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Single crystals of Sr 2 H 3 I andBa 5 H 2 I 3.9(2) O 2  were obtained by reacting Sr or Ba, respectively, with dried and sublimed NH 4 I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules for 13 h at 1200 K. The crystal structures of the new compounds have been determined by means of single-crystal X-ray diffraction. Sr 2 H 3 I crystallizes in a stuffed anti-CdI 2  structure isotypic to Ba 2 H 3 Cl in the space group P3m1 (no. 164) with the lattice parameters a = 426.0(1) and c = 774.9(2) pm, while Ba 5 H 2 I 3.9(2) O 2  crystallizes in a new structure type in the space group Cmcm (no. 63) with the lattice parameters a = 1721.0(2), b = 1452.5(2) and c = 639.03(9) pm. The structural results for Sr 2 H 3 I are corroborated by EUTAX calculations. For the disordered compound Ba 5 H 2 I 3.9(2) O 2 , EUTAX calculations on an approximated, ordered structural model were used to find possible insights into the disorder

AlkalineEarthMetal-Hydride-Iodide Compounds: Syntheses andCrystal Structures of Sr 2 H 3 I and Ba 5 H 2 I 3.9(2) O 2