Journal of the Serbian Chemical Society (May 2003)
Transition metal complexes with thiosemicarbazide-based ligands. Part 45. Synthesis, crystal and molecular structure of [2,6-diacetylpyridine bis(S-methylisothiosemicarbazonato)]diazide-iron(III)
Abstract
The template reaction of a warm methanolic solution of FeCl3.6H2O, S-methylisothiosemicarbazidehydroiodide and 2,6-diacetylpyridine in the presence of LiOAc and NaN3 yielded the high-spin complex [Fe(HL)(N3)2], were HL is the monoanion of the ligand 2,6-diacetylpyridine bis(S-methylisothiosemicarbazone). X-Ray analysis of the complex showed its pentagonal-bipyramidal configuration, with pentadenate (N5) HL in the equatorial plane and two monodentate azide groups in the axial positions. Crystal data are: monoclinic, P21/c, a = 1.0263(2), b = 1.2525(2), c = 1.6660(3) nm, b = 98.94°, V = 2.1154 nm3, Z = 4, rx = 1.499 g cm-3, r0 = 1.48 g cm-3, F(000) = 984, m = 9.40 cm-3.