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Copper(I) Derivative of Pyridine-3-carbaldehyde-N-ethylthiosemicarbazone and Triphenylphosphine—First Case of Crystal Structure Study

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Abstract

The synthesis and crystal structure of pyridine-3-carbaldehyde-N-ethylthiosemicarbazone (3-pytscH-NHEt) 1, and its CuI complex of stoichiometry, [CuCl(3-pytscH-NHEt)(PPh3)2] 2, studied using single crystal X-ray crystallography, are reported in this paper. Crystal data: 1, monoclinic, P21/n, a = 6.6322(3), b = 21.1200(8), c = 7.2989(3) Å; β = 91.883(4), T = 173(2), R factor = 0.0457; 2: triclinic, P-1, a = 19.3600(5), b = 20.6241(6), c = 23.8015(6) Å,α = 92.647(2), β = 104.388(2), γ = 114.377(3), R factor = 0.0662. The thio-ligand, as a neutral entity, is coordinating to Cu through its S donor atom in complex 2. It has exhibited an unusual feature of forming four independent molecules (A, B, C, D) in the unit cell, with minor differences in the bond angles / distances / torsion angles. The geometry of each molecule of 2 is distorted tetrahedral. Crystal packing, as well as Infrared, electronic absorption and proton NMR spectroscopic studies, are also reported. Copper compound 2 represents the first example of a structurally studied copper coordination compound of 3-pyridyl based thiosemicarbazones.

Graphical Abstract

Copper(I) chloride with pyridine-3-carbaldehyde-N-ethylthiosemicarbazone and PPh3 in CH3CN yielded a copper compound, 2 (Green-Cl, blue-N; aqua-Cu, orange-S, magneta-P).

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Funding

Financial assistance from the Council of Scientific and Industrial Research, New Delhi for SRF to Mani (Sanction letter No.: 09/254(0291)/2019-EMR-I) is gratefully acknowledged. TSL thanks The Guru Nanak Dev University for appointing Honorary Professor/ JPJ acknowledges the NSF–MRI program (Grant No. CHE-1039027) for funds to purchase the X-ray diffractometer.

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Author notes

  1. Jerry P. Jasinski Deceased on dated April 13, 2021.

Authors and Affiliations

  1. Department of Chemistry, Guru Nanak Dev University, Amritsar, 143 005, India

    Tarlok Singh Lobana, Mani Kaushal, Amandeep Kumar & Ritu Bala

  2. Departamento de Quimica Inorganica, Facultad de Farmacia, Universidad de Santiago, 15782, Santiago, Spain

    Isabel Garcia-Santos

  3. Department of Chemistry, Keene State College, Keene, NH, 03435-2001, USA

    Jerry P. Jasinski

  4. Department of Chemistry, Howard University, 525 College Street NW, Washington, DC, 20059, USA

    Ray J. Butcher

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  1. Tarlok Singh Lobana
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Correspondence to Tarlok Singh Lobana.

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Lobana, T.S., Kaushal, M., Kumar, A. et al. Copper(I) Derivative of Pyridine-3-carbaldehyde-N-ethylthiosemicarbazone and Triphenylphosphine—First Case of Crystal Structure Study. J Chem Crystallogr 52, 233–241 (2022). https://doi.org/10.1007/s10870-021-00911-3

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  • DOI: https://doi.org/10.1007/s10870-021-00911-3

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