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The average structures ( Immm ) of Gd 13 Br 18 B 3  ( A  = 3.9923(2) Å,  B  = 17.0462(12) Å,  C  = 28.3039(19) Å) and Tb 13 Br 18 B 3  ( A  = 3.9637(3) Å,  B  = 16.9063(13) Å,  C  = 28.1068(18) Å) were solved taking into account Bragg intensities only. The average structure contains an ordered honeycomb arrangement of chains formed from trans edge sharing Tb 6 B octahedra and disordered and partly occupied chains of double octahedra in the channels. Pronounced diffuse scattering which is elongated in [001]* indicates a 2D order of the structure. High resolution electron microscopy (HRTEM) gives insight into the nature of the ordering and leads to a model of discrete Tb 10 B 2  clusters in the channels which are perfectly ordered in layers in a 2 × 2 × 2 supercell. These layers are randomly stacked with well defined translation values to each other along [100].

Solution of the structure and disorder of Ln 13 Br 18 B 3 (Ln = Gd, Tb)