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  • preparation  (2)
  • 19F  (1)
  • Calculations, ab initio  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Structure of O-Methyl-N,N-bis(trifluoromethyl)hydroxylamine, (CF3)2NOCH3 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 653-656 
    Details
    ISSN: 0009-2940
    Keywords: Hydroxylamine, O-methyl-N,N-bis(trifluoromethyl)-, gas-phase structure of ; Electron diffraction ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The molecular structure of (CF3)2NOCH3 was determined by gas electron diffraction. The molecular intensities were reproduced by use of a single conformation with syn orientation of the O-CH3 group relative to the nitrogen lone pair. This was confirmed by ab initio calculations (HF/3-21G(*), polarization functions only on nitrogen, and MP2/6-31G*). The observed structure demonstrates that the generalized anomeric effect is of minor importance to this compound. The following skeletal geometric parameters (bond lengths [pm] and angles [°] with 3-s̰ uncertainties) were derived: N-C 142.9(7), N-O 142(3), O-C 145(3), CNC 118.0(9), CNO 108.1(17), and NOC 109.4(17). The experimental structure is well reproduced by the ab initio calculations.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290610
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  • 2
    Electronic Resource
    Electronic Resource
    Darstellung und spektroskopische Charakterisierung der Persulfoniumsalze (CH3)(CF3)SF3+SbF6- und (CH3)(CF3)2SF2+SbF6- und Kristallstruktur von CF3SF2+SbF6- (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 174-180 
    Details
    ISSN: 0044-2313
    Keywords: Persulfonium salts ; preparation ; vibrational spectra ; NMR spectra ; crystal structure of CF3SF2+SbF6- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Spectroscopic Characterization of the Persulfonium Salts (CH3)(CF3)SF3+SbF6- and (CH3)(CF3)2SF2+SbF6- and Crystal Structure of CF3SF2+SbF6- [1].The preparation of the persulfonium salts (CH3)(CF3)SF3+SbF6- and (CH3)(CF3)2SF2+SbF6- by methylation of the sulfuranes CF3SF3 and (CF3)2SF2 with CH3OSO+SbF6- in liquid SO2 is reported. The thermolabile compounds are characterized by IR, Raman, 1H, 13C, and 19F NMR spectroscopy.CF3SF2+SbF6- crystallizes in the space group C2/c with a=16.889(8) Å, b=7.261(4) Å, c=13.416(7) Å, β=91.08° with 8 formula units per unit cell at 167 K. Cations and anions are connected via short SF contacts forming a Ψ-octahedral surrounding of the central S atom which is in close analogy to the already known CF3SF2+AsF6-.
    Notes: Es wird über die Darstellung der Persulfoniumsalze (CH3)(CF3)SF3+SbF6- und (CH3)(CF3)2SF2+SbF6- durch Methylierung der Sulfurane CF3SF3 und (CF3)2SF2 mit CH3OSO+SbF6- in flüssigem SO2 berichtet. Die thermolabilen Verbindungen werden durch IR-, Raman-, 1H-, 13C- und 19F-NMR-Spektroskopie charakterisiert. CF3SF2+SbF6- kristallisiert in der Raumgruppe C2/c mit a=16,889(8) Å, b=7,261(4) Å, c=13,416(7) Å, β=91,08° und 8 Formeleinheiten pro Einheitszelle bei 167 K. Kationen und Anionen sind über kurze SF-Kontakte verbunden und bilden eine Ψ-oktaedrische Umgebung des zentralen S-Atoms. Diese Struktur stimmt gut mit der des bereits bekannten CF3SF2+AsF6- überein.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190129
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  • 3
    Electronic Resource
    Electronic Resource
    Darstellung von Tetramethylammoniumbistrifluormethoxybromat(I) (CH3)4N+Br(CF3O)2- (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 487-490 
    Details
    ISSN: 0044-2313
    Keywords: Tetramethylammonium bistrifluormethoxybromate(I) ; vibrational spectra ; 19F ; 13C NMR ; mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of Tetramethylammonium Bistrifluormethoxybromate(I) (CH3)4N+Br(CF3O)2-We describe the preparation and characterization of (CH3)4N+Br(CF3O)2-. It is prepared via comproportionation of CF3OCl with (CH3)4N+BrCl2- under formation of Cl2 at -70°C, respectively via addition elimination reaction of CF3OCl with (CH3)4N+Br- at -70°C. The thermolabile salt is characterized by i.r., Raman, 19F, 13C NMR and mass spectroscopy.
    Notes: Es wird über die Darstellung und Charakterisierung von (CH3)4N+Br(CF3O)2- berichtet. (CH3)4N+Br(CF3O)2- erhält man sowohl durch Komproportionierung von CF3OCl mit (CH3)4N+BrCl2- bei -70°C unter Bildung von elementarem Chlor, als auch über die Additions-Eliminierungsreaktion von CF3OCI mit (CH3)4N+Br bei-70°C. Die thermolabile Verbindung wird durch IR-, Raman-, 19F-, 13C-NMR sowie Massenspektroskopie charakterisiert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230177
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  • 4
    Electronic Resource
    Electronic Resource
    Über die Darstellung von Di(i-propyl)thiosulfonium-Salzen (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 557-561 
    Details
    ISSN: 0044-2313
    Keywords: Thiosulfonium salts ; preparation ; vibrational, NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Preparation of Di(i-propyl)thiosulfonium Salts [1]The preparation of the mercaptosulfonium salts (i-C3H7)2SSX+SbCl6- (X = H, D) and of the chlorothiosulfonium salts (i-C3H7)2SSCl+MF6- (M = As, Sb) and (i-C3H7)2SSSCl+SbCl6- is reported. They are formed by reaction of chlorinated or protonated (i-C3H7)2S with excess H2S or SCl2 and S2Cl2. The thiosulfonium compounds are characterized by vibrational and NMR spectroscopic methods.
    Notes: Es wird über die Darstellung der Mercaptosulfoniumsalze (i-C3H7)2SSX+SbCl6- (X = H, D) und der Chlorthiosulfoniumsalze (i-C3H7)2SSCl+MF6- (M = As, Sb) und (i-C3H7)2SSSCl+SbCl6- berichtet. Sie werden aus chloriertem oder protoniertem (i-C3H7)2S durch Kondensationsraktionen mit überschüssigem H2S oder SCl2 und S2Cl2 gebildet. Die Charakterisierung der Thiosulfoniumverbindungen erfolgt schwingungs- und NMR-spektroskopisch.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220328
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