Abstract
The reaction of elemental tellurium, tellurium tetrachloride, zirconium tetrachloride, and molybdenum oxytetrachloride yields black plate‐like crystals of Te4[MoZr2O2Cl11] (1) and yellow crystals of (TeCl3)2[Mo2O2Cl8]x[Zr2Cl10]1–x (2). Using molybdenum oxytrichloride instead of the oxytetrachloride, black crystals of (Te4)2[Mo2O2Cl8][ZrCl6] (3), Te8[ZrCl6] (4), and bronze‐colored crystals of Te4[ZrCl6] (5) are obtained. All obtained crystals are air‐sensitive and were characterized by single‐crystal X‐ray diffraction and energy‐dispersive X‐ray fluorescence spectroscopy. 1 contains a layered polymeric anion of unprecedented structural features with zirconium atoms coordinated in a pentagonal bipyramidal ZrO3Cl4 and ZrOCl6 environment. Magnetic susceptibility data of 1 and 2 show nearly ideal paramagnetic behavior according to the Curie law with magnetic moments of 1.55(7) μB for 1 and 1.66(6) μB for 2 indicating the presence of magnetically isolated d1 configured MoV. The double salt 3 adopts the structure type of the selenium containing congener (Se4)2[Mo2O2Cl8][ZrCl6], 4 and 5 are isotypic to the respective hafnium containing representatives Te4[HfCl6] and Te8[HfCl6].
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