TY - JOUR
T1 - Coordination of Zn II, Cd II, and Hg II by 2-pyridineformamide-3-piperidyl-thiosemicarbazone
AU - Castiñeiras, Alfonso
AU - García, Isabel
AU - Bermejo, Elena
AU - Ketcham, Karen A.
AU - West, Douglas X.
AU - El-Sawaf, Ayman K.
PY - 2002
Y1 - 2002
N2 - 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.
AB - 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.
KW - Cadmium
KW - Mercury
KW - Pyridine-formamide thiosemicarbazones
KW - Semicarbazones
KW - Zinc
UR - https://www.scopus.com/pages/publications/0036002223
U2 - 10.1002/1521-3749(200202)628:2<492::AID-ZAAC492>3.0.CO;2-V
DO - 10.1002/1521-3749(200202)628:2<492::AID-ZAAC492>3.0.CO;2-V
M3 - Article
AN - SCOPUS:0036002223
SN - 0044-2313
VL - 628
SP - 492
EP - 504
JO - Zeitschrift fur Anorganische und Allgemeine Chemie
JF - Zeitschrift fur Anorganische und Allgemeine Chemie
IS - 2
ER -