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  • preparation  (19)
  • crystal structure  (4)
  • NMR-Spectra  (2)
  • (difluoro)methylphosphine  (1)
  • Wiley-Blackwell  (23)
  • 1
    Electronic Resource
    Electronic Resource
    Preparation of Pseudohalidoheptasulfur(+1) Hexafluorometallates S7X+MF-6 (X = CN, OCN, SeCN; M = As, Sb) (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 96-100 
    Details
    ISSN: 0044-2313
    Keywords: Cycloheptasulfur cations ; preparation ; ir., n.m.r., RA, m.s. spectra ; stabilities ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung der Pesudohalogenheptaschwefel(+1)-hexaflourmatellate S7X+MF-6 (X = CN, OCN, SCN, SeCN; M = As, Sb)Es wird über die Darstellung und spektroskopische Charakterisierung von S7X+MF-6 (X = CN, OCN, SCN, SeCN; M = As, Sb) berichtet. Die Verbindungen werden in Analogie zur Darstellung der Halogencycloheptaschwefel(+1)-Kationen aus S2+8(MF-6)2 und Alkalimetallpseudohalogeniden in Schwefeldioxid als Lösungsmittel gebildet. Ihre thermische Stabilität nimmt mit wachsender „Pearson Härte“ der Pseudohalogenliganden ab.
    Notes: The preparation and spectroscopic characterization of S7X+MF-6 (X = CN, OCN, SCN, SeCN; M = As, Sb) is reported. The new compounds are formed in analogy to the preparation of halidocycloheptrasulfur(+1) cations from S2+8(MF-6)2 and alkali pseudohalides in So2 as solvent. Their thermal stabilities decrease with the increasing Pearson hardness of the pseudohalide ligands.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926070116
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  • 2
    Electronic Resource
    Electronic Resource
    Darstellung und spektroskopische Charakterisierung von Fluortrichlor-arsoniumhexafluoroarsenat, AsFCl3+AsF6-Wir danken dem Minister für Wissenschaft und Forschung des Landes Nordrhein-Westfalen für die finanzielle Unterstützung dieser Arbeit. (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 175-176 
    Details
    ISSN: 0044-2313
    Keywords: AsFCl3+ AsF6- ; preparation ; vibrational analysis ; 19F-NMR spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Spectroscopic Characterization of Fluorotrichloroarsonium Hexafluoroarsenate, AsFCl3+AsF6-The mixed halide pniktide cation AsFCl3+ is prepared by oxidative fluorination of AsCl3 with XeF+ AsF6-. AsFCl3+ AsF6- is characterized by IR, Raman, and 19F-NMR spectroscopy.
    Notes: Durch oxidative Fluorierung von AsCl3 mit XeF+ AsF6- wird das gemischt-halogenierte Pniktid-Kation AsFCl3+ hergestellt. AsFCl3+ AsF6- wird durch IR-, Raman- und 19F-NMR-Spektren charakterisiert.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926070131
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  • 3
    Electronic Resource
    Electronic Resource
    Darstellung und spektroskopische Charakterisierung der Fluorphosphonium-Salze X2FPSCH3+MF6- (X = Br, Cl; M = As, Sb) und XF2PSCH3+SbF6- (X = Br, Cl, F) (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 40-44 
    Details
    ISSN: 0044-2313
    Keywords: Fluorophosphonium salts ; preparation ; vibrational spectra ; NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Spectroscopic Characterization of the Fluorophosphonium Salts X2FPSCH3+MF6- (X = Br, Cl; M = As, Sb) and XF2PSCH3+SbF6- (X = Br, Cl, F)The preparation of the fluorophosphonium salts X2FPSCH3+MF6- (X = Br, Cl; M = As, Sb) and XF2PSCH3+SbF6- (X = Br, Cl, F) by methylation of the corresponding thiophosphorylhalides in the system CH3F/SO2/MF5 (M = As, Sb) is reported. The new salts are characterized by their vibrational and NMR spectra.
