Abstract
The title compound is obtained in high yield from the reaction of appropriate proportions of ZrCl 4, zirconium powder, amorphous boron, and BaCl 2 in sealed tantalum tubing for about 2 weeks at 800 °C. The isostructural BaSrZr 6Cl 17B and Ba 2Zr 6Cl 17Mn are obtained in a similar manner, but not analogues containing smaller cations, iron or carbon. An X-ray diffraction study of a single crystal prepared at a higher temperature (about 1000 °C) has identified the new structure type and composition Ba 2Zr 6Cl 17B (space group, I4/ m; Z = 2; a = 11.4735(4) A ̊ , c = 9.8812(5) A ̊ ; R R w = ( 1.7 2.5 )% for 1247 independent reflections; 2 θ < 65°; Mo Kα radiation). The structure contains infinite linear chains of bridged clusters [ (Zr 6Cl 12B)Cl 2 2 a-aCl 4 a] 4− with Ba 2+ in sites of S 4 symmetry binding these together in a parallel staggered ar/rangement. Small cluster distortions are noted that apparently arise because of the higher field cations. This cluster network completes the stoichiometric series (Zr 6Cl 12Z)Cl n for 0 ⩽ n ⩽ 6 and exhibits the expected connectivity.
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