Popis: |
The ligand exchange reactions of ReCl4(PPh3)2, ReOCl3(PPh3)2 and NiCl2(PPh3)2 with acetylacetone thiobenzoylhydrazone have been studied. An unexpected template reaction at the ReO3+ core forming the new tetradentate triacidic ligand triacetylmethane bis(thiobenzoylhydrazone) will be described and discussed. The final products were characterized by elemental analysis, mass spectroscopy, 1H NMR, IR, UV-VIS spectroscopy and X-ray structural analysis. [Acetylacetone thiobenzoylhydrazonato(2-)]chloro-oxorthenium(V) was isolated as an intermediate. The crystal structures have been determined of [triacetylmethane bis(thiobenzoylhydrazonato) (3-)- S,S′,N,N′]oxorhenium(V) C21H19N4O2S2Re, monoclinic P2 1 /m, a = 7.451(1), B = 11.262(3), c = 12.639(4) A , β = 90.66(2)°, Z = 2, R 1 = 0.0445 , and [acetylacetone thiobenzoylhydrazonato(2-)]-triphenylphosphane-nickel(II) C30H27N2OSPNi, orthombic Pbca, a = 16.658(2), b = 14.725(2), c = 21.950(2) A , Z = 8, R 1 = 0.0283 . |