    Notes: Es wird über die Darstellung der Fluorphosphoniumsalze X2FPSCH3+MF6- (X = Br, Cl; M = As, Sb) and XF2PSCH3+SbF6- (X = Br, Cl, F) durch oxidative Methylierung der korrespondierenden Thiophosphorylhalogenide mit dem System CH3F/SO2/MF5 (M = As, Sb) berichtet. Die Salze werden durch ihre Schwingungs- und NMR-Spektren charakterisiert.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926120108
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  • 4
    Electronic Resource
    Electronic Resource
    The reaction of XeF+MF6- (M = As, Sb) with sulfuranes; preparation of CF3(O)F2+SbF6- and (CF3)2SOXeF+SbF6- (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 35-39 
    Details
    ISSN: 0044-2313
    Keywords: CF3S(O)F2 +SbF6- ; (CF3)2SOXeP+SbF6- ; preparation ; vibrational spectra ; NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die Reaktion von XeF+SbF6- mit Sulfuranen; Präparation von CF3S(O)F2+SbF6- und (CF3)2SOXeF+SbF6-CF3S(O)F, (CF3)2SO, CF3SF3, (CF3)2SF2, und SF4 reagieren in unterschiedlicher Weise mit XeF+MF6- (M=As, Sb). Eine oxidative Fluorierung wird beobachtet beim CF3S(O)F unter Bildung des Persulfoniumsalzes CF3S(O)F2+SbF6-, während mit (CF3)2SO ein einfaches Xenon-enthaltendes Additionsprodukt (CF3)2SOXeF+SbF6- isoliert werden kann. Im Gegensatz dazu führt der Lewis-saure Charakter des XeF+ -Kations gegenüber (CF3)nSF4-n (n = 0 - 2) zu den entsprechenden Fluorsulfoniumsalzen (CF3)nSF3-n +MF6- (M=As. Sb) und XeF2.
    Notes: CF3S(O)F, (CF3)2SO, CF3SF3, (CF3)2SF2, and SF4 react in different manner with XeF+MF6- (M=As, Sb). An oxidative fluorination is observed by CF3S(O)F forming the persulfonium salt CF3S(O)F2+SbF6-, whereas by (CF3)2SO a simple addition product containing xenon can be isolated in form of the sulfonium salt (CF3)2SOXeF+SbF6-. On the contrary, the Lewis-acidic character of the XeF+-cation predominates against (CF3)nSF4-n (n = 0 - 2) leading to the corresponding fluorosulfonium salts (CF3)nSF3-n +MF6- (M=As, Sb) and XeF2.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926120107
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  • 5
    Electronic Resource
    Electronic Resource
    Über die Darstellung der Dichlormethylen-halogensulfenium-Salze Cl2CSCl+ AsF6- und Cl2CSBr+ AsF6- [1] (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 583-586 
    Details
    ISSN: 0044-2313
    Keywords: Sulfenium Salts ; Preparation ; Vibrational Spectra ; NMR-Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Synthesis of the Dichloromethylene-halogenosulfenium Salts Cl2CSCl+ AsF6- and Cl2CSBr+ AsF6-The sulfenium salts Cl2CSCl+ AsF6- and Cl2CSBr+ AsF6- are synthesized by oxidative halogenation of thiophosgene, Cl2CS with X2/AsF5 (X = Cl, Br) at 195 K and are characterized by vibrational as well as NMR spectroscopy.
    Notes: Die Sulfeniumsalze Cl2CSCl+ AsF6- und Cl2CSBr+ AsF6- werden aus Thiophosgen Cl2CS durch oxidative Halogenierung mit X2/AsF5 (X = Cl, Br) bei 195 K dargestellt und schwingungs- sowie NMR-spektroskopisch charakterisiert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190325
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  • 6
    Electronic Resource
    Electronic Resource
    Über die Kristallstrukturen von CH3PF2H+AsF6- und CH3PF2H+SbF6- und eine einfache Darstellung von CH3PF2 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 509-513 
    Details
    ISSN: 0044-2313
    Keywords: (difluoro)methylphosphine ; (difluoro)methylphosphonium salts ; preparation ; single crystall X-ray structure ; vibrational and NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structures of CH3PF2H+AsF6- and CH3PF2H+SbF6- and a simple Method for Preparation of CH3PF2A simple method for preparation of CH3PF2 from CH3PCl2 is reported. The phosphonium salts CH3PF2H+MF6- are obtained by the reaction of CH3PCl2 with superacidic systems HF/MF5 (M = As, Sb). CH3PF2H+SbF6- crystallizes in the space group P1 with a = 548.4(4) pm, b = 695.5(8) pm, c = 960.2(9) pm, α = 94.68(5)°, β = 97.19(6)°, γ = 94.41(6)° and Z = 2. CH3PF2H+SbF6- crystallizes in P1 with a = 554.3(3), b = 724.2(4), c = 970.4(5), α = 94.73(4)°, β = 96.14(5)°, γ = 95.30(4)°.
