Synthesis and Crystal Structure of the First Example of a Tris-Chelated Co(II) Complex Based on Oxamide Dioxime Ligand

Gouet Bebga¹, Emmanuel N. Nfor², Yves A. Mbiangué³, Patrick L. Djonwouo⁴, Justin Nenwa^4*

¹Department of Chemistry, Higher Teachers Training College, University of Yaounde 1, Yaounde, Cameroon.
²Department of Chemistry, University of Buea, Buea, Cameroon.
³Department of Chemistry, Higher Teachers Training College, University of Maroua, Maroua, Cameroon.
⁴Department of Inorganic Chemistry, Coordination Chemistry Laboratory, University of Yaounde 1, Yaounde, Cameroon.

DOI: 10.4236/csta.2015.42002                

Abstract

A new cobalt(II) complex, [Co(H₂ oxado)₃ ]C₂ O₄ H₂ oxado·2H₂ O (H₂ oxado = oxamide dioxime), has been synthesized in aqueous solution and characterized by elemental analysis and single crystal X-ray structure determination. The complex crystallizes in the triclinic space group P-1, with the parameters a = 9.46(4), b = 11.84(5), c = 12. 81(5) Å, α = 104.94(6), β = 99.29(5), γ = 106.73(5), V = 1284(9) ų, Z = 2. The central cobalt(II) cation is pseudo-octahedrally coordinated by six imino N atoms of the neutral oxamide dioxime ligand. In the solid state, each of the following bricks, namely the cationic complexes, the oxalate dianions as well as the oxamide dioxime crystallization molecules, pile up parallel to the a axis. The bulk structure is consolidated by an extended three-dimensional network of hydrogen bridgings—that link the ionic partners, oxamide dioxime and water molecules to one another—and by coulombic interactions.

Keywords

Crystal Structure, Cobalt(II) Complex, Oxamide Dioxime, Oxalate, Hydrogen Bridging

Conflicts of Interest

The authors declare no conflicts of interest.

References

[1]	Coronado, E., Forment-Aliaga, A., Galán-Mascarós, J.R., Giménez-Saiz, C., Gómez-García, C.J., Martinéz-Ferrero, E., Nuez, A. and Romero, F.M. (2003) Multifunctional Molecular Materials. Solid State Sciences, 5, 917–924. http://dx.doi.org/10.1016/S1293-2558(03)00116-X
[2]	Bein, T. and Stucky, G.D. (1996) Preface to the Special Issue. Chemistry of Materials, 8, 1569-1570. http://dx.doi.org/10.1021/cm960902s
[3]	Moulton, B. and Zaworotko, M.J. (2001) From Molecules to Crystal Engineering: Supramolecular Isomerism and Po- lymorphism in Network Solids. Chemical Reviews, 101, 1629-1658. http://dx.doi.org/10.1021/cr9900432
[4]	Rao, C.N.R. and Nath, M. (2003) Inorganic Nanotubes. Dalton Transactions, No. 1, 1-24. http://dx.doi.org/10.1039/b208990b
[5]	Bélombé, M.M., Nenwa, J., Mbiangué, Y.A., Evina-Nnanga, G., Mbomékallé, I.M., Hey-Hawkins, E., Lnnecke, 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, No. 11, 2117-2118. http://dx.doi.org/10.1039/b302489j
[6]	Bekaroglu,., Sarisaban, S., Koray, A.R., Nuber, B., Weidenhammer, K., Weiss, J. and Ziegler, M.L. (1978) The Crystal Structure of Tris(oxamide oxime)cobalt(III) Trichloride, [Co(C2H6N4O2)3]Cl3. Acta Crystallographica Section. B, 34, 3591-3593. http://dx.doi.org/10.1107/S0567740878011668
[7]	Bélombé, M.M., Jokwi, I., Ngameni, E., Roux, R. and Nuber, B. (1993) Transition Metal Complexes of Oxamide Oxime, 1. Synthesis and X-Ray Crystal Structure of Tris(oxamide oxime-N1,N1')cobalt(III) Triiodide [Co(H2oxao)3]I3. Zeitschrift für Naturforschung Teil B, 48, 1719-1722.
[8]	Bélombé, M.M., Nenwa, J., Bebga, G., Fokwa, B.P.T. and Dronskowski, R. (2007) Bis[tris(oxamide dioxime-κ2N,N') cobalt(III)] Oxalate bis(sulfate) Dodecahydrate. Acta Crystallographica Section E, 63, m2037-m2038. http://dx.doi.org/10.1107/S1600536807031169
[9]	Bélombé, M.M., Nenwa, J., Mbiangué, Y.A., Majoumo, F., Lnnecke, 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, No. 23, 4519-4525. http://dx.doi.org/10.1039/b818793b
[10]	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]23H2O}. Science Jet, 1, 1-9.
[11]	Ephraim, J. (1889) Zur Kenntniss des Rubeanwasserstoffs. Berichte der Deutschen Chemischen Gesellschaft, 22, 2305-2306. http://dx.doi.org/10.1002/cber.188902202108
[12]	Bailar, J.C. and Jones, E.M. (1939) Tris(oxalato) Salts. Inorganic Syntheses, 1, 35-38. http://dx.doi.org/10.1002/9780470132326.ch13
[13]	(2003) SMART & SAINT Software Reference Manual, Version 6.45. Bruker Analytical X-Ray Systems, Inc., Madison.
[14]	Sheldrick, G.M., SADABS, Version 2.05 (2002) A Software for Empirical Absorption Correction. University of Gottingen, Gottingen.
[15]	Sheldrick, G.M., SHELXL97 (1997) Program for Crystal Structure Refinement. University of Gottingen, Gottingen.
[16]	Endres, H., Genc, N. and Nothe, D. (1983) The Catena Structure and EPR Properties of Bis(oxamide oximato)copper(II) Oxamide oxime, [Cu(C2H5N4O2)2].C2H6N4O2. Acta Crystallographica Section C, 39, 701-703. http://dx.doi.org/10.1107/s0108270183005971