Synthesis, characterization and molecular structures of Cu(II) and Ba(II) fluorinated carboxylate complexes

Add time:10/01/2019    Source:sciencedirect.com

Various synthetic routes to Cu(II) and Ba fluorocarboylate derivatives as possible metal organic deposition (MOD) precursors of high Tc superconductors have been explored. The reactions between [Cu2(TFA)4]∞ or Cu2(TFA)4(MeOH)2 and [Ba(TFA)2]m (TFA = CF3CO2) with various O- and N-donor ligands give adducts such as Cu2(TFA)4L2 (L = THF, OHC2H4OiPr), Cu(TFA)2(pmdeta) (pmdeta = N,N,N′,N″,N″-pentamethyldiethylenetriamine) and Ba(TFA)2(mdeaH2)3 or Ba(TFA)2(teaH3)2 (mdeaH2 = N-methyldiethanolamine, teaH3 = triethanolamine). The TFA ligands on copper(II) are quite labile, giving the tetranuclear [Cu(μ,η2-TFA)(μ3,η2-OC2H4NMe2)]4 · 0.25THF carboxylatoalkoxide by reacting Cu2(TFA)4(MeOH)2 with dimethylaminoethanol. In contrast to the Cu–TFA derivatives, the perfluorobutyrate Cu2(PFB)4(THF)2 (PFB = O2CC3F7) is volatile and sublimes at 190 °C/2 × 10−4 Torr. Difluoroacetate derivatives Cu2(O2CCHF2)4(THF)2 and [Ba(O2CCHF2)2]m have also been prepared. In addition to elemental analysis, FT-IR, 1H NMR or ESR spectroscopies, some adducts have also been characterized by single crystal X-ray diffraction. Cu2(μ,η2-PFB)4(THF)2 and Cu2(μ,η2-TFA)4(η1-OHC2H4OiPr)2 show the usual paddle-wheel structure of the dinuclear Cu(II) carboxylate adducts. The barium derivative with N-methyldiethanolamine is the first example of an ionic barium trifluoroacetate derivative, all trifluoroacetates acting as counter ion.

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