13709-32-5Relevant articles and documents
Synthesis and characterization of uranium(V) fluoride fluorosulfates and uranium(V) oxyfluorosulfate: UF3(SO3F)2, UF(SO3F)4, and UO(SO3F)3
Masson,Naulin,Charpin,Bougon
, p. 1858 - 1861 (1978)
The new uranium(V) fluoride fluorosulfate compounds UF3(SO3F)2 and UF(SO3F)4 and uranium(V) oxyfluorosulfate UO(SO3F)3 have been synthesized. UF3(SO3F)2, a pale green solid, resulted from the reaction of UF5 and S2O6F2 in CFCl3 at 40°C for 20 days; under these conditions the solvent also reacted and was partly transformed into CFCl2OSO2F and CF2Cl2. The beige solid UF(SO3F)4 was prepared by mixing UF6 and SO3 in CFCl3 at low temperature (3F)3, a tetragonal gray-beige solid. These three compounds were characterized by chemical analysis. Their thermal stabilities and vibrational and electronic spectra are also reported. The +5 oxidation state of uranium was confirmed by magnetic susceptibility measurements. Despite several attempts under different conditions, no uranium(VI) fluorosulfate or fluoride fluorosulfate was obtained.
Synthesis and characterization of the difluorotris(fluorosulfate) of uranium(V): UF2(SO3F)3
Wilson,Naulin,Bougon
, p. 2252 - 2257 (1977)
A new U(V) compound, UF2(SO3F)3, has been synthesized by the reaction of UF6 and SO3 in both the gaseous phase and CFCl3 solution. This leads to a blue-green solid, the x-ray powder diffraction pattern of which has been recorded. Its oxidation state has been deduced from chemical analysis, the electronic absorption spectrum, and magnetic measurements. The environment around uranium is discussed from Raman and infrared spectra recorded at ambient and liquid nitrogen temperatures.
METHODS OF MAKING HALOGENATED FLUORINATED ETHER-CONTAINING COMPOUNDS
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Paragraph 0087-0088, (2016/06/28)
Described herein are three methods for making halogenated fluorinated ether-containing compounds using a fluorinated olefin or hexafluoropropylene oxide.
Cationic carbonyl complexes of rhodium(I) and rhodium(III): Syntheses, vibrational spectra, NMR studies, and molecular structures of tetrakis(carbonyl)rhodium(I) heptachlorodialuminate and -gallate, [Rh(CO)4][Al2Cl7] and [Rh(CO)4][Ga2Cl7]
Von Ahsen, Britta,Bach, Christian,Berkei, Michael,Kockerling, Martin,Willner, Helge,Hagele, Gerhard,Aubke, Friedhelm
, p. 3801 - 3814 (2008/10/08)
Dimeric rhodium(I) bis(carbonyl) chloride, [Rh(CO)2(μ-Cl)]2, is found to be a useful and convenient starting material for the syntheses of new cationic carbonyl complexes of both rhodium(I) and rhodium(III). Its reaction with the Lewis acids AlCl3 or GaCl3 produces in a CO atmosphere at room temperature the salts [Rh(CO)4][M2Cl7] (M = Al, Ga), which are characterized by Raman spectroscopy and single-crystal X-ray diffraction. Crystal data for [Rh(CO)4][Al2Cl7]: triclinic, space group P1 (No. 2); a = 9.705(3), b = 9.800(2), c = 10.268(2) A; α = 76.52(2), β = 76.05(2), γ = 66.15(2)°; V = 856.7(5) A3; Z = 2; T = 293 K; R1 [I > 2σ(I)] = 0.0524, wR2 = 0.1586. Crystal data for [Rh(CO)4][Ga2Cl7]: triclinic, space group P1 (No. 2); a = 9.649(1), b = 9.624(1), c = 10.133(1) A; α = 77.38(1), β = 76.13(1), γ = 65.61(1)°; V = 824.4(2) A3; Z = 2; T = 143 K; R1 [I > 2σ(I)] = 0.0358, wR2 = 0.0792. Structural parameters for the square planar cation [Rh(CO)4]+ are compared to those of isoelectronic [Pd(CO)4]2+ and of [Pt(CO)4]2+. Dissolution of [Rh(CO)2Cl]2 in HSO3F in a CO atmosphere allows formation of [Rh(CO)4]+(solv). Oxidation of [Rh(CO)2Cl]2 by S2O6F2 in HSO3F results in the formation of ClOSO2F and two seemingly oligomeric RH(III) carbonyl fluorosulfato intermediates, which are easily reduced by CO addition to [Rh(CO)4]+(solv). Controlled oxidation of this solution with S2O6F2 produces fac-Rh(CO)3(SO3F)3 in about 95% yield. This RH(III) complex can be reduced by CO at 25 °C in anhydrous HF to give [Rh(CO)4]+(solv); addition of SbF5 at -40 °C to the resulting solution allows isolation of [Rh(CO)4][Sb2F11]2, which is found to have a highly symmetrical (D4h) [Sb2F11]- anion. Oxidation of [Rh(CO)2Cl]2 in anhydrous HF by F2, followed in a second step by carbonylation in the presence of SbF5, is found to be a simple, straightforward route to pure [Rh(CO)5Cl][Sb2F11]2, which has previously been structurally characterized by us. All new complexes are characterized by vibrational and NMR spectroscopy. Assignment of the vibrational spectra and interpretation of the structural data are supported by DFT calculations.