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  • 11
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 91 (1958), S. 1947-1950 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ein neues Verfahren zur Herstellung von Heptaschwefelimid, S7NH, wird be-schrieben. Es beruht auf der Umsetzung zwischen Ammoniak und Schwefel-chloriden in Dimethylformamid als Lösungsmittel.
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  • 12
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 56-62 
    ISSN: 0044-2313
    Keywords: 1λ5,3λ5-diphosphete ; addition compounds with GeCl2, SnCl2, (CO)5W(Z-cyclooctene) ; n.m.r., i.r., mass spectra ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphete as Ligand in Coordination Compounds1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphete, 1, reacts with GeCl2 · 1,4-dioxane, SnCl2, and (CO)5W(Z-cyclooctene) to give the complexes {HCP[N(CH3)2]2}2 · GeCl2, 3, {HCP[N(CH3)2]2}2 · SnCl2, 4, and {HCP[N(CH3)2]2}2 · W(CO)5, 5, respectively. The n.m.r., mass, and i.r. spectra of the new compounds as well as the crystal and molecular structures of 3 and 4 are reported and the bonding situation in compounds 3-5 is discussed.
    Notes: 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet, 1 bildet mit GeCl2 · 1,4-Dioxan, SnCl2 bzw. (CO)5W(Z-cycloocten) die komplexe {HCP[N(CH3)2]2}2 · GeCl2, 3, {HCP[N(CH3)2]2}2 · SnCl2, 4, bzw. {HCP[N(CH3)2]2}2 · W(CO)5, 5. Die NMR-, Massen- und IR-Spektren der neuen Verbindungen sowie die Kristall- und Molekülstruktur von 3 und 4 werden mitgeteilt und die Bindungsverhältnisse in den Verbindungen 3-5 diskutiert.
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  • 13
    ISSN: 0044-2313
    Keywords: Diaminophosphanylethylene ; mono- and bis(difluorophosphoranyl)-ethylene ; n-hexylidene-fluorophosphorane ; 2,4-di-n-pentyl-1λ5, 3λ5 -diphosphete; n. m. r., ir spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mono- and Bis(difluorophosphoranyl)ethylene, n-Hexylidene-fluorophosphorane, and a 2,4-Di-n-pentyl-1λ5, 3λ5 -diphospheteBis(diethylamino)phosphanylethylene, 1, is converted by SF4 into bis(diethylamino)difluorophosphoranylethylene, 2. Analogously trans-1,2-bis(diphenylphosphanyl)ethylene, 3, is converted into trans-1,2-bis(difluorodiphenylphoranyl)ethylene, 4. 2 reacts with n-butyllithium to give n-hexylidene-bis(diethylamino)fluorophosphorane, 5. With more n-butyllithium, the main product n-hexylidene-bis(diethylamino)-n-butylphosphorane, 7, and the by-product 2,4-di-n-pentyl-1,1,3,3-tetrakis(diethylamino)-1λ5, 3λ5 -diphosphete, 8, are formed. With t-butyllithium 2 yields 3,3-dimethyl-butylidene-bis(diethylamino)fluorophosphorane, 6. All new compounds 1, 2, 4-8 are characterized by their nmr and ir spectra.
    Notes: Bis(diethylamino)phosphanylethylen, 1, wird durch SF4 in Bis(diethylamino)difluorphosphoranylethylen, 2, übergeführt. Auf analoge Weise entsteht aus trans-1,2-Bis(diphenylphosphanyl)ethylen, 4. 2 reagiert mit n-Butyllithium zu n-Hexyliden-bis(diethylamino)fluorphosphoran, 5, aus dem mit weiterem n-Butyllithium als Hauptprodukt n-Hexyliden-bis(diethylamino)-n-butylphosphoran, 7, und als Nebenprodukt 2,4-Di-n-pentyl-1,1,3,3-tetrakis(diethylamino)-1λ5, 3λ5-diphosphet, 8, entsteht. Mit t-Butyllithium bildet 2 3,3-Dimethyl-butyliden-bis(diethylamino)fluorphosphoran, 6. Alle neuen Verbindungen 1, 2, 4-8 werden durch ihre NMR- und IR-Spektren charakterisiert.
