Synthesis, Characterization and Crystal Structure of Bis[4-Methyl-1-{1-(Pyridin-2-Yl)Ethylidene} Thiosemicarbazide-Κ3s,N,N]Zinc(II)
Gorgui Awa Seck
Department of Chemistry, University Cheikh Anta Diop, Dakar, 10700, Senegal.
Mamour Sarr
Department of Chemistry, University Cheikh Anta Diop, Dakar, 10700, Senegal.
Mbosse Ndiaye Gueye
Department of Chemistry, University Cheikh Anta Diop, Dakar, 10700, Senegal.
Marc Lenertz
Institut de Physique et Chimie des Matériaux de Strasbourg, Université de Strasbourg, CNRS UMR 7504, 67034 Strasbourg Cedex 2, France.
Emilie Delahaye
Institut de Physique et Chimie des Matériaux de Strasbourg, Université de Strasbourg, CNRS UMR 7504, 67034 Strasbourg Cedex 2, France.
Julia Mouton
Ecole Polytechnique Féminine (EPF), 21 Boulevard Berthelot, 34000 Montpellier, France.
Mayoro Diop *
Department of Chemistry, University Cheikh Anta Diop, Dakar, 10700, Senegal.
Mohamed Lamine Gaye
Department of Chemistry, University Cheikh Anta Diop, Dakar, 10700, Senegal.
*Author to whom correspondence should be addressed.
Abstract
Schiff base ligand (4-methyl-1-(1-(pyridin-2-yl)ethylidene)thiosemicarbazide (H2L) was synthesized via condensation of 2-acetylpyridine and 4-methyl-3-thiosemicarbazide in ethanol. The Zn(II) complex was obtained from 2:1 (H2L/Zn(OAc)2.2H2O) molar ratio reaction, yielding a neutral compound formulated as [Zn(HL)2]. Elemental analysis, 1H and 13C NMR, conductance measurements and FT-IR spectroscopy were used for the characterization of the ligand and the complex. The complex is non-electrolyte in DMF solution. The structure of the complex was determined by single crystal X-ray diffraction study. Two ligand coordinated the Zn(II) ion. Each of the azomethine ligand was coordinated to Zn(II) ion through one azomethine nitrogen atom, one pyridine nitrogen atom and one sulfur atom, yielding an octahedral Zn(II) complex. The compound crystallizes in the triclinic space group P-1 with unit cell dimensions a = 8.551 (6) Å, b = 10.948 (5) Å, c = 12.060 (4) Å, a = 91.66 (3)°, b = 100.03 (5)°, g = 109.92 (3)°, V = 1040.5 (10) Å3, Z = 2, R1 = 0.066 and wR2 = 0.158. The Zn(II) cation in N4S2 inner is situated in a distorted octahedral environment.
Keywords: FTIR, zinc, acetylpyridine, 4N-methylthiosemicarbazone, octahedral, x-ray diffraction