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Vol.6 , No. 1, Publication Date: Jan. 10, 2020, Page: 1-6
 perchlorate hexahydrate, (Co(ClO<sub>4</sub>)<sub>2</sub>.6H<sub>2</sub>O) was reacted with a water soluble sulphonated pyridyl-triazole <i>N,N</i>-bidentate ligand (2-(1-((pyridine-2-yl)methyl)-1<i>H</i>-1,2,3-triazol-4-yl)ethyl sodium sulfate, `ligand 1.Na) in methanol to form [Co(ligand 1)<sub>2</sub>(H<sub>2</sub>O)<sub>2</sub>].4H<sub>2</sub>O as a microcrystalline solid. In this context, ligand 1.Na was first synthesized by the cycloaddition reaction of 2-(azidomethyl)pyridine and sodium 3-butyn-1-sulfate in 4:1 <i>tert</i>-BuOH/water solvents in presence of Cu(AcO)<sub>2</sub>H<sub>2</sub>O (10-15 mol %) as catalyst. The ligand 1.Na was white solid, absorbed moisture at open air, soluble in methanol and DMSO and characterized by elemental analysis, ESI-MS spectrum in the negative mode, <sup>1</sup>H NMR and <sup>13</sup>C NMR spectroscopy. In the <sup>1</sup>H NMR spectrum of ligand 1.Na in CD<sub>3</sub>OD, a characteristic triazole strong singlet peak appeared at 7.97 ppm, a remarkable shift of δ value for CH<sub>2</sub> proton of 2-(azidomethyl)pyridine was observed. In the <sup>13</sup>C NMR spectrum, the triazole carbon resonates at 137.90 ppm. The prepared complex was characterized by physical data, FT-IR, ESI-MS and elemental analysis. The light pink crystals are fairly stable at open atmosphere even if they slowly loose the lattice solvent. The ESI-MS spectrum of [Co(ligand 1)<sub>2</sub>(H<sub>2</sub>O)<sub>2</sub>].4H<sub>2</sub>O indicates the species [Co(ligand 1.Na)(ligand 1)]<sup>+</sup> and [Co(ligand 1.Na)]<sup>+</sup> which corresponds to the <i>m/z</i> value at 648.6 and 402.6 respectively. Based on the observed data, octahedral geometry of the synthesized complex was suggested.&picture=http://www.aascit.org/aascit/decorators/img/journal/978.jpg)
| [1] | Md. Mahbubul Alam, Department of Molecular Science and Nanosystems (DSMN), University of Venice, Via Torino, Italy; Department of Chemistry, Shahjalal University of Science and Technology, Sylhet, Bangladesh. |
| [2] | Beghetto Valentina, Department of Molecular Science and Nanosystems (DSMN), University of Venice, Via Torino, Italy. |
| [3] | Alberto Scrivanti, Department of Molecular Science and Nanosystems (DSMN), University of Venice, Via Torino, Italy. |
| [4] | Matteo Bertoldini, Department of Molecular Science and Nanosystems (DSMN), University of Venice, Via Torino, Italy. |
| [5] | Mohammad Salim, Department of Chemistry, Shahjalal University of Science and Technology, Sylhet, Bangladesh. |
Cobalt(II) perchlorate hexahydrate, (Co(ClO4)2.6H2O) was reacted with a water soluble sulphonated pyridyl-triazole N,N-bidentate ligand (2-(1-((pyridine-2-yl)methyl)-1H-1,2,3-triazol-4-yl)ethyl sodium sulfate, `ligand 1.Na) in methanol to form [Co(ligand 1)2(H2O)2].4H2O as a microcrystalline solid. In this context, ligand 1.Na was first synthesized by the cycloaddition reaction of 2-(azidomethyl)pyridine and sodium 3-butyn-1-sulfate in 4:1 tert-BuOH/water solvents in presence of Cu(AcO)2H2O (10-15 mol %) as catalyst. The ligand 1.Na was white solid, absorbed moisture at open air, soluble in methanol and DMSO and characterized by elemental analysis, ESI-MS spectrum in the negative mode, 1H NMR and 13C NMR spectroscopy. In the 1H NMR spectrum of ligand 1.Na in CD3OD, a characteristic triazole strong singlet peak appeared at 7.97 ppm, a remarkable shift of δ value for CH2 proton of 2-(azidomethyl)pyridine was observed. In the 13C NMR spectrum, the triazole carbon resonates at 137.90 ppm. The prepared complex was characterized by physical data, FT-IR, ESI-MS and elemental analysis. The light pink crystals are fairly stable at open atmosphere even if they slowly loose the lattice solvent. The ESI-MS spectrum of [Co(ligand 1)2(H2O)2].4H2O indicates the species [Co(ligand 1.Na)(ligand 1)]+ and [Co(ligand 1.Na)]+ which corresponds to the m/z value at 648.6 and 402.6 respectively. Based on the observed data, octahedral geometry of the synthesized complex was suggested.
