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Synthesis and Crystal Structures of the Five-Coordinate Diorganotin(IV) Complex [Ph2Sn(L)]·DMF and its 5-Hydroxypyrazoline Ligand (H2L)

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Abstract

A five-coordinate diorganotin(IV) complex [Ph2Sn(L)]·DMF and its ligand, 5-hydroxy-3-methyl-5-phenyl-(N 4-phenylthiosemicarbazone)pyrazoline (H2L), were synthesized and characterized by elemental analysis, IR, NMR (1H, 13C) spectroscopies and X-ray crystallography techniques. Our studies revealed that H2L has formed as 5-hydroxy-4,5-dihydropyrazoline derivative in orthorhombic, Pbca space group with a = 15.4330(3) Å, b = 11.5427(2) Å, c = 18.1440(3) Å whereas [Ph2Sn(L)]·DMF crystallizes with two independent molecules (a and b) in the asymmetric unit in triclinic system, Pī space group with a = 9.2795(1) Å, b = 15.8315(2) Å, c = 19.9895(3) Å, α = 100.855(1)°, β = 92.985(1)°, γ = 102.243(1)°. In molecule a, the central Sn(IV) atom adopts a distorted tetragonal–pyramidal (TTP) geometry with N2 atom at apical position, while in molecule b the Sn(IV) occupies the centre of a trigonal-bipyramid (TBP) with N2 atom of the ONS-tridentate ligand and both Ph groups occupying equatorial positions. One molecule of DMF (crystallization solvent) helps in stabilizing the crystal structure.

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Acknowledgments

This work was sponsored by grants from CNPq and FINEP (CT-INFRA 0970/01). GFS also gratefully acknowledges the financial support of the Conselho Nacional de Desenvolvimento Científico e Tecnológico-CNPq (Edital Universal-2007, Processo 307412/2008-3).

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Authors and Affiliations

  1. Instituto de Química, Universidade de Brasília, 70919-970, Brasília, DF, Brazil

    Gerimário F. de Sousa, Daniel R. Marques & Inês S. Resck

  2. Instituto de Física, Universidade Federal de Goiás, 74001-970, Goiânia, GO, Brazil

    José R. Sabino

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  1. Gerimário F. de Sousa
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  2. Daniel R. Marques
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  3. Inês S. Resck
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  4. José R. Sabino
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Correspondence to Gerimário F. de Sousa.

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de Sousa, G.F., Marques, D.R., Resck, I.S. et al. Synthesis and Crystal Structures of the Five-Coordinate Diorganotin(IV) Complex [Ph2Sn(L)]·DMF and its 5-Hydroxypyrazoline Ligand (H2L). J Chem Crystallogr 41, 528–532 (2011). https://doi.org/10.1007/s10870-010-9914-4

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