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Synthesis, Structural Characterization and Spectroscopic Properties of [Pt(bddn)]Cl2 · 3.5H2O (bddn = 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane)

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Abstract

The reaction of the potentially tetradentate ligand 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane (bddn) with [PtCl2(CH3CN)2] yields a mixture of complexes, where the ligand acts as bidentate SS, or tetradentate 2NS or NSSN. This mixture of complexes SS, 2NS, and NSSN was crystallized with dichloromethane/n-pentane (1:1) and crystals of [Pt(bddn)]Cl2 (isomer NSSN) were obtained. The complex has been characterized by elemental analyses, mass spectrometry, conductivity, IR, 1H, 13C{1H}, 1H{195Pt}, 195Pt{1H}NMR, HSQC and NOESY spectroscopies, and X-ray diffraction. Compound [PtCl2(bddn)] · 3.5H2O crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 15.430(7) Å, b = 17.405(4) Å, c = 18.887(7) Å, β = 91.24(2)°, V = 5071(3) Å3, Z = 4, R 1 = 0.0354, wR2 = 0.1034. This compound consist of discrete cations [Pt(bddn)]2+, Cl anions and water molecules of crystallization. The platinum(II) is tetracoordinated by two azine nitrogen atoms and two sulfur atoms of the thioether-pyrazole ligand, in a distorted square planar geometry.

Graphical Abstract

Synthesis, Structural Characterization and Spectroscopic Properties of [Pt(bddn)]Cl 2  · 3.5H 2 O (bddn = 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane)

Antonio de Leon, Josefina Pons*, Jordi García-Antón, Xavier Solans, Mercè Font-Bardia, Josep Ros*

Reaction of the ligand 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane (bddn) with [PtCl2(CH3CN)2], yields a mixture of complexes. The mixture was crystallized with dichloromethane/pentane (1:1) and crystals of [Pt(bddn)]Cl2 · 3.5 H2O was obtained.

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Acknowledgement

Support by the Spanish Ministerio de Educación y Cultura (project CTQ2007-63913 BQU) is gratefully acknowledged.

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Correspondence to Josefina Pons.

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de Leon, A., Pons, J., García-Antón, J. et al. Synthesis, Structural Characterization and Spectroscopic Properties of [Pt(bddn)]Cl2 · 3.5H2O (bddn = 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane). J Chem Crystallogr 37, 801–805 (2007). https://doi.org/10.1007/s10870-007-9251-4

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