Keywords
Pyridyl Ligand, Octahedral Geometry, Cobalt(II) Perchlorate Hexahydrate, 3-butyn-1-sulfate
Reference
| [01] | Rostovtsev, V. V.; Green, L. G.; Fokin, V. V.; Sharpless, K. B.; Angewandte Chemie International Edition. 2002, 41, 2596. |
| [02] | Himo, F.; Lovell, T.; Hilgraf, R.; Rostovtsev, V. V.; Noodleman, L.; Sharpless, K. B.; Fokin, V. V.; Journal of American Chemical Society. 2005, 127, 210. |
| [03] | Tornøe, C. W.; Christensen, C.; Meldal, M.; Journal of Organic Chemistry. 2002, 67, 3057. |
| [04] | Struthers, H.; Mindt, T. L.; Schibli, R.; Dalton Transactions. 2010, 39, 675. |
| [05] | Urankar, D.; Pinter, B.; Pevec, A.; Proft, F. D.; Turel, J. Kosmrlj, I.; Inorganic Chemistry. 2010, 49, 4820. |
| [06] | Bratsos, I.; Urankar, D.; Zangrando, E.; Kalou, P. G.; Kosmrlj, J.; Alessio, E.; Turel, I.; Dalton Transactions. 2011, 40, 5188. |
| [07] | Detz, R. J.; Heras, S. A.; de Gelder, R.; van Leeuwen, P. W. N. M.; Hiemstra, H.; Reek, J. N. H.; van Maarseveen, J. H.; Organic Letters. 2006, 8, 3227. |
| [08] | Amadio, E.; Scrivanti, A.; Chessa, G.; Matteoli, U.; Beghetto, V.; Bertoldini, M.; Rancan, M.; Dolmella, A.; Venzo, A.; Bertani, R.; Journal of Organometallic Chemistry. 2012, 716, 193. |
| [09] | Amadio, E.; Bertoldini, M.; Scrivanti, A.; Chessa, G.; Beghetto, V.; Matteoli, U.; Bertani, R.; Dolmella, A.; Inorganica Chimica Acta. 2011, 370, 388. |
| [10] | Dio, S. D.; Marchetti, M.; Paganelli, S.; Piccolo, O.; Applied Catalysis A: General. 2011, 399, 205-210. |
| [11] | Fukuoka, A.; Kosugi, W.; Morishita, F.; Hirano, M.; McCaffrey, L.; Henderson, W.; Komiya, S.; Chemical Communications. 1999, 489. |
| [12] | Amadio, E.; Scrivanti, A.; Beghetto, V.; Bertoldini, M.; Alam Md. M.; Matteoli, U.; RSC Advances. 2013, 3, 21636. |
| [13] | Golas, P. L.; Tsarevsky, N. V.; Macromolecular Rapid Communications. 2008, 29, 1167. |
| [14] | Herves, A. S.; Megia E. F.; Riguera, R.; Chemical Communications. 2008, 3136. |
| [15] | Brotherton, W. S.; Michaels, H. A.; Simmons, J. T.; Zhu, L.; Organic Letters. 2009, 11, 4954. |
| [16] | Barluenga, J.; Valdés, C.; Beltrán, G.; Escribano, M.; Aznar, F.; Angewandte Chemie International Edition. 2006, 45, 6893. |
| [17] | Armarego, W. L. F.; Perrin, D. D.; Purification of Laboratory Chemicals, 3rd edn., Pergamon Press, 1988. |