    Notes: Es wird über eine einfache Darstellung von CH3PF2 aus CH3PCl2 berichtet, welches in den supersauren Systemen HF/MF5 (M = As, Sb) zu den Phosphoniumsalzen CH3PF2H+MF6- protoniert wird. CH3PF2H+AsF6- kristallisiert in der Raumgruppe P1 mit a = 548,4(4) pm, b = 695,5(8) pm, c = 960,2(9) pm, α = 94,68(5)°, β = 97,19(6)°, γ = 94,41(6)° und Z = 2, das isostrukturelle CH3PF2H+SbF6- mit a = 554,3(3), b = 724,2(4), c = 970,4(5), α = 94,73(4)°, β = 96,14(5)°, γ = 95,30(4)°.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200319
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  • 7
    Electronic Resource
    Electronic Resource
    Über die Darstellung der Bis(triphenylsilyl)-sulfane (C6H5)3Si—Sx—Si(C6H5)3 (x = 3, 4) und die Kristallstruktur von (C6H5)3Si—S4—Si(C6H5)3Professor Friedo Huber zum 65. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 981-986 
    Details
    ISSN: 0044-2313
    Keywords: Bis(triphenylsilyl)sulfanes ; preparation ; single crystal X-ray structure ; vibrational spectra ; NMR spectra ; UV-VIS spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Preparation of Bis(triphenylsilyl)sulfanes (C6H5)3Si—Sx—Si(C6H5)3 (x = 3, 4) and the Crystal Structure of (C6H5)3Si—S4—Si(C6H5)3The preparation of the bis(triphenylsilyl)sulfanes Ph3Si—Sx—SiPh3 (x = 3, 4) from Ph3SiSNa and SCl2 resp. S2Cl2 is reported. They are characterized by vibrational, NMR and UV-VIS spectroscopic measurements. Ph3Si—S4—SiPh3 crystallizes in space group P1 with a = 943.6(6) pm, b = 945.7(5) pm, c = 1 881.7(12) pm, α = 82.11(5)°, β = 78.95(5)°, γ = 83.15(5)° and Z = 2.
    Notes: Es wird über die Darstellung der Bis(triphenylsilyl)-sulfane Ph3Si—Sx—SiPh3 (x = 3, 4) aus Ph3SiSNa und SCl2 bzw. S2Cl2 berichtet. Ihre Charakterisierung erfolgt schwingungs-, NMR-, und UV-VIS-spektroskopisch.Ph3Si—S4—SiPh3 kristallisiert in der Raumgruppe P1 mit a = 943,6(6) pm, b = 945,7(5) pm, c = 1 881,7(12) pm, α = 82,11(5)°, β = 78,95(5)°, γ = 83,15(5)° und Z = 2.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200605
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  • 8
    Electronic Resource
    Electronic Resource
    Reaktion von Chlornitrat mit CF3I: Isolierung von Trifluormethylchloriodnitrat CF3I(Cl)ONO2 und Kristallstruktur von Trifluormethylioddinitrat CF3I(ONO2)2 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1552-1557 
    Details
    ISSN: 0044-2313
    Keywords: Chlorine Nitrate ; Trifluormethylchloroiodinenitrate ; Trifluormethyliodinedinitrate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Chlorine Nitrate with CF3I: Isolation of Trifluormethylchloroiodinenitrate CF3I(Cl)ONO2 and the Crystal Structure of Trifluormethyliodinedinitrate CF3I(ONO2)2CF3I reacts with ClONO2 to Iodine(III)-compounds. After an addition CF3I(Cl)ONO2 is isolated and characterized by vibrational spectra. With surplus ClONO2 it is formed CF3I(ONO2)2.CF3I(ONO2)2 crystallizes monoclinic in the space group P21/c with the cell parameters a = 1 024.3(6) pm, b = 873.5(6) pm, c = 873.4(6) pm and Z = 4.We measered following bonding distances: I—O: 207.3(3) and 220.8(2) pm, I—C: 221.1(4) pm and N—O: from 119.1(4) to 141.5(3) pm.Through an intermolecular I ··· O-contact the central iodine becomes a distorted plane geometry.
