Dihydroxycoumarin Schiff base synthesis and structure determination from powder diffraction data

•The new Schiff base could have wide application in many biological aspects.•The tetradentate Schiff-base could form stable complex with transition metals.•The complete powder diffraction study in conjunction with NMR, UV-VIX and FT-IR.•Problematic parts of refinement and structure determination are...

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Bibliographic Details
Published in:Journal of molecular structure 2013-11, Vol.1051, p.280-284
Main Authors: Rohlíček, Jan, Ketata, Imen, Ayed, Taïcir Ben, Hassen, Rached Ben
Format: Article
Language:English
Subjects:
Asymmetry
condensation
Crystal structure
Diffraction
Dihydroxycoumarine
Infrared
Molecular structure
Names
NMR spectroscopy
nuclear magnetic resonance spectroscopy
Powder diffraction
Schiff base
schiff bases
Structure solution
X-radiation
X-rays
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Summary:•The new Schiff base could have wide application in many biological aspects.•The tetradentate Schiff-base could form stable complex with transition metals.•The complete powder diffraction study in conjunction with NMR, UV-VIX and FT-IR.•Problematic parts of refinement and structure determination are explained.•Title compound is probably iminoenol-type. The titled compound with systematic name 4-hydroxy-3-((E)-1-(2-((E)-1-(4-hydroxy-2-oxo-2H-chromen-3-yl)ethylideneamino)ethylimino) ethyl)-2H-chromene-2-one is a new tetradentate (ONNO) Schiff-base which was synthesized by condensation of ethylenediamine and 3-acethyl 4-hydroxycoumarin. Its crystal structure was ab initio determined from laboratory X-ray powder diffraction data by using the direct space approach. The structure is monoclinic with space group P21/n and unit cell parameters a=10.4153(4)Å, b=12.8319(4)Å, c=7.48229(15)Å, β=98.892(3)Å, V=987.97(5)Å3. The asymmetric part of the structure contains one half of the centrosymmetric molecule. The obtained product was also characterized by infrared, UV–VIS and 1H NMR spectroscopy.
ISSN:0022-2860
1872-8014
DOI:10.1016/j.molstruc.2013.08.031