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Br14K2Mo6, cubic, Pn3 (no. 201), a = 13.800(2) A, V = 2628.1 A 3 , Z =4 ,Rgt(F) = 0.077, wRref(F 2 ) = 0.186, T = 293 K. Source of material A silica tube ( =1 5 mm,D =1m m,L = 90 mm) charged with 462 mg (0.300 mmol) Mo6Br12 (Alfa, 98+ %) and 72 mg (0.600 mmol) KBr (ACROS 98 %) was heated in the temperature gradient 925/915 K for one week. Orange plate-shaped crystals were formed in the low temperature zone and Mo in the high temperature zone. Experimental details Refinements gave an occupancy of the K2 cation close to 2 3 ,b efore the parameter was fixed at this value. The large R values may be due to the inferior crystal quality.

Crystal structure of dipotassium octakis(//3-bromo)hexabromo-octahedro hexamolybdenate, K 2 [Mo 6 Br 14 ]