Structural analysis of powder complex of [Mn(phen)₃](CF₃SO₃)₂.6.5H₂O Available to Purchase

The objective of this work was to synthesise of complex containing manganese(II), 1,10-phenanthroline (phen) as ligand and a counter anion of trifluoromethanesulfonate (triflate). The complex was prepared by interaction of the corresponding nitrate salt and slightly excess of phenanthroline in aqueous solution, whereupon the precipitate was produced on addition of an excess of saturated potassium triflate solution when reducing the solvent. It was then characterised in terms of electrical conductivity, metal content, magnetic moment, electronic and infrared spectral properties, and powder XRD. The atomic absorption spectral data and the equivalent conductance suggest that the resulted complex was found to be ionic hydrated complex with the content of three ions per molecule, with an equivalent conductance in the range values of the three ionic standard, but much higher than the two ionic standard and much lower than the four ionic standard. The formula of [Mn(phen)₃](CF₃SO₃)₂.6,5H₂O was then proposed. The corresponding IR spectrum indicated the presence of typical function group of phenantroline and the triflate ion in the complex. The complex was found to be yellowish, and paramagnetic (μ_eff = 5.8-5.95 BM) corresponding to high spin Mn(II)-3d⁵. The electronic spectrum of [Mn(phen)₃]²⁺ revealed typical bands concentrated at ν₁ ∼ 13966 cm⁻¹, ν₂ ∼ 16474 cm⁻¹, ν₃ ∼ 19493 cm⁻¹, ν₄ ∼ 26325 cm⁻¹ as a shoulder, and ν₅ ∼ 30769 cm⁻¹. These bands might be respectively associated with the spin-forbidden transitions of ⁶A_1g → ⁴T_1g (G), ⁶A_1g → ⁴T_2g (G), ⁶A_1g → ⁴E_g, ⁴A_1g (G), ⁶A_1g → ⁴T_2g (D), and ⁶A_1g → ⁴E_g(D). The powder X-ray diffraction of the complex was then solved with Rietica-Le Bail method, and found to be structurally triclinic with space group of PI (lattice parameters, a = 12. 633 Ǻ; b = 17.062 Ǻ; c = 22.481 Ǻ; α = 106.876°; β = 110.901°; γ = 99.562°; V = 4130.4169 Ǻ³; R_p = 3.67; R_wp = 7.34; R_exp = 3.61) for the cationic complex.