Redetermination of the Crystal Structure of Bis(Tri-2 Bis(Perchlorate), and a New Refinement of the Isotypic Nickel(II) Analogue: Treatment of the Perchlorate Anion Disorder

Abstract

The redetermination of the structure of the title compound, [Fe(C<inf>15</inf> H<inf>12</inf> N<inf>4</inf>)<inf>2</inf> ](ClO<inf>4</inf>)<inf>2</inf>, (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...O hydrogen bonds. The isotypic nickel(II) analogue, [Ni(C<inf>15</inf> H<inf>12</inf> N<inf>4</inf>)<inf>2</inf> ](ClO<inf>4</inf>)<inf>2</inf>, (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. © Setifi et al. 2018.