Synthesis and characterisation of double-layered octahedral coordination networks built up from divalent metal ions, mixed carboxylate anions, and ethyl carbazate ligands

Subramani Sathiyakumar, Pitchai Selvam, Faruck Lukmanul Hakkim, Krishnan Srinivasan (Corresponding Author), William T. A. Harrison (Corresponding Author)

Research output: Contribution to journalArticle

Abstract

A new hydrazone, Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate(C9H11N3O2; Hpyec) and its metal complexes bis(Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate) nickel(II) monohydrate, [Ni(pyec)2]·H2O (1) and bis(acetato)(Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate) cadmium (II), [Cd(Hpyec)(CH3COO)2](2), have been prepared by mechano-chemical syntheses and characterized by elemental analysis, UV-visible, IR and NMR spectroscopy, TG-DTA, and solid state emission techniques. The X-ray single crystal structures of both complexes were determined: in 1, the Ni2+ion is coordinated by two N, N, O-tridentate anionic ligands to generate a distorted cis-NiO2N4 octahedron. In 2, the cadmium atom is seven-coordinated by one neutral N,N.O-tridentate ligand and two chelating acetate ions to generate a very-distorted CdN2O5 pentagonal bipyramid with the Hpyec atoms occupying both axial and one equatorial site. Crystal data: 1, C18H22N6NiO5, Mr = 461.12, monoclinic, P21/c, a = 10.8759 (3) Å, b = 11.7055 (4) Å, c = 16.8424 (5) Å, b = 108.583 (1)°, V = 2032.38 (11) Å3, Z = 4, R(F) = 0.023, wR(F2) = 0.065;2, C13H17CdN3O6, Mr = 423.69, monoclinic, Cc, a = 13.0215 (10) Å, b = 15.8104 (11) Å, c = 7.99 (6) Å, b = 96.692 (2)°, V = 1621.7 (2) Å3, Z = 4, R(F) = 0.017, wR(F2) = 0.038.
Original languageEnglish
JournalJournal of Molecular Structure
Publication statusAccepted/In press - 18 Dec 2018

Fingerprint

hydrazine
Anions
Metal ions
Ligands
Cadmium
Ions
Hydrazones
Atoms
Coordination Complexes
Chelation
Nickel
Differential thermal analysis
Nuclear magnetic resonance spectroscopy
Infrared spectroscopy
Acetates
Crystal structure
Single crystals
X rays
Crystals
Chemical analysis

Keywords

  • Green synthesis
  • hydrazone
  • metal complexes
  • crystal structures
  • emission study

Cite this

Synthesis and characterisation of double-layered octahedral coordination networks built up from divalent metal ions, mixed carboxylate anions, and ethyl carbazate ligands. / Sathiyakumar, Subramani ; Selvam, Pitchai ; Hakkim, Faruck Lukmanul ; Srinivasan, Krishnan (Corresponding Author); Harrison, William T. A. (Corresponding Author).

In: Journal of Molecular Structure, 18.12.2018.

Research output: Contribution to journalArticle

@article{45b879cf857845e6997f090a81cc8e83,
title = "Synthesis and characterisation of double-layered octahedral coordination networks built up from divalent metal ions, mixed carboxylate anions, and ethyl carbazate ligands",
abstract = "A new hydrazone, Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate(C9H11N3O2; Hpyec) and its metal complexes bis(Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate) nickel(II) monohydrate, [Ni(pyec)2]·H2O (1) and bis(acetato)(Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate) cadmium (II), [Cd(Hpyec)(CH3COO)2](2), have been prepared by mechano-chemical syntheses and characterized by elemental analysis, UV-visible, IR and NMR spectroscopy, TG-DTA, and solid state emission techniques. The X-ray single crystal structures of both complexes were determined: in 1, the Ni2+ion is coordinated by two N, N, O-tridentate anionic ligands to generate a distorted cis-NiO2N4 octahedron. In 2, the cadmium atom is seven-coordinated by one neutral N,N.O-tridentate ligand and two chelating acetate ions to generate a very-distorted CdN2O5 pentagonal bipyramid with the Hpyec atoms occupying both axial and one equatorial site. Crystal data: 1, C18H22N6NiO5, Mr = 461.12, monoclinic, P21/c, a = 10.8759 (3) {\AA}, b = 11.7055 (4) {\AA}, c = 16.8424 (5) {\AA}, b = 108.583 (1)°, V = 2032.38 (11) {\AA}3, Z = 4, R(F) = 0.023, wR(F2) = 0.065;2, C13H17CdN3O6, Mr = 423.69, monoclinic, Cc, a = 13.0215 (10) {\AA}, b = 15.8104 (11) {\AA}, c = 7.99 (6) {\AA}, b = 96.692 (2)°, V = 1621.7 (2) {\AA}3, Z = 4, R(F) = 0.017, wR(F2) = 0.038.",
keywords = "Green synthesis, hydrazone, metal complexes, crystal structures, emission study",
author = "Subramani Sathiyakumar and Pitchai Selvam and Hakkim, {Faruck Lukmanul} and Krishnan Srinivasan and Harrison, {William T. A.}",
note = "This work is funded by DST-SERB, India, Under EMEQ scheme (SB/EMEQ-164/2014).",
year = "2018",
month = "12",
day = "18",
language = "English",
journal = "Journal of Molecular Structure",
issn = "0022-2860",
publisher = "Elsevier Science B. V.",

