Abstract
Oxotetrachloroaquorhenium(VI), ReOCl4•H2O, has been prepared and characterized for the first time by analysis, infrared spectroscopy and single crystal X-ray diffraction. The crystals were orthorhombic, a = 10.834(8), b = 11.089(8), c = 5.517(4) Å, Pn21a, Z = 4. Intensity data were recorded by integrating film methods and measured with a Joyce–Loebl microdensitometer, and 624 observable of the 704 measured independent reflections were given non-zero weight in the final cycle of full matrix least-squares refinement where R1 = 0.0572 and R2 = 0.0687. The molecular structure is based on a very distorted octahedron with a strongly bonded oxo-group (Re—O, 1.63(2) Å) trans (177(2)°) to a weakly bonded aquo-group (Re—O, 2.27 (2) Å). The Re—Cl distances do not differ significantly (2.29(1) Å av). The chlorine atoms are bent away from the oxo-group (angles vary from (94–102°(1)).
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