflections (Rint=0.056), 8979 observed reflections with I>2σ(I), 308 parameters, max residual electron density 1.544 e Å−3, R1=0.040, wR2=0.092; K, Se, Mo, Cl refined anisotropically. K2[SeIVMo6O21(O2CCHCH3NH3)3]⋅4.5 H2O: 0.30×0.20×0.10 mm3, orthorhombic, space group P212121, Z=4, T=293(2) K, a=11.2576(16), b=16.655(2), c=19.285(3) Å, V=3616.0(9) Å3, 2θmax=56.6°, ρcalcd=2.587 Mg m−3, μ=3.364 mm−1, min/max transmission 0.375/0.621, 40 856 reflections collected, 8833 independent reflections (Rint=0.067), 7967 observed reflections with I>2σ(I), 267 parameters, max residual electron density 1.316 e Å−3, R1=0.038, wR2=0.097; K, Se, Mo refined anisotropically. K2[TeIVMo6O21(O2CCH2NH3)3]⋅8 H2O: 0.30×0.14×0.10 mm3, orthorhombic, space group Pnma, Z=4, T=173(2) K, a=13.9561(18), b=20.805(3), c=12.3770(16) Å, V=3593.7(8) Å3, 2θmax=56.6°, ρcalcd=2.709 Mg m−3, μ=3.176 mm−1, min/max transmission 0.596/0.719, 39 150 reflections collected, 4557 independent reflections (Rint=0.051), 4156 observed reflections with I>2σ(I), 144 parameters, max residual electron density 1.663 e Å−3, R1=0.057, wR2=0.132; K, Te, Mo refined anisotropically. K(H3N(CH2)2COOH)[TeIVMo6O21(O2C(CH2)2NH3)3]⋅3 H2O: 0.20×0.16×0.08 mm3, monoclinic, space group P21/c, Z=4, T=173(2) K, a=10.7020(14), b=20.831(3), c=16.771(2) Å, β=97.527(2), V=3706.6(9) Å3, 2θmax=56.7°, ρcalcd=2.657 Mg m−3, μ=2.966 mm−1, min/max transmission 0.634/0.704, 42 108 reflections collected, 9096 independent reflections (Rint=0.062), 6903 observed reflections with I>2σ(I), 265 parameters, max residual electron density 1.660 e Å−3, R1=0.043, wR2=0.090; K, Te, Mo refined anisotropically. Cs2[TeIVMo6O21(O2C(CH2)3NH3)3]⋅5.25 H2O: 0.18×0.16×0.10 mm3, monoclinic, space group P21/n, Z=4, T=293(2) K, a=11.3740(16), b=22.231(3), c=16.887(2) Å, β=102.535(2), V=4168.3(10) Å3, 2θmax=56.7°, ρcalcd=2.697 Mg m−3, μ=4.259 mm−1, min/max transmission 0.507/0.612, 46 889 reflections collected, 10 230 independent reflections (Rint=0.051), 8117 observed reflections with I>2σ(I), 282 parameters, max residual electron density 1.471 e Å−3, R1=0.039, wR2=0.086; Cs, Te, Mo refined anisotropically. K2Na[AsIIIMo6O21(O2CCH2NH3)3]⋅6 H2O⋅0.5 Cl: 0.22×0.06×0.04 mm3, monoclinic, space group P21, Z=2, T=173(2) K, a=11.7166(17), b=13.753(2), c=11.8154(17) Å, β=115.121(2), V=1723.8(4) Å3, 2θmax=56.8°, ρcalcd=2.749 Mg m−3, μ=3.479 mm−1, min/max transmission 0.636/0.856, 20 056 reflections collected, 7708 independent reflections (Rint=0.076), 6330 observed reflections with I>2σ(I), 277 parameters, max residual electron density 1.320 e Å−3, R1=0.050, wR2=0.102; K, Na, As, Mo, Cl refined anisotropically. K2.5Na[SbIIIMo6O21(O2CCH2NH3)3]⋅6 H2O⋅0.5 Cl: 0.10×0.08×0.02 mm3, monoclinic, space group P21, Z=2, T=173(2) K, a=11.7166(17), b=13.753(2), c=11.8154(17) Å, β=115.121(2), V=1723.8(4) Å3, 2θmax=56.8°, ρcalcd=2.877 Mg m−3, μ=3.354 mm−1, min/max transmission 0.705/0.819, 20 076 reflections collected, 8344 independent reflections (Rint=0.068), 6870 observed reflections with I>2σ(I), 277 parameters, max residual electron density 1.682 e Å−3, R1=0.051, wR2=0.097. K, Na, Sb, Mo, Cl refined anisotropically. CCDC-190479–190487 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]). 24I. D. Brown, D. Altermatt, Acta Crystallogr. Sect. B 1985, 41, 244–247. 25G. M. Sheldrick, Acta Crystallogr. Sect. A 1990, 46, 467–473; SHELXS-97, Structure Determination Software Programs, SAINT, Version 4.050, 1996 and SADABS, Bruker Analytical X-ray Instruments, Madison, Wisconsin, USA, 1997. Citing Literature Volume41, Issue21November 4, 2002Pages 4070-4073 ReferencesRelatedInformation

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