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

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Setifi Z., Setifi F., Dege N., El Ati R., Glidewell C.

ACTA CRYSTALLOGRAPHICA SECTION E-CRYSTALLOGRAPHIC COMMUNICATIONS, vol.74, pp.668-684, 2018 (ESCI) identifier identifier identifier

  • Publication Type: Article / Article
  • Volume: 74
  • Publication Date: 2018
  • Doi Number: 10.1107/s2056989018005601
  • Journal Name: ACTA CRYSTALLOGRAPHICA SECTION E-CRYSTALLOGRAPHIC COMMUNICATIONS
  • Journal Indexes: Emerging Sources Citation Index (ESCI), Scopus
  • Page Numbers: pp.668-684
  • Keywords: crystal structure, polypyridyl complexes, redetermination, perchlorate anion disorder, hydrogen bonding, supramolecular assembly, PHENYLPHOSPHONIC ACID, MAGNETIC-PROPERTIES, 3 DIMENSIONS, 4,4'-SULFONYLDIPHENOL, 4,4'-THIODIPHENOL, DIPERCHLORATE, ADDUCTS, BLOCK
  • Ondokuz Mayıs University Affiliated: Yes

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 supramolecular assembly, not reported previously, takes the form of a complex three-dimensional framework built from C-H center dot center dot center dot 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.