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  • 14
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 483-488 
    ISSN: 0044-2313
    Keywords: o-1λ5,3λ5-Diphosphaphenylene-bis(diphenylphosphane) ; nickel(II) chloride chelate complex ; crystal structure ; NMR, Ir spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: o-1λ5,3λ5-Diphosphaphenylene-bis(diphenylphosphane) and its Chelating PropertiesBis(diphenylphosphanyl)acetylene and 1,1′,3,3′-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete react at higher temperatures to yield the title compound 5, which forms easily the chelate complex 6 with nickel(II) chloride.
    Notes: Bis(diphenylphosphanyl)acetylen und 1,1′,3,3′-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet reagieren bei höheren Temperaturen zur Titelverbindung 5, die mit Nickel(II)-chlorid leicht den Chelatkomplex 6 bildet.
    Additional Material: 3 Ill.
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  • 15
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of 1,1,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5-diphosphete with Monosubstituted Acetylenes and Acetylene. 1λ5, 3λ5-Diphosphabenzenes. IVThe monosubstituted acetylenes H—C≡C—COOCH3 and H—C≡C—CF3 react with 1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete 1 to give 1,1,3,3-tetrakis (dimethylamino)- 4-methoxycarboxylato-1λ5,3λ5-diphosphorine 3, and -4-trifluoromethyl-1λ5,3λ5-diphosphorine 5, respectively. In contrast, phenylacetylene and 1 form two isomers, namely 1,1,3,3- tetrakis(dimethyl-amino)-4-phenyl-1λ5,3λ5-diphosphorine 4a und -5-phenyl-1λ5,3λ5-diphosphorine 4b. The reaction between acetylene and 1 yields the 1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphorine 6, unsubstituted at the carbon atoms of the ring. Various mechanisms are discussed for the formation of the compounds 3, 4a, 4b, 5 and 6. All new compounds are characterized by their n.m.r., mass, and i.r. spectra.
    Notes: Die monosubstituierten Acetylene H—C≡C—COOCH3 und HC≡C—CF3 reagieren mit 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet 1 zu 1, 1, 3, 3-Tetrakis(dimethylamino)- 4-methoxycarboxylato-1λ5,3λ5-diphosphorin 3 bzw. -4-trifluormethyl-1λ5,3λ5-diphosphorin 5. Im Gegensatz dazu bildet Phenylacetylen mit 1 zwei Isomere, nämlich 1,1,3,3- Tetrakis(dimethylamino)-4-phenyl-1λ5,3λ5-diphosphorin 4a und -5-phenyl-1λ5,3λ5-diphosphorin 4b. Acetylen und 1 reagieren zu dem an den Kohlenstoffatomen des Rings unsubstituierten 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphorin 6. Für die Bildung der Verbindungen 3, 4a, 4b, 5 und 6 werden verschiedene Mechanismen diskutiert. Alle neuen Verbindungen sind durch ihre NMR-, Massen- und IR-Spektren charakterisiert.
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  • 16
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 601 (1991), S. 65-72 
    ISSN: 0044-2313
    Keywords: 1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete ; hydrolysis ; bis(dimethylamino)-phosphorylmethylidene-methyl-bis(dimethylamino)phosphorane ; bis(dimethylamino)phosphoryl-methyl(dimethylamino)phosphonylmethylene ; nmr, mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrolysis of 1,1,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5 -diphospheteHydrolysis of 1,1,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5 -diphosphet (2) yields in the first step Bis(dimethylamino)phosphorylmethyliden-methyl-bis(dimethylamino)phosphorane (5). In the second step Bis(dimethylamino)phosphoryl-methyl(dimethylamino)phosphosphonylmethylen (6) is the main product of hydrolysis. In addition small amounts of methylphosphonic-bis(dimethylamide) (7) are formed. Properties, nmr and mass spectra of 5 and 6 are described, their mechanism of formation is discussed.
