Redetermination of the crystal structure of bis-(tri-2-pyridyl-amine)-iron(II) bis-(perchlorate), and a new refinement of the isotypic nickel(II) analogue: treatment of the perchlorate anion disorder

Zouaoui Setifi; Fatima Setifi; Necmi Dege; Rafika El Ati; Christopher Glidewell

doi:10.1107/S2056989018005601

Redetermination of the crystal structure of bis-(tri-2-pyridyl-amine)-iron(II) bis-(perchlorate), and a new refinement of the isotypic nickel(II) analogue: treatment of the perchlorate anion disorder

Acta Crystallogr E Crystallogr Commun. 2018 Apr 17;74(Pt 5):668-672. doi: 10.1107/S2056989018005601. eCollection 2018 May 1.

Authors

Zouaoui Setifi^{1

2}, Fatima Setifi², Necmi Dege³, Rafika El Ati⁴, Christopher Glidewell⁵

Affiliations

¹ Département de Technologie, Faculté de Technologie, Université 20 Août 1955-Skikda, BP 26, Route d'El-Hadaiek, Skikda 21000, Algeria.
² Laboratoire de Chimie, Ingénierie Moléculaire et Nanostructures (LCIMN), Université Ferhat Abbas Sétif 1, Sétif 19000, Algeria.
³ Ondokuz Mayıs University, Arts and Sciences Faculty, Department of Physics, 55139 Atakum-Samsun, Turkey.
⁴ Laboratoire de Chimie Appliquée et Environnement, (LCAE), Faculté des Sciences, Université Mohamed Premier, BP 524, 60000, Oujda, Morocco.
⁵ School of Chemistry, University of St Andrews, St Andrews, Fife KY16 9ST, UK.

Abstract

The redetermination of the structure of the title compound, [Fe(C₁₅H₁₂N₄)₂](ClO₄)₂, (I), confirms the structure previously reported [Kucharski et al. (1978a ▸). Aust. J. Chem. 31, 53-56], but models the perchlorate over four sets of atomic sites, rather than using just one set of sites as in the original report. The supra-molecular assembly, not reported previously, takes the form of a complex three-dimensional framework built from C-H⋯O hydrogen bonds. The isotypic nickel(II) analogue, [Ni(C₁₅H₁₂N₄)₂](ClO₄)₂, (III), has been refined using the original data set [Wang et al. (2011 ▸). Acta Cryst. E67, m78], again using a four-component disorder model for the anion, rather than a two-component model as in the original report, leading to more satisfactory Cl-O distances and O-Cl-O angles.

Keywords: crystal structure; hydrogen bonding; perchlorate anion disorder; polypyridyl complexes; redetermination; supramolecular assembly.

Grants and funding

This work was funded by Direction Générale de la Recherche Scientifique et du Développement Technologique grant . Université Ferhat Abbas Sétif 1 grant .