
Canadian Journal of Chemistry p. 2095 - 2105 (1996)
Update date:2022-08-03
Topics:
Chopra
Damude
Dean
Vittal
Reactions between Sn(E′Ph)n and the bis(pyridine) dichalcogenides 2,2′-(C5H4NE)2 have been studied using multinuclear (77Se, 119Sn, 125Te) magnetric resonance. In this way the occurrence of the pyridine-2-chalcogenate complexes Sn(E′Ph)4-x(Epy)x has been demonstrated. The pattern of 119Sn NMR chemical shifts for Sn(E′Ph)4-x(Sepy)x is consistent with bidentate bonding for the pySe- ligand when x = 1 and 2. The pyTe- ligand is probably bidentate also in all four complexes containing this ligand. As part of the NMR analysis, 77Se and (or) 125Te NMR data were obtained for py2Te2 and for the new mixed dichalcogenides PhE′ER, which were produced in the systems Ph2E′2:R2E4. The complex Sn(SPh)2(Sepy)2 (1) was isolated pure and its structure determined by the single crystal X-diffraction technique. The structure confirms that the PySe- ligand behaves in a chelating manner. The molecule Sn(SPh)2(2-Se-C5H4N-N,Se)2 has a distorted octahedral structure with the PhS- ligands in cis positions and the two Se donor atoms in trans positions. En route to 1, the yellow crystalline compound Sn(SPh)1.85(2-Se-C5H4N)2.15 (2) was isolated. This was shown by 119Sn NMR spectroscopy to contain both Sn(2-Se-C5H4N)2 and Sn(2-Se-C5H4N)3(SPh). The crystal and molecular structure of 2 was determined by single crystal X-ray diffraction techniques.
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