Electron-diffraction study of hexamethyl digermoxane [(CH3)3Ge]2O and hexamethyl distannoxane [(CH3)3Sn]2O in vapor

Vilkov, L. V.; Tarasenko, N. A.

doi:10.1007/bf00745917

Cited by 16 publications

(24 citation statements)

References 4 publications

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“…The chemical shifts of the CF 3 and CF 2 groups in the 19 FNMR spectrum of the bromogermane (C 2 F 5 ) 3 GeBr are comparable with those of (C 2 F 5 ) 3…”

Section: Resultsmentioning

confidence: 69%

“…The 19 FNMR spectrum shows as inglet at À81.9 ppm for the CF 3 group and as inglet at À115.2 ppm for the CF 2 group.…”

Section: Resultsmentioning

confidence: 95%

“…As mentioned before, the reaction of (C 2 F 5 ) 3 GeNEt 2 with gaseous HCl yields the chlorogermane (C 2 F 5 ) 3 GeCl. The 19 FNMR spectrumi sa se xpected (Table 1).…”

Section: Resultsmentioning

confidence: 99%

“…(5)]. T he volatile solid was analysed and characterized by 19 F, 13 CNMR and IR spectroscopy,EIm ass spectrometry,and X-ray diffraction.…”

Section: Resultsmentioning

confidence: 99%

“…[16] This angle is more obtuse than in the nonfluorinated germanes( H 3 Ge) 2 O( 126.58), [17] (Ph 3 Ge) 2 O( 135.2(2)8) [18] and [(CH 3 ) 3 Ge] 2 O( 1418). [19] The GeÀOs eparations of 175.0(2) pm and 174. 3(1) pm are also comparablew ith those in the trifluoromethyld erivative (172 pm), [16] but 2-3 pm shorter than in (H 3 Ge) 2 O( 176 pm), (Ph 3 Ge) 2 O( 176.5(3)/176.9(3) pm), [18] and [(CH 3 ) 3 Ge] 2 O( 177.0 pm).…”

Section: Resultsmentioning

confidence: 99%

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Synthesis of Tris(pentafluoroethyl)germanes

Pelzer

Neumann

Stammler

et al. 2016

Chemistry A European J

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The synthesis of tris(pentafluoroethyl)germanium derivatives is described. The reaction of germanium tetrachloride with three equivalents of the pentafluoroethylation reagent LiC F does not lead selectively to the formation of tris(pentafluoroethyl)chlorogermane, (C F ) GeCl. Here the introduction of a diethylamino function as a protecting group was beneficial. Thus, treatment of Cl GeNEt with LiC F smoothly afforded (C F ) GeNEt . The replacement of the amino substituent by halides was accomplished by reaction with HBr or HCl on a multigram scale. The combination of (C F ) GeCl with Ag CO gave rise to the formation of the digermoxane [(C F ) Ge] O. An obtuse Ge-O-Ge angle of 150.2(1)° was determined by X-ray diffraction. Attempted hydrolysis of the digermoxane leads to an equilibrium mixture of the precursor, (C F ) GeOH, and water.

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“…The chemical shifts of the CF 3 and CF 2 groups in the 19 FNMR spectrum of the bromogermane (C 2 F 5 ) 3 GeBr are comparable with those of (C 2 F 5 ) 3…”

Section: Resultsmentioning

confidence: 69%

“…The 19 FNMR spectrum shows as inglet at À81.9 ppm for the CF 3 group and as inglet at À115.2 ppm for the CF 2 group.…”

Section: Resultsmentioning

confidence: 95%

“…As mentioned before, the reaction of (C 2 F 5 ) 3 GeNEt 2 with gaseous HCl yields the chlorogermane (C 2 F 5 ) 3 GeCl. The 19 FNMR spectrumi sa se xpected (Table 1).…”

Section: Resultsmentioning

confidence: 99%

“…(5)]. T he volatile solid was analysed and characterized by 19 F, 13 CNMR and IR spectroscopy,EIm ass spectrometry,and X-ray diffraction.…”

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

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Synthesis of Tris(pentafluoroethyl)germanes

Pelzer

Neumann

Stammler

et al. 2016

Chemistry A European J

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Structural Tin Chemistry

Zubieta

Zuckerman

1978

Progress in Inorganic Chemistry

185

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Darstellung und Eigenschaften von Bis‐tris(trifluormethyl)‐ germyl‐chalkogeniden, (CF₃)₃GeEGe(CF₃)₃ (E = O, S, Se, Te) Die Molekülstruktur des [(CF₃)₃Ge]₂O

Eujen¹,

Laufs²,

Oberhammer³

1988

Zeitschrift anorg allge chemie

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Die Verbindungen [(CF3)3Ge]2E (E = O, S, Se) wurden durch Umsetzung von (CF3)3GeI mit Ag2E, [(CF3)3Ge]2Te aus (CF3)3GeI und Li2Te Bzw. aus (CF3)3GeF und Te(SiMe3)2 dargestellt und in ihren physikalischen, chemischen und spektroskopischen Eigenschaften charakterisiert. Durch Hydrolyse des Oxids oder Sulfids bzw. ihre Umsetzung mit überschüssigem H2S wurde das nur im Gleichgewicht mit H2E beständige (CF3)3GeEH (E = O, S) erzeugt und schwingungsspektroskopisch unter Einbeziehung der deuterierten Spezies charakterisiert. Für die oberhalb von 100° C ohne CF2‐Eliminierung ablaufende Thermolyse wurden unterschiedliche Reaktionswege gefunden. Die Molekülstruktur des Oxids (CF3)3GeOGe(CF3)3 wurde durch Elektronenbeugungsmethoden bestimmt: ra(GeO) 172,4(6) pm, ra(GeC) 200,4(4) pm, ra(CF) 133,7(2) pm, ∢GeOGe 151,5(14)°. Die Molekülparameter werden unter Einbeziehung von aus schwingungsspektroskopischen Analysen abgeleiteten Daten diskutiert.

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Electron-diffraction study of hexamethyl digermoxane [(CH3)3Ge]2O and hexamethyl distannoxane [(CH3)3Sn]2O in vapor

Cited by 16 publications

References 4 publications

Synthesis of Tris(pentafluoroethyl)germanes

Synthesis of Tris(pentafluoroethyl)germanes

Structural Tin Chemistry

Darstellung und Eigenschaften von Bis‐tris(trifluormethyl)‐ germyl‐chalkogeniden, (CF₃)₃GeEGe(CF₃)₃ (E = O, S, Se, Te) Die Molekülstruktur des [(CF₃)₃Ge]₂O

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Electron-diffraction study of hexamethyl digermoxane [(CH3)3Ge]2O and hexamethyl distannoxane [(CH3)3Sn]2O in vapor

Cited by 16 publications

References 4 publications

Synthesis of Tris(pentafluoroethyl)germanes

Synthesis of Tris(pentafluoroethyl)germanes

Structural Tin Chemistry

Darstellung und Eigenschaften von Bis‐tris(trifluormethyl)‐ germyl‐chalkogeniden, (CF3)3GeEGe(CF3)3 (E = O, S, Se, Te) Die Molekülstruktur des [(CF3)3Ge]2O

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Darstellung und Eigenschaften von Bis‐tris(trifluormethyl)‐ germyl‐chalkogeniden, (CF₃)₃GeEGe(CF₃)₃ (E = O, S, Se, Te) Die Molekülstruktur des [(CF₃)₃Ge]₂O