}

TY - JOUR

T1 - Synthesis and characterisation of double-layered octahedral coordination networks built up from divalent metal ions, mixed carboxylate anions, and ethyl carbazate ligands

AU - Sathiyakumar, Subramani

AU - Selvam, Pitchai

AU - Hakkim, Faruck Lukmanul

AU - Srinivasan, Krishnan

AU - Harrison, William T. A.

N1 - This work is funded by DST-SERB, India, Under EMEQ scheme (SB/EMEQ-164/2014).

PY - 2018/12/18

Y1 - 2018/12/18

N2 - A new hydrazone, Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate(C9H11N3O2; Hpyec) and its metal complexes bis(Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate) nickel(II) monohydrate, [Ni(pyec)2]·H2O (1) and bis(acetato)(Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate) cadmium (II), [Cd(Hpyec)(CH3COO)2](2), have been prepared by mechano-chemical syntheses and characterized by elemental analysis, UV-visible, IR and NMR spectroscopy, TG-DTA, and solid state emission techniques. The X-ray single crystal structures of both complexes were determined: in 1, the Ni2+ion is coordinated by two N, N, O-tridentate anionic ligands to generate a distorted cis-NiO2N4 octahedron. In 2, the cadmium atom is seven-coordinated by one neutral N,N.O-tridentate ligand and two chelating acetate ions to generate a very-distorted CdN2O5 pentagonal bipyramid with the Hpyec atoms occupying both axial and one equatorial site. Crystal data: 1, C18H22N6NiO5, Mr = 461.12, monoclinic, P21/c, a = 10.8759 (3) Å, b = 11.7055 (4) Å, c = 16.8424 (5) Å, b = 108.583 (1)°, V = 2032.38 (11) Å3, Z = 4, R(F) = 0.023, wR(F2) = 0.065;2, C13H17CdN3O6, Mr = 423.69, monoclinic, Cc, a = 13.0215 (10) Å, b = 15.8104 (11) Å, c = 7.99 (6) Å, b = 96.692 (2)°, V = 1621.7 (2) Å3, Z = 4, R(F) = 0.017, wR(F2) = 0.038.

AB - A new hydrazone, Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate(C9H11N3O2; Hpyec) and its metal complexes bis(Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate) nickel(II) monohydrate, [Ni(pyec)2]·H2O (1) and bis(acetato)(Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate) cadmium (II), [Cd(Hpyec)(CH3COO)2](2), have been prepared by mechano-chemical syntheses and characterized by elemental analysis, UV-visible, IR and NMR spectroscopy, TG-DTA, and solid state emission techniques. The X-ray single crystal structures of both complexes were determined: in 1, the Ni2+ion is coordinated by two N, N, O-tridentate anionic ligands to generate a distorted cis-NiO2N4 octahedron. In 2, the cadmium atom is seven-coordinated by one neutral N,N.O-tridentate ligand and two chelating acetate ions to generate a very-distorted CdN2O5 pentagonal bipyramid with the Hpyec atoms occupying both axial and one equatorial site. Crystal data: 1, C18H22N6NiO5, Mr = 461.12, monoclinic, P21/c, a = 10.8759 (3) Å, b = 11.7055 (4) Å, c = 16.8424 (5) Å, b = 108.583 (1)°, V = 2032.38 (11) Å3, Z = 4, R(F) = 0.023, wR(F2) = 0.065;2, C13H17CdN3O6, Mr = 423.69, monoclinic, Cc, a = 13.0215 (10) Å, b = 15.8104 (11) Å, c = 7.99 (6) Å, b = 96.692 (2)°, V = 1621.7 (2) Å3, Z = 4, R(F) = 0.017, wR(F2) = 0.038.

KW - Green synthesis

KW - hydrazone

KW - metal complexes

KW - crystal structures

KW - emission study

M3 - Article

JO - Journal of Molecular Structure

JF - Journal of Molecular Structure

SN - 0022-2860

ER -