Synthesis and characterisation of [[µ-(1,7,11,17-tatraaza-2.6.12.16-tetraoxacycloeicosane)][µ-(aquo)bis(acac)(ethanol)Ni(II)]][BPh4]2

M. A. Novak, P. F. Prado, M. V. D. R. E. Silva, Janet Mabel Scott Skakle, M. G. F. Vaz, J. L. Wardell, S. M. S. V. Wardell

Research output: Contribution to journalArticle

Abstract

The pale blue title compound, 4, was obtained from the reaction between 1,7,11,17-tetraaza-2,6,12,16-tetraoxacycloeicosane, Ni(acac)(2) and NaBPh4 in aqueous acetone. X-ray structure determination at 120 K revealed that the dication of the ionic complex, 4, contains two independent octahedral Ni-II centres with trans-Ni2N2O4 chromophores. The macrocyclic ligand and an aqua ligand act as bridges to the two nickel centres: the Ni-O(aquo)-N bond angle is 137.65(17)degrees. Each Ni centre is bonded to two nitrogens of the macrocycle, to a chelating acac unit, to an ethanol molecule as well as the bridging oxygen of the aqua group. The two nickel atoms sit outside the macrocycle cavity, such that the macrocyclic ligand acts as a canopy for the remainder of the dication. While none of the macrocycle oxygens are involved in the coordination to Ni, they are involved in internal hydrogen bonding with the aqua and ethanol ligands. Magnetic measurements show a paramagnetic behaviour down to 2 K, with an effective moment of 2.8 Bohr magnetons at room temperature. (c) 2004 Elsevier B.V. All rights reserved.

Original languageEnglish
Pages (from-to)941-946
Number of pages5
JournalInorganica Chimica Acta
Volume358
DOIs
Publication statusPublished - 2005

Keywords

  • macrocycle ligand
  • magnetic behaviour
  • nickel complex
  • crystallography
  • CRYSTAL-STRUCTURE
  • COPPER(II) COMPLEXES
  • NICKEL(II) COMPLEXES
  • CHEMISTRY
  • 1,4,8,11-TETRAAZACYCLOTETRADECANE
  • MACROCYCLES
  • CYCLAM

Cite this

Synthesis and characterisation of [[µ-(1,7,11,17-tatraaza-2.6.12.16-tetraoxacycloeicosane)][µ-(aquo)bis(acac)(ethanol)Ni(II)]][BPh4]2. / Novak, M. A.; Prado, P. F.; Silva, M. V. D. R. E.; Skakle, Janet Mabel Scott; Vaz, M. G. F.; Wardell, J. L.; Wardell, S. M. S. V.

In: Inorganica Chimica Acta, Vol. 358, 2005, p. 941-946.

Research output: Contribution to journalArticle

Novak, M. A. ; Prado, P. F. ; Silva, M. V. D. R. E. ; Skakle, Janet Mabel Scott ; Vaz, M. G. F. ; Wardell, J. L. ; Wardell, S. M. S. V. / Synthesis and characterisation of [[µ-(1,7,11,17-tatraaza-2.6.12.16-tetraoxacycloeicosane)][µ-(aquo)bis(acac)(ethanol)Ni(II)]][BPh4]2. In: Inorganica Chimica Acta. 2005 ; Vol. 358. pp. 941-946.
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title = "Synthesis and characterisation of [[µ-(1,7,11,17-tatraaza-2.6.12.16-tetraoxacycloeicosane)][µ-(aquo)bis(acac)(ethanol)Ni(II)]][BPh4]2",
abstract = "The pale blue title compound, 4, was obtained from the reaction between 1,7,11,17-tetraaza-2,6,12,16-tetraoxacycloeicosane, Ni(acac)(2) and NaBPh4 in aqueous acetone. X-ray structure determination at 120 K revealed that the dication of the ionic complex, 4, contains two independent octahedral Ni-II centres with trans-Ni2N2O4 chromophores. The macrocyclic ligand and an aqua ligand act as bridges to the two nickel centres: the Ni-O(aquo)-N bond angle is 137.65(17)degrees. Each Ni centre is bonded to two nitrogens of the macrocycle, to a chelating acac unit, to an ethanol molecule as well as the bridging oxygen of the aqua group. The two nickel atoms sit outside the macrocycle cavity, such that the macrocyclic ligand acts as a canopy for the remainder of the dication. While none of the macrocycle oxygens are involved in the coordination to Ni, they are involved in internal hydrogen bonding with the aqua and ethanol ligands. Magnetic measurements show a paramagnetic behaviour down to 2 K, with an effective moment of 2.8 Bohr magnetons at room temperature. (c) 2004 Elsevier B.V. All rights reserved.",
keywords = "macrocycle ligand, magnetic behaviour, nickel complex, crystallography, CRYSTAL-STRUCTURE, COPPER(II) COMPLEXES, NICKEL(II) COMPLEXES, CHEMISTRY, 1,4,8,11-TETRAAZACYCLOTETRADECANE, MACROCYCLES, CYCLAM",
author = "Novak, {M. A.} and Prado, {P. F.} and Silva, {M. V. D. R. E.} and Skakle, {Janet Mabel Scott} and Vaz, {M. G. F.} and Wardell, {J. L.} and Wardell, {S. M. S. V.}",
year = "2005",
doi = "10.1016/j.ica.2004.10.023",
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journal = "Inorganica Chimica Acta",
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T1 - Synthesis and characterisation of [[µ-(1,7,11,17-tatraaza-2.6.12.16-tetraoxacycloeicosane)][µ-(aquo)bis(acac)(ethanol)Ni(II)]][BPh4]2

