Abstract
AbstractThe anion-mixed niobium tetrahalides Nb(Br0.62(4)Cl0.38(4))2Cl2and NbI2Cl2were obtained by heating NbBr5with NbCl5and NbI5with NbCl5, respectively, in equimolar ratios with niobium metal in evacuated, torch-sealed silica ampoules at 720 K for 3 days. The orthorhombic title compounds form as very brittle black needles and were characterized by single-crystal X-ray diffraction [space group:Immm,Z=4;a=704.27(6),b=824.13(7),c=929.64(8) pm for Nb(Br0.62(4)Cl0.38(4))2Cl2anda=753.76(6),b=829.38(7) andc=983.41(8) pm for NbI2Cl2]. Surprisingly enough, these mixed-anionic halides are not isostructural with either NbCl4, NbBr4or NbI4, but crystallize isotypically with TaI2Cl2, thus being examples for differential site occupancy stabilized materials. Structural features of other niobium(IV) halides are compiled and compared to those of Nb(Br0.62(4)Cl0.38(4))2Cl2and NbI2Cl2. Except for NbF4, they all exhibit chains oftrans-edge connected [NbX6]2−octahedra, which allowPeierlsdistortions to form Nb–Nb single bonds. The packing of these chains differ, however, depending on the actual halide or mixed-halide combination.
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