Structural Analysis of Powder Tris(phenanthroline)

The powder complex of tris(phenanthroline)nickel(II) trifluoroacetate has been synthesized by interaction of the corresponding nitrate salt in an aqueous solution and slightly excess of 1,10-phenanthroline in water/ethanol, whereupon the precipitate was produced on addition of an excess of saturated sodium trifluoroacetate solution while reducing the solvent. AAS measurement showed the content of metal to be 6.43 % being relatively close to the corresponding theoretical value of 6.60 % masss in [Ni(phen)3](CF3COO)2.3.5H2O. Moreover, the TGA confirmed the lost of 6.943% mass of complex corresponding to 3.43 H2O. The analysis of conductance producing the charge ratio of cation by anion to be 2:1, clearly fonfirms the formula. The magnetic moment, μeff, of this complex which was to be 3.19-3.31 BM, indicates that the complex is paramagnetic corresponding to two unpaired electrons which is clearly higher than the spin only value (2.87 BM) due to the spin-orbit coupling. UV-Vis spectrum ...