    Notes: Die Hydrolyse von 1,1,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5 -diphosphet (2) führt in erster Stufe zu Bis(dimethylamino)phosphorylmethyliden-methyl-bis(dimethylamino)phosphorane (5). In zweiter Stufe wird vornehmlich Bis(dimethylamino)phosphoryl-methyl(dimethylamino)phosphosphonylmethylen (6) neben geringen Mengen von Methylphosphonsphonsäure-bis(dimethylamid) (7) gebildet. Eigenschaften, NMR- und Massenspektren von 5 und 6 sind beschrieben, ihr Bildungsmechanismus wird diskutiert.
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  • 17
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1682-1684 
    ISSN: 0044-2313
    Keywords: Lithium iodide ; DME complex ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of [Li(DME)2I].LiI can be dissolved at 50°C in toluene/DME (2:1). At - 20°C [Li(DME)2I] (1) was isolated in 75% yield. 1 was characterized by NMR techniques as well as an X-Ray structure determination. 1 crystallizes in the space group C2/c with a = 1 356.9(2), b = 813.2(1), c = 1 259.1(2) pm, and β = 99.74(1)°.
    Notes: LiI kann bei 50°C in Toluol/DME (2:1) in Lösung gebracht werden. Bei - 20°C wird [Li(DME)2I] (1) in 75% Ausbeute isoliert. 1 wurde mittels NMR-Spektroskopie sowie durch eine Röntgenstrukturanalyse charakterisiert. 1 kristallisiert in der Raumgruppe C2/c mit a = 1 356,9(2), b = 813,2(1), c = 1 259,1(2) pm und β = 99,74(1)°.
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  • 18
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1714-1718 
    ISSN: 0044-2313
    Keywords: Alkinyl thiophosphinous acid ester ; alkinyl [1,3,2]dithiaphospholane ; [1,4]dithiane ; nmr, mass, i.r. spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phenylethinyl-[1,3,2]dithiaphospholane. Bis(dithiaphospholanyl)-[1,4]dithianeNucleophilic substitution of the amino group but no cycloaddition occurs in the reaction of phenyl phenylethinyl phosphinous acid diethylamide, 5, with 2-aminothiophenol forming compound 6. By analogous reaction, phenylethinyl phosphonic bis(diethylamide), 7, and ethane-1,2-dithiol form compound 8. Cycloaddition besides nucleophilic substitution is observed, however, when acetylene bis(phosphonic diethyl-amide), 9, and ethane-1,2-dithiol are reacted resulting in compound 11. All new products are characterized by their nmr, mass, and i.r. spectra. Furthermore, the results of an X-ray structure analysis of 11 are reported.
    Notes: Bei der Reaktion von Phenyl-phenylethinyl-phosphinigsäure-diethylamid, 5, mit 2-Aminothiophenol findet keine Cycloaddition statt sondern eine nukleophile Substitution der Aminogruppe, die zu Verbindung 6 führt. Analog reagiert Phenylethinyl-phosphonigsäure-bis(diethylamid), 7, mit Ethan-1,2-dithiol zu Verbindung 8. Cycloaddition und nukleophile Substitution werden jedoch bei der Umsetzung von Acetylen-bis(phosphonigsäurediethylamid), 9, und Ethan-1,2-dithiol beobachtet; es entsteht Verbindung 11. Alle neuen Reaktions-produkte sind durch ihre NMR-, Massen- und IR-Spektren charakterisiert. Von 11 wird eine Kristallstrukturanalyse mitgeteilt.
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  • 19
    ISSN: 0044-2313
    Keywords: Dihydro-diphosphinines ; dihydro-diphosphinine disulfides ; dihydro-diphosphinine dioxide ; crystal structures ; nmr, ir, mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,4-Dihydro-1λ5,4λ5-[1,4]diphosphinines and a 1,4-Dihydro-1λ3,4λ3-[1,4]diphosphinineReaction of thio- or dithiocarbonic acids with ethinyl amino phosphanes leads to 1,4-dihydro-1λ5,4λ5-[1,4]diphosphinine-1,4-disulfides. By this route compounds 4, 7, and 8 have been prepared. Desulfurization of 4 with tri-n-butylphosphane results in 1,2,4,5-tetraphenyl-1,4-dihydro-1λ3,4λ3-[1,4]-diphosphinine 5, which can be oxidized with tert-butyl-peroxide to the corresponding dioxide, 6. From the reaction mixture of phenyl-phenylethinyl diethylamino phosphane and thioacetamide compound 4 and the unsymmetrical 1,4-dihydro-1λ5,4λ5-[1,4]diphosphinine 9 were isolated. Properties, nmr, ir and mass spectra of all new products are reported. A mechanism for the formation of 9 is suggested. The results of the X-ray structure determination of 8 and 9 are described.
