Abstract
Sodium in dry methanol reduces 2-cyanopyridine in the presence of 3-piperidylthiosemicarbazide and produces 2-pyridine-formamide-3-piperidylthiosemicarbazone, HAmpip. Complexes with zinc(II), cadmium(II), and mercury(II) have been prepared and characterized by elemental analyses and spectroscopic techniques. In addition, the crystal structures of [Zn(Ampip) 2], [Zn(Ampip)(Oac)] 2, [Cd(HAmpip)Cl 2]·(CH 3) 2SO, [Cd(HAmpip)Br 2]·(CH 3) 2SO, [Cd(HAmpip)I 2]·(CH 3) 2SO, [Cd(Ampip) 2] and [Hg(HAmpip)Br 2]·(CH 3) 2SO have been solved. Coordination of the anionic and neutral thiosemicarbazone ligand is via the pyridyl nitrogen, imine nitrogen and thiolato/thione sulfur atom, respectively. In [Zn(Ampip)(OAc)] 2 one of the bridging acetato ligands has monodentate coordination and the other bridges in a bidentate manner. 113Cd NMR studies were carried out on the [Cd(HAmpip)X 2] (X = Cl, Br or I) and [Cd(Ampip)(OAc)] 2 complexes. The 113Cd chemical shifts are affected by the halogen and range from 411 to 301 ppm, and the spectrum of [Cd(Ampip)(OAc)] 2 shows two signals at 450 and 251 ppm. The 199Hg NMR spectrum of [Hg(HAmpip)Cl 2] also is discussed.
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