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Synthesis, Crystal Structure and Thermal Behavior of a 3-D Barium(II)/Iron(III)-Oxalate Polymer

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DOI: 10.4236/ojic.2014.42004    3,257 Downloads   5,228 Views   Citations


Reaction of Ba(NO3)2 with Fe(NO3)9H2O and H2C2O2H2O in aqueous medium readily affords, in high yield, the bimetallic complex polymer of chemical composition {Ba6(H2O)17[Fe(C2O4)3]4}·7H2O (1), consistent with the expected ratio of 3BaII vs. 2FeIII. Compound 1 was fully characterized by elemental and thermal analyses, vibrational FTIR spectroscopy, and by single crystal X-ray structure determination. The bulk structure of 1 is a 3-D metal-organic framework held together by intermetallic linkages across oxalate and aqua oxygen bridgings. Thermal analyses of 1 show significant weight losses corresponding to water molecules (lattice and coordinated), followed by the decomposition of the network.

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Makon Ma Houga, N. , S. Dolinar, B. , Nenwa, J. and Bebga, G. (2014) Synthesis, Crystal Structure and Thermal Behavior of a 3-D Barium(II)/Iron(III)-Oxalate Polymer. Open Journal of Inorganic Chemistry, 4, 21-29. doi: 10.4236/ojic.2014.42004.


