Inorganic Chemistry, Vol.35, No.4, 929-942, 1996
Tetrachlorostibonium(V) and Tetrabromostibonium(V) Cations - Raman and F-19, Sb-121, and Sb-123 NMR Spectroscopic Characterization and X-Ray Crystal-Structures of Sbcl4+sb(Otef5)(6)(-) and Sbbr4+sb(Otef5)(6)(-)
The stable salts, SbCl4+Sb(OTeF5)(6)(-) and SbBr4+Sb(OTeF5)(6)(-), have been prepared by oxidation of Sb(OTeF5)(3) with Cl-2 and Br-2, respectively. The SbBr4+ cation is reported for the first time and is only the second example of a tetrahalostibonium(V) cation. The SbCl4+ cation had been previously characterized as the Sb2F11-, Sb2Cl2F9-, and Sb2Cl0.5F10.5- salts. Both Sb(OTeF5)(6)(-) salts have been characterized in the solid state by low-temperature Raman spectroscopy and X-ray crystallography. Owing to the weakly coordinating nature of the Sb(OTeF5)(6)(-) anion, both salts are readily soluble in SO2ClF and have been characterized in solution by Sb-121, Sb-123, and F-19 NMR spectroscopy.
Keywords:NUCLEAR-MAGNETIC-RESONANCE;FLUOROPHOSPHONIUM CATIONS;VIBRATIONAL-SPECTRA;BOND-VALENCE;ANTIMONY;AS-75;HEXAFLUOROARSENATE;REDETERMINATION;TRIHALIDES;COMPLEXES