Synthesis of Sulfur Difluoride (Difluorophosphinyl)‐imide and Sulfur Oxide Difluoride (Fluorosulfonyl)imide

Glemser, Oskar; Roesky, Herbert W.; Heinze, Petra

doi:10.1002/anie.196707101

Cited by 11 publications

(3 citation statements)

References 2 publications

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“…Only after the amine was chemically modified did evidence of the amine become apparent. In a similar manner, the existence of the amine is supported by the appearance of a broad peak at 1470 cm –1 after lithiation, which is attributed to the SO 2 asymmetric and symmetric stretches of the sulfonimide salt. , …”

Section: Resultsmentioning

confidence: 77%

“…In a similar manner, the existence of the amine is supported by the appearance of a broad peak at 1470 cm −1 after lithiation, which is attributed to the SO 2 asymmetric and symmetric stretches of the sulfonimide salt. 19,20 To explore the depotonation conditions, a small molecule model, N-pentenylsulfonimide, was exposed to n-butyllithium in toluene. As shown in Supporting Information Figure S2, the NH stretch at 3250 cm −1 is lost upon deprotonation by nbutyllithium under these conditions.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

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Plasticized Polymer Composite Single-Ion Conductors for Lithium Batteries

Zhao

Asfour

et al. 2015

ACS Appl. Mater. Interfaces

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Lithium bis(trifluoromethane) sulfonamide (TFSI) is a promising electrolyte salt in lithium batteries, due to its good conductivity and high dissociation between the lithium cation and its anion. By tethering N-pentane triflouromethane sulfonamide (C5NHTf), a TFSI analogue molecule, onto the surface of silica nanoparticle as a monolayer coverage should increase the Li + transference number to unity since anions bound to particles have reduced mobilities. Silica polymer composite has better mechanical property than that of the pure PEO. Analogously trifluoromethane sulfonic aminoethylmethacrylate (TfMA), a TFSI analogue vinyl monomer was polymerized on silica nanoparticle surface as a multilayer coverage. Anchored polyelectrolytes to particle surfaces offer multiple sites for anions, and in principle, the carrier concentration would increase arbitrarily and approach the carrier concentration of the bulk polyelectrolyte. Monolayer grafted nanoparticle have a lithium content of 1.2*10 -3 g Li/g and multilayer grafted nanoparticle have a lithium content over an order higher at 2*10 -2 g Li/g. Electrolytes made from monolayer grafted particles exhibit a weak conductivity dependence on temperature, exhibiting an ionic conductivity in the range of 10 -6 S/cm when temperatures increase to 80 °C. While electrolytes made from multilayer grafted particles show a steep increase in conductivity with temperature with an ionic conductivity increase to 3*10 -5 S/cm at 80 °C, with a O/Li ratio of 32.

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Section: Resultsmentioning

confidence: 77%

Section: ■ Results and Discussionmentioning

confidence: 99%

Plasticized Polymer Composite Single-Ion Conductors for Lithium Batteries

Zhao

Asfour

et al. 2015

ACS Appl. Mater. Interfaces

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“…From the reactions with primary amines or N,N-bis-silylated amines, with Me 3 SiNCNSiMe 3 or Si(NCO) 4 the derivatives FSO 2 NSOF 2 [10,11], F 5 SNSOF 2 [12,13], NCNSOF 2 [14][15][16], and FC(O)NSOF 2 [17,18] were isolated. These materials have been structurally characterised by gas-phase electron diffraction, but because of their low melting points, data on their solid-state structures is more limited, and of the compounds listed, only in one case, FC(O)NSOF 2 , was the crystal structure also reported.…”

Section: Introductionmentioning

confidence: 99%

Comparison of intermolecular interactions in two phases of MeNSOF₂

Mews

Parsons

2014

Zeitschrift Für Kristallographie - Crystalline Materials

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MeNSOF 2 was crystallised by laser-assisted zone refinement at 150 K. The structure obtained by X-ray diffraction initially on cooling to 140 K was triclinic, P-1, but this transformed slowly to a second phase, which was monoclinic C2/c. Bond distances and angles are similar to equivalent interactions in (MeN) 2 SF 2 and SO 2 F 2 . Intermolecular interactions in both phases are dominated by dispersion, though electrostatics are also important in all the most energetic contacts. Though no interatomic contacts fall within the sums of van der Waals radii of the contacting atoms, PIXEL calculations indicate that some intermolecular energies are similar to medium-strength hydrogen bonds. The monoclinic phase is denser than the triclinic phase, having stronger dispersion interactions. PIXEL and DFT calculations indicate that the two phases are energetically very finely balanced, but phase I becomes competitive at higher temperature on account of the entropy advantage of its 'looser' structure. DFT phonon energy calculations suggest that the mechanism of the transition may involve coupling between acoustic and low energy optical phonons.

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N‐(Fluorformyl)iminoschwefeldichlorid und N‐(Chlorformyl)iminoschwefeldichlorid

Roesky

Mews

1968

Angewandte Chemie

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den SP(N H2)3 161 die verbliebene Schwefelfunktion durch Alkylieren aktiviert 171 und durch schonende abermalige Ammonolyse die vierte Aminogruppe einfiihrt.Das aus Thiophosphorslure-triamid und Methyljodid erhaltliche (I) 181 ist auRer in Anilin in organischen Solventien unlbslich. Von aliphatischen Arninen, Alkoholen und Wasser wird es irn Gegensatz zurn SP(NH2)j rasch zersetzt. Die Halbwertszeit der Hydrolyse bei 0 "C wurde an einer 40-proz. Lbsung in D20 IH-NMR-spektroskopisch zu rund 20 Minuten bestimmt. Die Hydrolyse verlauft nicht einheitlich; nur zum Teil wird dabei die Methylthiogruppe abgespalten, zum etwas geringeren Teil bleibt sie an den Phosphor gebunden. Bei Raumtemperatur ist die Hydrolyse nach wenigen Minuten vollstandig. 6'H = 2,56 ppm Dublett -CH,S -P = 0 J p s c~ = 16,2 Hz I NH2 CH,SH + HJ PPm YH2 -CH,S-P=O I OH 6lII = -2.42 ppm 6'H = -2,34 ppm Dublett Dublett J p s C H = 14,8 Hz JpSCH = 13,3 HZ Verschiebungen in DLO gcgen TMS als externen Standard.

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Synthesis of Sulfur Difluoride (Difluorophosphinyl)‐imide and Sulfur Oxide Difluoride (Fluorosulfonyl)imide

Cited by 11 publications

References 2 publications

Plasticized Polymer Composite Single-Ion Conductors for Lithium Batteries

Plasticized Polymer Composite Single-Ion Conductors for Lithium Batteries

Comparison of intermolecular interactions in two phases of MeNSOF₂

N‐(Fluorformyl)iminoschwefeldichlorid und N‐(Chlorformyl)iminoschwefeldichlorid

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Synthesis of Sulfur Difluoride (Difluorophosphinyl)‐imide and Sulfur Oxide Difluoride (Fluorosulfonyl)imide

Cited by 11 publications

References 2 publications

Plasticized Polymer Composite Single-Ion Conductors for Lithium Batteries

Plasticized Polymer Composite Single-Ion Conductors for Lithium Batteries

Comparison of intermolecular interactions in two phases of MeNSOF2

N‐(Fluorformyl)iminoschwefeldichlorid und N‐(Chlorformyl)iminoschwefeldichlorid

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Comparison of intermolecular interactions in two phases of MeNSOF₂