    Notes: Die Reaktion von Thio- oder Dithiocarbonsäuren mit Ethyinylaminophosphanen führt zu den 1,4-Dihydro-1λ5,4λ5-[1,4]diphosphinin-1,4-disulfiden. Auf diese Weise wurden die Verbindungen 4, 7 und 8 dargestellt. Die Entschwefelung von 4 mit Hilfe von Tri-n-butylphosphan ergibt 1,2,4,5-Tetraphenyl-1,4-dihydro-1λ3,4λ3-[1,4]diphosphinin 5, das mit tert-Butylperoxid zum entsprechenden Dioxid 6 oxidiert werden kann. Aus der Reaktionsmischung von Phenyl(phenylethinyl)diethylaminophosphan und Thioacetamid wurden 4 und das unsymmetrische 1,4-Dihydro-1λ5,4λ5-[1,4]diphosphinin 9 isoliert. Die Verbindungen sind durch ihre Eigenschaften, NMR-, IR- und Massenspektren charakterisiert. Für die Bildung von 9 wird ein Reaktionsmechanismus vorgeschlagen. Die Ergebnisse der Kristallstrukturanalysen von 8 und 9 werden mitgeteilt und diskutiert.
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  • 20
    ISSN: 0044-2313
    Keywords: Diphosphete ; Phosphorus-Ylid-Iminophosphoranes ; Syntheses ; NMR, IR, Mass Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphete with N—H and P—H Acidic Compounds1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphete, 1, reacts with aniline to give by opening of the ring 2,2,4,4-tetrakis(dimethylamino)-1-phenyl-1,2λ5,4λ5-azadiphosphapenta-1,3-diene, 2, with p-CN—C6F4—NH2 the product is 1-(4-cyano-2,3,5,6-tetrafluorophenyl)-2,2,4,4-tetrakis(dimethylamino)-1,2λ5,4λ5-azadiphosphapenta-1,3-diene, 3. t-Butylamine or diethylamine do not react with 1. Mesitylphosphane opens the ring system 1 forming by reduction of one phosphorus atom {[bis(dimethylamino)phosphanyl]methylidene}bis(dimethylamino)methylphosphorane, 4. The same product 4 is obtained by reaction with phenylphosphane. The reaction products 2-4 are characterized by their nmr, mass, and ir spectra. Their way of formation is discussed. In 4 a 5J(PH), in 3 a 7J(CF) long range coupling constant could be identified.
    Notes: 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet, 1, reagiert mit Anilin unter Ringöffnung zu 2,2,4,4-Tetrakis(dimethylamino)-1-phenyl-1,2λ5,4λ5-azadiphosphapenta-1,3-dien, 2, mit p-CN—C6F4—NH2 zu 1-(4-Cyan-2,3,5,6-tetrafluorphenyl)-2,2,4,4-tetrakis(dimethylamino)-1,2λ5,4λ5-azadiphosphapenta-1,3-dien, 3. t-Butylamin oder Diethylamin reagieren nicht mit 1. Mesitylphosphan öffnet das Ringsystem 1 und bildet unter Reduktion eines Phosphoratoms {[Bis(dimethylamino)phosphanyl]methyliden}bis(dimethylamino)methylphosphoran 4. Das gleiche Produkt 4 liefert auch die Umsetzung mit Phenylphosphan. Die Reaktionsprodukte 2-4 sind durch ihre NMR-, Massen- und IR-Spektren charakterisiert. Ihr Bildungsweg wird diskutiert. Bei 4 kann eine 5J(PH)- und bei 3 eine 7J(CF)-long-range-Kopplungskonstante nachgewiesen werden.
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