195Pt-NMR-spektroskopischer Nachweis gemischter Hexahalogenodiplatinate(II), [Pt2ClnBr6 − n]2−, n = 0 – 6 |
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Authors: | J. Duvigneau G. Peters W. Preetz |
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Abstract: | 195Pt NMR Spectroscopic Evidence of Mixed Hexahalogenodiplatinates(II), [Pt2ClnBr6 ? n]2?, n = 0 – 6 The complete system of the mixed complex ions [195Pt2ClnBr6 – n]2?, n = 0 – 6, is formed by stirring a suspension of the tetrabutylammonium salt(TBA)2[195PtCl4] in an aqueous solution of KBr at 80°C. The mixture recrystallized from acetone/diethyl ether contains the 24 possible species, 12 with two equivalent 195Pt atoms resulting in 12 singlets and 12 with inequivalent 195Pt atoms resulting in 24 dublets. The expected 60 signals are really observed in the high resolution 1D-195Pt-nmr spectrum. Using characteristic increments of chemical shifts, differentiating 2J(195Pt ? 195Pt) coupling constants and a 2D-195Pt/195Pt-COSY spectrum the complete and unambiguous assignment of all resonances is achieved. The presence of all components including the geometric isomers and their distribution derived from measured intensities reveal the statistical formation. |
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Keywords: | Binuclear mixed-ligand platinum complexes preparation 1D- and 2D-195Pt nmr chemical shift increments statistical evaluation |
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