Abstract
AbstractSyntheses and Crystal Structures of the Rhenium(VII) Nitride Chlorides ReNCl4 and ReNCl4·H2ORhenium(VII) nitride chloride, ReNCl4 (1) is obtained in form of brown needles with metallic luster by the reaction of ReCl5 with Cl3VNCl at 140 °C under vacuum in a sealed glass ampoule. It crystallizes in the tetragonal space group I4 with the lattice parameters a = 826.7(4), c = 405.1(2) pm, and Z = 2. The square pyramidal molecules are connected by asymmetric nitrido bridges to form chains along the crystallographic c axis. The shorter Re‐N distance of 163.0(5) pm corresponds to a triple bond, while the pronounced longer distance of 242.0(5) pm can be interpreted with a weak donor bond.The reaction of ReCl5 with VN at 170 °C under vacuum in a sealed glass ampoule yields red needles of ReNCl4·H2O (2). It crystallizes in the orthorhombic space group Pnma with a = 1075.4(2), b = 1108.5(2), c = 547.7(5) pm and Z = 4. The Re atoms exhibit a distorted octahedral coordination with the aqua ligand in trans position to the nitrido ligand. The Re‐N triple bond has a bond distance of 166.1(11) pm. The complexes are connected by hydrogen bridges O‐H···N to form chains.
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