    Notes: CF3I reagiert mit ClONO2 in einer oxidativen Additionsreaktion zu Iod(III)-Verbindungen. Das Additionsprodukt CF3I(Cl)ONO2 wird isoliert und schwingungsspektroskopisch charaktersiert. Mit überschüssigem ClONO2 bildet sich CF3I(ONO2)2.CF3I(ONO2)2 kristallisiert monoklin in der Raumgruppe P21/c mit a = 1 024,3(6) pm, b = 873,5(6) pm, c = 873,4(6) pm und Z = 4.Es werden folgende Bindungslängen gemessen: I—O: 207,3(3) bzw. 220,8(2) pm, I—C: 221,2(4) pm und N—O: 119,1(4) bis 141,5(3) pm.Durch einen intermolekularen I ··· O-Kontakt erlangt das zentrale Iodatom eine verzerrt-planare Umgebung.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210920
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  • 9
    Electronic Resource
    Electronic Resource
    Darstellung von Cyanhalogenmethyl- und Dicyanhalogensulfoniumsalzen CH3(CN)SHal+MF6- und (CN)2 SHal+MF6- (Hal = F, Cl, Br, I; M = As, Sb) sowie von Methylthionitrillium- und (μ-Thio)bisnitriliumhexafluorometallaten CH3SCNX+MF6- und S(CNH)22+ (MF6-)2 (X = H, D) (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 77-88 
    Details
    ISSN: 0044-2313
    Keywords: Cyanhalogenomethyl salts ; dicyanhalosulfonium salts ; methylthionitrilium metallates ; (μ-thio)bisnitriliumhexafluoro metallates ; preparation ; i.r., n.m.r. data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of Cyanhalogenomethyl and Dicyanhalogensulfonium Salts CH3(CN)SHal+MF6- and (CN)2SHal+MF6- (Hal = F, Cl, Br, I; M = As, Sb) and Methylthionitrilium and (μ-Thio)bisnitriliumhexafluoro Metallates CH3SCNX+MF6- and S(CNH)22+ (MF6-)2 (X = H, D)Oxidative halogenation of CH3SCN and S(CN)2 with XeF+MF6-, Cl2/MF5/SO2, Br2/MF5/SO2 and I3+MF6- leads to S-coordinated cations. The complete spectroscopic series of the halogensulfonium salts CH3S(CN)Hal+MF6- and (CN)2SHal+MF6- (Hal = F, Cl, Br, I; M = As, Sb) as well as hexafluoroarsenate and -antimonate were recorded.However the protonation of divalent cyansulfanes in superacidic media HF/MF5 takes place at the nitrogen atom to nitrilium salts in analogy to the adduct formation with strong Lewis acids.
    Notes: Bei der oxidativen Halogenierung von CH3SCN und S(CN)2 mit XeF+MF6-, Cl2/MF5/SO2, Br2/MF5/SO2 und I3+MF6- erfolgt eine Koordination am Schwefel, und es wurden die kompletten spektroskopischen Reihen der S-Halogensulfoniumsalze CH3S(CN)Hal+MF6- und (CN)2SHal+MF6-(Hal = F, Cl, Br, I; M = As, Sb) jeweils als Hexafluoroarsenat und -antimonat hergestellt.Dagegen erfolgt die Protonierung der divalenten Cyansulfane im supersauren Milieu HF/MF5 am Stickstoff zu Nitriliumsalzen analog wie die Koordination bei der Adduktbildung mit starken Lewissäuren.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915960111
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  • 10
    Electronic Resource
    Electronic Resource
    Über die Darstellung der Dimercapto(methyl)sulfonium-Salze[CH3S(SH)2]+AsF-6 und [CH3S(SH)2]+SbCl-6 und der Bis(chlorthio)Methylsulfonium-Salze [CH3S(SCI)2]+ AsF6-und [CH3S(SCL)2]+SbCl-6Professor Peter Sartori zum 60. Geburtstage am 19. Dezember 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 605 (1991), S. 101-107 
    Details
    ISSN: 0044-2313
    Keywords: dimercapto(methyl)sulfonium salts ; bis(chlorothio)methylsulfonium ; salts ; preparation ; Ramanspectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Preparation of Dimercapto(methyl)Sulfonium Salts [CH3S(SH)2]+ AsF6- and [CH3S(SH)2]+SbCl6- and the Bis(chlorothio)methylsulfonium Salts [CH3S(SCI)2]+ AsF6- and [CH3S(SCI)2]+ SbCl6-The preparation of the dimercapto(methyl)sulfonium salts [CH3S(SH)2]+ AsF6- and [CH3S(SH)2]+SbCl6- from [CH3SCl2]+ salts and H2S at 195 K is reported. The salts are stable below 210 K. They are characterized by additional Raman spektroscopic measurements of the isotopic labelled cations [CH3S(SD)2]+, [CH3S(34SH)2]+ and [CH3S(34SD)2]+. The dimercapto(methyl)sulfonium salts are transfered into bis(chlorthio)methylsulfonium salts by reaction with Cl2 at 195 K.
    Notes: Es wird über die Darstellung der Dimercapto(methyl)sulfoniumsalze [CH3S(SH)2]+ AsF6- und [CH3S(SH)2]+SbCl6- aus den [CH3SCl2]+-salzen und H2S bei 195 K berichtet. Beide Verbindungen sind unterhalb 210 K haltbar. Ihre Charakterisierung erfolgt Raman-spektroskopisch durch zusätzliche Messungen an den markierten Kationen [CH3S(SD)2]+, [CH3S(34SH)2]+ und [CH3S(34SD)2]+. Beide [CH3S(SH)2]+-Salze reagieren mit Chlor zu den Bis(chlorthio)methylsulfonium-salzen [CH3S(SCl)2]+AsF6- und [CH3S(SCl)2]+SbCl6-.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916050111
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