[1] Moulton, B. and Zaworotko, M.J. (2001) From Molecules to Crystal Engineering: Supramolecular Isomerism and Polymorphism in Network Solids. Chemical Reviews, 101, 1629-1658.
[2] Rao, C.N.R. and Nath, H. (2003) Inorganic Nanotubes. Dalton Transactions, 1-24.
[3] Andrés, R., Brissard, M., Gruselle, M., Train, C., Vaissermann, J., Malézieux, B., Jamet, J.P. and Verdaguer, M. (2001) Rational Design of Three-Dimensional (3D) Optically Active Molecule-Based Magnets: Synthesis, Structure, Optical and Magnetic Properties of {[Ru(bpy)3]2+, , [MnIICrIII(ox)3]-}n and {[Ru(bpy)2ppy]+, [MIICrIII(ox)3]-}n, with MII = MnII, NiII. X-Ray Structure of {[ΔRu(bpy)3]2+, , [ΔMnIIΔCrIII(ox)3]-}n and {[ΛRu(bpy)2ppy]+,
[ΛMnIIΛCrIII(ox)3]-}n. Inorganic Chemistry, 40, 4633-4640.
[4] Coronado, E., Galán-Mascarós, J.R., Gómez-García, C.J. and Martínez-Agudo J.M. (2001) Molecule-Based Magnets Formed by Bimetallic Three-Dimensional Oxalate Networks and Chiral Tris(bipyridyl) Complex Cations. The Series [ZII(bpy)3][ClO4][MIICrIII(ox)3] (ZII = Ru, Fe, Co, and Ni; MII = Mn, Fe, Co, Ni, Cu, and Zn; ox = Oxalate Dianion). Inorganic Chemistry, 40, 113-120.
[5] Vaidhyanathan, R., Natarajan, S. and Rao, C.N.R. (2001) Three-Dimensional Yttrium Oxalates Possessing Large Channels. Chemistry of Materials, 13, 185-191.
[6] Lacroix, P.G., Malfant, I., Bénard, S., Yu, P., Rivière, E. and Nakatani K. (2001) Hybrid Molecular-Based Magnets Containing Organic NLO Chromophores: A Search toward an Interplay between Magnetic and NLO Behavior. Chemistry of Materials, 13, 441-449.
[7] Ferlay, S., Mallah, T., Ouahès, R., Veillet, P. and Verdaguer, M. (1995) A Room-Temperature Organometallic Magnet Based on Prussian Blue. Nature, 378, 701-703.
[8] Verdaguer, M. (1996) Molecular Electronics Emerges from Molecular Magnetism. Science, 272, 698-699.
[9] Hua, X., Larsson, K., Neal, T.J., Wyllie, G.R.A., Shang, M. and Lappin, A.G. (2001) Structure and Magnetic Properties of [Cr(en)2(ox)][Cr(en)(ox)2] 2H2O, Δ-[Cr(en)3]Δ-[Cr(ox)3] and Δ-[Co(en)3]Δ-[Cr(ox)3]. Inorganic Chemistry Communications, 4, 635-639.
[10] Decurtins, S., Schmalle, H.W., Schneuwly, P., Ensling, J. and Guetlich, P. (1994) A Concept for the Synthesis of 3-Dimensional Homo- and Bimetallic Oxalate-Bridged Networks [M2(ox)3]n. Structural, Moessbauer, and Magnetic Studies in the Field of Molecular-Based Magnets. Journal of American Chemical Society, 116, 9521-9528.
[11] Decurtins, S., Schmalle, H.W., Pellaux, R., Schneuwly, P. and Hauser, A. (1996) Chiral, Three-Dimensional Supramolecular Compounds: Homo- and Bimetallic Oxalate- and 1,2-Dithiooxalate-Bridged Networks. A Structural and Photophysical Study. Inorganic Chemistry, 35, 1451-1460.
[12] Bélombé, M.M., Nenwa, J., Mbiangué, Y.A., Evina-Nnanga, G., Mbomékallé, I.M., Hey-Hawkins, E., Lonnecke, P. and Majoumo, F. (2003) Unusual Aquation of Ba2+ Ions in the Solid State: Synthesis and X-Ray Structural and Spectroscopic Characterization of the Novel Polymeric Complex Salt of Empirical Formula {Ba6(H2O)17[Cr(ox)3]4}·7H2O (ox = Oxalate Dianion). Dalton Transactions, 2117-2118.
[13] Bélombé, M.M., Nenwa, J., Mbiangué, Y.A., Gouet, B., Majoumo, F., Hey-Hawkins, E. and Lonnecke, P. (2009) Water-Filled Pseudo-Nanotubes in Ag11.60H0.40[Cr(C2O4)3]4·15H2O: Synthesis, Characterization and X-Ray Structure. Inorganica Chimica Acta, 362, 1-4.
[14] Bélombé, M.M., Nenwa, J., Mbiangué, Y.A., Majoumo, F., Lonnecke, P. and Hey-Hawkins, E. (2009) Hydrogen-Bonded Pillars of Alternating Chiral Complex Cations and Anions: 1. Synthesis, Characterization, X-Ray Structure and Thermal Stability of catena-{[Co(H2oxado)3][Cr(C2O4)3]·5H2O} and of Its Precursor (H3oxado)[Co(H2oxado)3](SO4)2·2H2O. Dalton Transactions, 4519-4525.
[15] Mbiangué, Y.A., Nenwa, J., Bélombé, M.M., Ngoune, J. and álvarez, E. (2012) Hydrogen-Bonded Pillars of Alternating Chiral Complex Cations and Anions: 2. Synthesis, Characterization and X-Ray Structure of Isomorphous catena-{(H3O)[K(H2O)3]@[Ni(H2oxado)3]2[Cr(C2O4)3]2·3H2O} and catena-{(H3O)[Li(H2O)3]@[Ni(H2oxado)3]2-
[Cr(C2O4)3]2·3H2O}. Science Jet, 1, 1-9.
[16] Neo, K.E., Ong, Y.Y., Huynh, H.V. and Andy-Hor, T.S. (2006) A Single-Molecular Pathway from Heterometallic MM’ (M = BaII, MnII; M’ = CrIII) Oxalato Complexes to Intermetallic Composite Oxides. Journal of Materials Chemistry, 17, 1002-1006.
[17] APEX-II (Version 2013. 2-0), SADABS (Version 2012-1), SAINT (Version 8.30C). (2007-2013) Bruker AXS Inc., Madison.
[18] Guzei, I.A. (2013) Internal Laboratory Computer Programs Gn.
[19] Bélombé, M.M., Nenwa, J., Tene, T.O. and Fokwa, B.P.T. (2010) Synthesis, X-Ray Structure and Thermal Behavior of Isomorphous Silver-Deficient Channel Lattice Frameworks with General Formula [(Ag0.25/M0.25)(H2O)]@ [Ag2M(C2O4)3]·4H2O (M = CoIII, CrIII). Global Journal of Inorganic Chemistry, 1, 34-41.
[20] Saritha, A., Raju, B., Ramachary, M., Raghavaiah, P. and Hussain, K.A. (2012) Synthesis, Crystal Structure and Characterization of Chiral, Three-Dimensional Anhydrous Potassium Tris(Oxalate)Ferrate(III). Physica B, 407, 4208-4213.
[21] Kaziro, R., Hambly, T.W., Binstead, R.A. and Beattie, J.K. (1989) Potassium Tris(oxalato)ruthenate(III). Inorganica Chimica Acta, 164, 85-91.

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