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Synthesis and X-ray powder diffraction characterization of tetra- and hexa-imidazole complexes of magnesium(II)

Published online by Cambridge University Press:  29 February 2012

Norberto Masciocchi
Affiliation:
Dipartimento di Scienze Chimiche e Ambientali, Università dell’Insubria, via Valleggio 11, 22100 Como, Italy
Luigi Garlaschelli
Affiliation:
Dipartimento di Chimica Inorganica, Metallorganica e Analitica, Università di Milano, via Venezian 21, 20133 Milano, Italy
Giulia Peli
Affiliation:
Dipartimento di Scienze Chimiche e Ambientali, Università dell’Insubria, via Valleggio 11, 22100 Como, Italy

Abstract

X-ray powder diffraction data for two ionic salts containing imidazole (Him) complexes of the magnesium(II) ion, [Mg(Him)4(H2O)2]Cl2 and [Mg(Him)6](NO3)2, are reported. Their crystal and molecular structures were determined by simulated annealing and full-profile Rietveld refinement methods. [Mg(Him)4(H2O)2]Cl2 was found to crystallize in the monoclinic system with space group C2/c, a=12.3980(3) Å, b=11.0234(2) Å, c=14.4691(3) Å, and β=107.024(1)°. [Mg(Him)6](NO3)2 crystallizes in the trigonal R-3 space group with a=b=12.4631(4) Å and c=14.9449(6)Å. Both species contain centrosymmetric complexes, and Mg is octahedrally coordinated by six imidazoles, as in [Mg(Him)6](NO3)2, or by four imidazoles and two water molecules, as in [Mg(Him)4(H2O)2]Cl2. Additional analytic, thermogravimetric, calorimetric, and spectroscopic characterizations were also performed.

Type
Technical Articles
Copyright
Copyright © Cambridge University Press 2008

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References

Cingolani, A., Galli, S., Masciocchi, N., Pandolfo, L., Pettinari, C., and Sironi, A. (2005). “Sorption-desorption behavior of bispyrazolato-copper(II) 1D coordination polymers,” J. Am. Chem. Soc.JACSAT10.1021/ja050856+ 127, 61446145.CrossRefGoogle ScholarPubMed
Galli, S., Masciocchi, N., Tagliabue, G., Sironi, A., Barea, E., Salas, J. M., Mendez, L., Domingo, M., Perez-Mendoza, M., and Navarro, J. A. R. (2008). “Polymorphic coordination networks responsive to CO2, moisture and thermal stimuli: porous cobalt(II) and zinc(II) fluoropyrimidinolates,” Chem.-Eur. J.CEUJED, in the press.Google ScholarPubMed
Gong, Y., Hu, C., Li, H., Pan, W., Niu, X., and Pu, Z. (2005). “Synthesis and crystal structure of two novel nickel (imidazole) complexes having hydrogen-bonded networks,” J. Mol. Struct.JMOSB4 740, 153158.CrossRefGoogle Scholar
Kahn, O. and Codjovi, E. (1996). “Iron(II)-1,2,4-triazole spin transition molecular materials,” Philos. Trans. R. Soc. London, Ser. APTRMAD10.1098/rsta.1996.0012 354, 359379.Google Scholar
Masciocchi, N., Ardizzoia, G. A., LaMonica, G., Maspero, A., and Sironi, A. (1998). “Unique formation of a crystal phase containing cyclic oligomers and helical polymers of the same monomeric fragment,” Angew. Chem., Int. Ed.ACIEF510.1002/(SICI)1521-3773(19981231)37:24<3366::AID-ANIE3366>3.0.CO;2-Z 37, 33663369.3.0.CO;2-Z>CrossRefGoogle ScholarPubMed
Masciocchi, N., Bruni, S., Cariati, E., Cariati, F., Galli, S., and Sironi, A. (2001). “Extended polymorphism in copper(II) imidazolate polymers: a spectroscopic and XRPD structural study,” Inorg. Chem.INOCAJ10.1021/ic010384+ 40, 58975905.CrossRefGoogle ScholarPubMed
Masciocchi, N., Galli, S., and Sironi, A. (2005). “X-ray powder diffraction characterization of polymeric metal diazolates,” Comments Inorg. Chem.COICDZ10.1080/02603590590920361 26, 137.CrossRefGoogle Scholar
Masciocchi, N., Galli, S., Sironi, A., Barea, E., Navarro, J. A. R., Salas, J. M., and Tabares, L. C. (2003). “Rich structural and magnetic chemistry of cobalt(II) pyrimidin-2-olate and pyrimidin-2-olate complexes. Synthesis, X-ray powder diffraction studies, and thermal behaviour,” Chem. Mater.CMATEX 15, 21532160.CrossRefGoogle Scholar
Maspero, A., Galli, S., Masciocchi, N., and Palmisano, G. (2008). “Facile preparation of polytopic azoles: synthesis, characterization, and X-ray powder diffraction studies of 1,4-bis(pyrazol-4-yl)- and 1,4-bis(tetrazol-5-yl)benzene,” Chem. Lett.CMLTAG 37, 956957.CrossRefGoogle Scholar
Navarro, J. A. R., Barea, E., Galindo, M. A., Salas, J. M., Romero, M. A., Quirós, M., Masciocchi, N., Galli, S., Sironi, A., and Lippert, B. (2005). “Soft functional polynuclear coordination compounds containing pyrimidine bridges,” J. Solid State Chem.JSSCBI 178, 24362451.CrossRefGoogle Scholar
Navarro, J. A. R., Barea, E., Salas, J. M., Masciocchi, N., Galli, S., Sironi, A., Ania, C. O., and Parra, J. B. (2006). “H2, N2, CO, and CO2 sorption properties of a series of robust sodalite-type microporous coordination polymers,” Inorg. Chem.INOCAJ 45, 23972399.CrossRefGoogle ScholarPubMed
Navarro, J. A. R., Barea, E., Salas, J. M., Masciocchi, N., Galli, S., Sironi, A., Ania, C. O., and Parra, J. B. (2007). “Borderline microporous-ultramicroporous palladium(II) coordination polymer networks. Effect of pore functionalisation on gas adsorption properties,” J. Mater. Chem.JMACEP 17, 19391946.CrossRefGoogle Scholar
Navarro, J. A. R., Barea, E., Rodriguez-Dieguez, A., Salas, J. M., Ania, C. O., Parra, J. B., Masciocchi, N., Galli, S., and Sironi, A. (2008). “Guest-induced modification of a magnetically active ultramicroporous, gismondine-like, copper(II) coordination network,” J. Am. Chem. Soc.JACSAT 130, 39783984.CrossRefGoogle ScholarPubMed
Shiu, K.-B., Yen, C.-H., Liao, F.-L., and Wang, S.-L. (2003). “trans-Diaquatetrakis(imidazole)nickel(II) dichloride,” Acta Crystallogr., Sect. E: Struct. Rep. OnlineACSEBH 59, m1189m1191.CrossRefGoogle Scholar
Xamena, F. X. L. I., Abad, A., Corma, A., and Garcia, H. (2007). “MOFs as catalysts: Activity, reusability and shape-selectivity of a Pd-containing MOF,” J. Catal.JCTLA5 250, 294298.Google Scholar