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The reaction of 1,8-diaminooctane with hydroiodic acid in the presence of iodine gave a new polyiodide-containing salt: 1,8-diaminiumoctane bis(triiodide), (H3N-(CH2)8-NH3)[I3]2. The title compound has been characterized by crystallographic and spectroscopic methods. The polyiodide ion is the first example of a hydrogen bonded I62− dianion consisting of two very asymmetric triiodide components with I−I distances of 2.7739(4) and 3.1778(4) Å interacting by a weak halogen bond (I···I: 3.5017(2) Å). The structural parameters of the triiodide anions, derived from X-ray crystallographic data, are in good agreement with the Raman and Far-IR spectroscopic results

I62− Anion Composed of Two Asymmetric Triiodide Moieties: A Competition between Halogen and Hydrogen Bond