Coordination of Zn II, Cd II, and Hg II by 2-pyridineformamide-3-piperidyl-thiosemicarbazone

Alfonso Castiñeiras; Isabel García; Elena Bermejo; Karen A. Ketcham; Douglas X. West; Ayman K. El-Sawaf

doi:10.1002/1521-3749(200202)628:2<492::AID-ZAAC492>3.0.CO;2-V

Coordination of Zn ^II, Cd ^II, and Hg ^II by 2-pyridineformamide-3-piperidyl-thiosemicarbazone

Alfonso Castiñeiras
, Isabel García
, Elena Bermejo
, Karen A. Ketcham
, Douglas X. West
, Ayman K. El-Sawaf

Research output: Contribution to journal › Article › peer-review

21 Scopus citations

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.

Original language	English
Pages (from-to)	492-504
Number of pages	13
Journal	Zeitschrift fur Anorganische und Allgemeine Chemie
Volume	628
Issue number	2
DOIs	https://doi.org/10.1002/1521-3749(200202)628:2<492::AID-ZAAC492>3.0.CO;2-V
State	Published - 2002
Externally published	Yes

Keywords

Cadmium
Mercury
Pyridine-formamide thiosemicarbazones
Semicarbazones
Zinc

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10.1002/1521-3749(200202)628:2<492::AID-ZAAC492>3.0.CO;2-V

Cite this

@article{0017af43beb041ee923f2b100c38f3e8,

title = "Coordination of Zn II, Cd II, and Hg II by 2-pyridineformamide-3-piperidyl-thiosemicarbazone",

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.",

keywords = "Cadmium, Mercury, Pyridine-formamide thiosemicarbazones, Semicarbazones, Zinc",

author = "Alfonso Casti{\~n}eiras and Isabel Garc{\'i}a and Elena Bermejo and Ketcham, \{Karen A.\} and West, \{Douglas X.\} and El-Sawaf, \{Ayman K.\}",

year = "2002",

doi = "10.1002/1521-3749(200202)628:2<492::AID-ZAAC492>3.0.CO;2-V",

language = "English",

volume = "628",

pages = "492--504",

journal = "Zeitschrift fur Anorganische und Allgemeine Chemie",

issn = "0044-2313",

publisher = "Wiley-VCH Verlag",

number = "2",

}

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 -

Coordination of Zn ^II, Cd ^II, and Hg ^II by 2-pyridineformamide-3-piperidyl-thiosemicarbazone

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