14986-57-3Relevant articles and documents
Structure of the fluorosulfite anion: Rotational disorder of SO2F- in the alkali metal fluorosulfites and crystal structures of α- and β-CsSO2F
Kessler,Van Wuellen,Jansen
, p. 7040 - 7046 (2001)
19F solid-state NMR spectra of the alkali metal fluorosulfites KSO2F, RbSO2F, α-CsSO2F, and β-CsSO2F show that the fluorosulfite anion is subjected to dynamical disorder at room temperature. This disorder can be modeled by 120° rotational jumps with respect to the C3-pseudoaxis of the anion. The exchange frequency of this disorder decreases with decreasing temperature. The calculated jump frequencies at room temperature are 5 x 105 Hz for KSO2F, 2 × 105 Hz for RbSO2F, 1 × 107 Hz for α-CsSO2F, and 5 × 105 Hz for β-CsSO2F, respectively. The crystal structures of α- and β-CsSO2F were determined for the first time (α: Pnma; Z = 4; a = 790.98(8), b = 666.07(7), c = 798.93(9) pm; T = 293 K. β: R3m; Z = 3; a= 659.22(6), c = 800.50(4) pm; T = 293 K). X-ray single-crystal data of KSO2,F RbSO2F, and α-CsSO2F taken at various temperatures were refined using the disorder model developed from the NMR results. It is shown that it is impossible to obtain reliable structural parameters of the SO2F- ion by refinement of X-ray data as long as rotational disorder persists. The preference of an ordered structure increases with decreasing temperature. The degree of disorder remaining in α-CsSO2F at 93 K is small. The structural parameters of the fluorosulfite anion as obtained by a routine refinement of this phase (S-F, 169.0(2) pm; S-O, 147.8(1) pm) are the best lower (S-F) and upper (S-O) limits of the true bond lengths determined experimentally. They comply with the values obtained from quantum chemical calculations.
METHOD OF MAKING A HALOSILOXANE
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Paragraph 0041; 0051; 0052, (2019/01/06)
A method of producing a halosiloxane, the method comprising: i) combining water, a halosilane, and a first solvent to form a reaction mixture, ii) partially hydrolyzing and condensing the halosilane to form a reaction product mixture comprising the halosiloxane, the solvent, unreacted halosilane, and hydrogen halide, iii) adding a second solent, where the second solent has a boiling point the boiling point of the halosiloxane, to the reaction mixture in i) or to the reaction product mixture in ii), and iv) recovering the halosiloxane from the reaction product mixture.
Crystal structures of monofluorosulfites MSO2F (M = K, Rb)
Kessler, Ulrich,Jansen, Martin
, p. 385 - 388 (2008/10/08)
Single crystals of potassium and rubidium fluorosulfite were obtained for the first time by reacting the alkali metal fluorides with sulfur dioxide in acetonitrile at 75 °C. According to the results of X-ray structure determinations they are isotypic (monoclinic, P21/m, Z = 2, KSO2F: a = 696.2(2), b = 566.3(2), c = 465.8(1) pm, β = 107.73(2)o, RbSO2F: a = 717.2(1), b = 586.7(1), c = 484.0(1) pm, β = 107.14(1)o) and structurally analogous to potassium chlorate. In contrast to potassium fluoroselenite in which the complex anions are polymerized to linear chains by unsymmetric fluorine bridges, the fluorosulfite anion is isolated. The S-F-distance of 159.1(2) pm (KSO2F) corresponds to a S-F single bond, the S-O-distance of 152.6(2) pm indicates a bond order of 1.5.
