Isomorphous crystal structures of 4,7,13,16,21,24-hexaoxo-1,10-diaziniabicyclo[8.8.8]•hexacosane bis(tribromide) and bis(bromoiodide)

Two compounds, 7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane bis(tribromide) and bis(bromodiiodide) - [H-2(Crypt-222)](2+)center dot 2Br(3)(-) (I) and [H-2(Crypt-222)](2+)center dot 1.45(BrI2)(-)center dot 0.4(Br2I)(-)center dot 0.15 I-3(-) (II) - are prepared and characterized by single crystal XRD; the refinement of the second compound was more accurate. Isomorphous monoclinic structures (I, space group C2/c, Z = 4, a = 12.090, b = 15.833 angstrom, c = 15.732 angstrom, beta = 95.83 degrees; II, a = 12.548 angstrom, b = 16.417 angstrom, c = 15.748 angstrom, beta = 94.53 degrees) are solved by a direct method and refined in the anisotropic full-matrix approximation to R = 0.057 (I) and 0.044 (II) using all 2635 (I) and 2852 (II) measured independent reflections (automated CAD-4 diffractometer, lambda MoK (alpha)). In the structures of I and II one of the trihalide anions sits at the inversion center i(000), and the second trihalide anion and the dication [H-2(Crypt-222)](2+) are situated at crystallographic axis 2. In the structure of II iodine is located in the center of trihalide anions, while the terminal atoms are disordered and are represented by a statistical combination of iodine and bromine atoms.