Synthesis, structural characterization and thermal analysis of Co(II) monomer based on 2,3-pyridinedicarboxylic acid
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Chimie. Cristalografie. Mineralogie (2025)
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COŞCODAN, Elena, MELNIK, E., PETUHOV, Oleg, CHIŞCA, Diana. Synthesis, structural characterization and thermal analysis of Co(II) monomer based on 2,3-pyridinedicarboxylic acid. In: Ecological and environmental chemistry : - 2022, Ed. 7, 3-4 martie 2022, Chișinău. Chisinau: Centrul Editorial-Poligrafic al USM, 2022, Ediția 7, Vol.1, pp. 72-73. ISBN 978-9975-159-07-4.. 10.19261/eec.2022.v1
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Ecological and environmental chemistry
Ediția 7, Vol.1, 2022
Conferința "Ecological and environmental chemistry 2022"
7, Chișinău, Moldova, 3-4 martie 2022

Synthesis, structural characterization and thermal analysis of Co(II) monomer based on 2,3-pyridinedicarboxylic acid

CZU: 541.64:547.82

Pag. 72-73

Coşcodan Elena1, Melnik E.12, Petuhov Oleg3, Chişca Diana12
 
1 Tiraspol State University,
2 Institute of Applied Physics,
3 Institute of Chemistry
 
Proiecte:
 
Disponibil în IBN: 4 martie 2022


Rezumat

Dicarboxylate ligands are widely used to assemble supramolecular networks organized by coordination bonds, hydrogen bonds and π–π stacking interactions. Due to the sets of N- and O-donors, pyridindicarboxylic ligands can contrast versatile structural motifs, which eventually aggregate to generate various supramolecular architectures with exciting properties. The design and synthesis of metal coordination polymers can be influenced by many factors, especially by the nature of metal ions, anions, and ligands. As one of the dicarboxylate ligands, 2,3-pyridinedicarboxylic acid often acts as a bidentate chelating ligand through the nitrogen atom and one oxygen atom of the carboxylic group to form a discrete complex or 2-D layer. Here we report the preparation of new compound [Co(2,3-pyd)2(H2O)2]·Me-DMF, which was analyzed by X-ray diffraction, IR spectroscopy and thermogravimetric analysis. This compound was obtained as a result of interaction between Co(NO3)2·6H2O and 2,3-pyridinedicarboxylic acid (2,3-pyd) in CH3CN and DMF solvents. The compound crystallizes in triclinic P-1 space group: a =7.5963(5), b = 9.3731(7), c = 9.4277(7) Å, α= 88.599(6), β = 74.846(6), γ = 83.113(6)°, V = 643.23(8) Å3 and represents a mononuclear Co(II) complex where 2,3-pyd works as a bidentate ligand (Figure). The Co atom is coordinated by N and O atoms from two 2,3-pyd ligands and O atoms from two water molecules, forming a distorted N2O4 octahedral coordination environment. In the crystal, the monomers are united via O−H···O hydrogen bonds forming supramolecular chains. Infrared spectroscopy showed the presence of organic ligands used in the synthesis. The band at 3319 cm-1 is attributed to the hydrogen-bonded O–H stretching vibration. The absorption bands at 2934 and 2880 cm-1 correspond to the asymmetric and symmetric aromatic C–H stretching vibrations respectively. The C=O stretching vibration of 2,3-pyridinedicarboxylic acid is observed at 1659 cm-1. The COO– asymmetric and symmetric stretching vibrations appear at 1562 and 1388 cm-1 respectively. The difference Δν = νas(COO-)- νs(COO-) is equal to 174 cm-1, which tells us about the bidentate mode of coordination of the pyridinedicarboxylate anion in the compound. The aromatic C–C stretching vibrations are exhibited at 1477 and 1505 cm-1. The C–H bending vibration is observed at 755 cm-1 and the C–N stretching vibration appears at 871 cm-1. The thermal analysis was performed in inert atmosphere. The first stage occurs in the range of 95-158 oC accompanied by an endothermic process due to the elimination of water molecules. The second step starts up at 239 oC and ends at 268 oC with a mass loss of 22.76 % (theor. 22.56%), that is assigned to the loss of the Me-DMF molecules. In the next step that begins at 351 oC, decomposition of the carboxylate ligand occurs. The final residue is a cobalt oxide.