Premium
Coordination of Zn II , Cd II , and Hg II by 2‐Pyridineformamide‐3‐piperidyl‐thiosemicarbazone
Author(s) -
Castiñeiras Alfonso,
García Isabel,
Bermejo Elena,
Ketcham Karen A.,
West Douglas X.,
ElSawaf Ayman K.
Publication year - 2002
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/1521-3749(200202)628:2<492::aid-zaac492>3.0.co;2-v
Subject(s) - chemistry , denticity , semicarbazone , zinc , medicinal chemistry , ligand (biochemistry) , pyridine , imine , cadmium , halogen , methanol , crystal structure , inorganic chemistry , stereochemistry , crystallography , organic chemistry , biochemistry , alkyl , receptor , catalysis
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 ) 2 SO, [Cd(HAm‐pip)Br 2 ] · (CH 3 ) 2 SO, [Cd(HAmpip)I 2 ]·(CH 3 ) 2 SO, [Cd(Ampip) 2 ] and [Hg(HAmpip)Br 2 ]·(CH 3 ) 2 SO 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. 113 Cd NMR studies were carried out on the [Cd(HAmpip)X 2 ](X = Cl, Br or I) and [Cd(Ampip)(OAc)] 2 complexes. The 113 Cd 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 199 Hg NMR spectrum of [Hg(HAmpip)Cl 2 ] also is discussed.