AU - Novak, M. A.

AU - Prado, P. F.

AU - Silva, M. V. D. R. E.

AU - Skakle, Janet Mabel Scott

AU - Vaz, M. G. F.

AU - Wardell, J. L.

AU - Wardell, S. M. S. V.

PY - 2005

Y1 - 2005

N2 - The pale blue title compound, 4, was obtained from the reaction between 1,7,11,17-tetraaza-2,6,12,16-tetraoxacycloeicosane, Ni(acac)(2) and NaBPh4 in aqueous acetone. X-ray structure determination at 120 K revealed that the dication of the ionic complex, 4, contains two independent octahedral Ni-II centres with trans-Ni2N2O4 chromophores. The macrocyclic ligand and an aqua ligand act as bridges to the two nickel centres: the Ni-O(aquo)-N bond angle is 137.65(17)degrees. Each Ni centre is bonded to two nitrogens of the macrocycle, to a chelating acac unit, to an ethanol molecule as well as the bridging oxygen of the aqua group. The two nickel atoms sit outside the macrocycle cavity, such that the macrocyclic ligand acts as a canopy for the remainder of the dication. While none of the macrocycle oxygens are involved in the coordination to Ni, they are involved in internal hydrogen bonding with the aqua and ethanol ligands. Magnetic measurements show a paramagnetic behaviour down to 2 K, with an effective moment of 2.8 Bohr magnetons at room temperature. (c) 2004 Elsevier B.V. All rights reserved.

AB - The pale blue title compound, 4, was obtained from the reaction between 1,7,11,17-tetraaza-2,6,12,16-tetraoxacycloeicosane, Ni(acac)(2) and NaBPh4 in aqueous acetone. X-ray structure determination at 120 K revealed that the dication of the ionic complex, 4, contains two independent octahedral Ni-II centres with trans-Ni2N2O4 chromophores. The macrocyclic ligand and an aqua ligand act as bridges to the two nickel centres: the Ni-O(aquo)-N bond angle is 137.65(17)degrees. Each Ni centre is bonded to two nitrogens of the macrocycle, to a chelating acac unit, to an ethanol molecule as well as the bridging oxygen of the aqua group. The two nickel atoms sit outside the macrocycle cavity, such that the macrocyclic ligand acts as a canopy for the remainder of the dication. While none of the macrocycle oxygens are involved in the coordination to Ni, they are involved in internal hydrogen bonding with the aqua and ethanol ligands. Magnetic measurements show a paramagnetic behaviour down to 2 K, with an effective moment of 2.8 Bohr magnetons at room temperature. (c) 2004 Elsevier B.V. All rights reserved.

KW - macrocycle ligand

KW - magnetic behaviour

KW - nickel complex

KW - crystallography

KW - CRYSTAL-STRUCTURE

KW - COPPER(II) COMPLEXES

KW - NICKEL(II) COMPLEXES

KW - CHEMISTRY

KW - 1,4,8,11-TETRAAZACYCLOTETRADECANE

KW - MACROCYCLES

KW - CYCLAM

U2 - 10.1016/j.ica.2004.10.023

DO - 10.1016/j.ica.2004.10.023

M3 - Article

VL - 358

SP - 941

EP - 946

JO - Inorganica Chimica Acta

JF - Inorganica Chimica Acta

SN - 0020-1693

ER -