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We report on the synthesis and crystal structure of the octaammine calcium(II) halides [Ca(NH 3 ) 8 ]Br 2 , and [Ca(NH 3 ) 8 ]I 2 , which were synthesized by the reaction of the respective calcium( II) halides with dry liquid ammonia. The compounds form colorless crystals which crystallize isotypically at 123 K with Z = 4 in the orthorhombic space group Pnma with a = 12:0478(3), b = 7:4406(2), c = 15:7216(4) Å, V = 1409:33(6) Å 3  for the bromide, and a = 12:1113(4), b = 7:7706(3), c = 16:7145(6) Å, V = 1573:0(1) Å 3  for the iodide. Instead of the expected tetragonal antiprism for the eightfold-coordinated Ca 2+  ions, we observed a coordination polyhedron best described as a twofold capped trigonal prism. After evaporation of the liquid ammonia and warming of [Ca(NH 3 ) 8 ]I 2  to room temperature, [Cu(NH 3 ) 6 ]I 2  was obtained as a colorless powder. The hexaammine calcium(II) iodide crystallizes isotypically to [Mn(NH 3 ) 6 ]I 2  (CaF 2  type) in the cubic space group Fm3̅m with a = 11:18580(6) Å, V = 1399:59(1) Å 3 , Z = 4 at 293 K

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The Unusual Coordination Sphere in the Octaammine Calcium(II) Ions of [Ca(NH 3 ) 8 ]Br 2  and [Ca(NH 3 ) 8 ]I 2  and the Thermal Decomposition of the Iodide to [Ca(NH 3 ) 6 ]I 2