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The rare earth-based zinc compounds  RE  13 Pd 25+ x  Zn 28– x   ( RE  = Y, Ho–Lu) were synthesized from the elements in sealed niobium ampoules with a maximum reaction temperature of 1470 K followed by different annealing sequences. The structures of all compounds were refined from single crystal X-ray diffraction data, indicating substantial Zn/Pd mixing on one 8 c  and one 24 g  zinc site. Exemplarily, the homogeneity range of the solid solution Yb 13 Pd 25+ x  Zn 28– x   was manifested from samples of different starting compositions and five single crystal data sets. The  RE  13 Pd 25+ x  Zn 28– x   structures are cubic, space group  I 4̅3 m  with lattice parameters ranging from 1295 to 1307 pm, as a function of the rare earth element and the Zn/Pd mixing. Hierarchically, one can derive the  RE  13 Pd 25+ x  Zn 28– x   structures from the simple  bcc  packing. A group–subgroup scheme was developed for this new 4 × 4 × 4 tungsten superstructure which shows vacancy ordering and dumbbell formation. Temperature dependent magnetic susceptibility measurements show diamagnetism for a Lu 13 Pd 29 Zn 24  sample and Curie–Weiss paramagnetism for Tm 13 Pd 29 Zn 24  down to 3 K.

RE 13 Pd 25+ x Zn 28– x ( RE = Y, Ho–Lu) – A 4 × 4 × 4 tungsten superstructure with short Pd/Zn dumbbells as structural motif