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  • 1
    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.
    Additional Material: 3 Ill.
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  • 2
    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.
    Additional Material: 2 Ill.
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  • 3
    ISSN: 0044-2313
    Keywords: 1λ5,3λ5-diphosphete ; iron, chromium, tungsten complexes ; nmr, mass, ir spectra ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Complexes of 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-Diphosphete1,1,3,3-Tetrakis(dimethylamino)-1λ5,3aλ5-diphosphete, 1, reacts with W(CO)6 to yield the isomeric complexes {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)tungsten 4 and {1,1,3,3-tetrakis(dimethylamino)-1,4-dihydro-1λ5,3λ5-[1,3]diphosphetium}(pentacarbonyl)tungsten 5. With Cr(CO)6 the complex {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)chromium 6 is formed. From the reaction products of Fe3(CO)12 and Fe2(CO)9 with 1 the complex {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)iron 7 could be isolated. Properties, nmr, ir and mass spectra of the new compounds are reported. 6 and 7 were characterized by X-ray structure determinations.
    Notes: 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet, 1, reagiert mit W(CO)6 zu den isomeren Komplexen {1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet}(pentacarbonyl)wolfram 4 und {1,1,3,3-Tetrakis(dimethylamino)-1,4-dihydro-1λ5,3λ5-[1,3]diphosphetium}(pentacarbonyl)wolfram 5, mit Cr(CO)6 zu dem Komplex {1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet}(pentacarbonyl)chrom 6. Aus den Reaktionsprodukten von Fe3(CO)12 und Fe2(CO)9 mit 1 konnte der Komplex {1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet}(pentacarbonyl)eisen 7 isoliert werden. Eigenschaften, NMR-, IR- und Massenspektren der neuen Verbindungen werden mitgeteilt. 6 und 7 wurden zusätzlich durch Kristallstrukturanalysen charakterisiert.
    Additional Material: 4 Ill.
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  • 4
    ISSN: 0044-2313
    Keywords: 1λ5, 3λ5-diphosphete ; aluminium ; indium complexes ; n.m.r ; mass ; ir spectra ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [1,l,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5-diphosphet]trimethylaluminiuin and -indium1,1,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5-diphosphet, 1, reacts with A1(CH3)3 and In(CH3)3 to give the complexes [l,l,3,3-tetrakis(dimethylamino)-1λ5, 3λ5-diphosphete]-trimethylaluminium, 2, and [1,1,3,3-Tetrakis(dimethylamino)-l,1λ5, 3λ55-diphosphete]-trimethylindium, 3, as crystalline products, respectively. Properties, n.m.r., mass and i.r. spectra are reported and interpreted. Compounds 2 and 3 are further characterized by X-ray structural analyses; the bonding situation in both complexes is discussed in detail
    Notes: 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet, 1, reagiert mit Al(CH3)3 bzw. In(CH3)3 zu den Komplexen [1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet]trimethylaluminium, 2, bzw. [1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet]trimethylindium, 3, die jeweils als kristalline Produkte erhalten werden. Die Eigenschaften, NMR-, Massen- und IR-Spektren werden mitgeteilt und interpretiert. 2 und 3 sind zusätzlich durch Kristallstrukturanalysen charakterisiert; die Bindungsverhältnisse in beiden Komplexen wurden eingehend diskutiert.
    Additional Material: 5 Ill.
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  • 5
    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.
    Additional Material: 2 Tab.
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  • 6
    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.
    Additional Material: 3 Ill.
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  • 7
    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.
    Additional Material: 1 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 974-980 
    ISSN: 0044-2313
    Keywords: 1λ5,3λ5-diphosphete ; (phosphonioalkinyl)(tetracarbonyl)iron ; acyl(tetracarbonyl)iron ; nmr, mass, ir spectra ; X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A (Phosphonioalkinyl)- and an Acetyl(tetracarbonyl)ironFrom the reaction of 1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete, 1, and Fe(CO)5 {[bis(dimethylamino)phosphoryl-methyl]-bis(dimethylamino)phosphonioethinyl}(tetracarbonyl)iron, 4, and {1,1,3,3-tetrakis(dimethylamino)-1,4-dihydro- 1λ5,3λ5-[1,3]diphosphetium-2-carbonyl}(tetracarbonyl)-iron, 5, can be isolated as crystalline products. The nmr, mass and ir spectra of the two compounds as well crystal and molecular structures of 4 are reported. The bonding situation in compounds 4 and 5 are discussed in detail.
    Notes: Aus dem Reaktionsgemisch von 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet, 1, und Fe(CO)5 können {[Bis(dimethylamino)phosphoryl-methyl]-bis(dimethylamino)phosphonioethinyl}(tetracarbonyl)eisen, 4, und{1,1,3,3-Tetrakis(dimethylamino)-1,4-dihydro-1λ5,3λ5-[1,3]diphosphetium-2-carbonyl}(tetracarbonyl)eisen, 5, als kristalline Produkte isoliert werden. Die NMR-, Massen- und IR-Spektren der beiden Verbindungen werden mitgeteilt. Von 4 konnten die Kristall-und Molekülstruktur ermittelt werden. Die Bindungsverhältnisse in 4 und 5 werden eingehend diskutiert.
    Additional Material: 2 Ill.
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  • 9
    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.
    Additional Material: 1 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 139-148 
    ISSN: 0044-2313
    Keywords: Fluoromethylidenephosphorane ; tris[(difluorophosphoranyl)methyl]phosphane ; n.m.r. spectra ; triple resonance ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Bis(dimethylamino)fluoromethylidenephosphorane with CIPF2 and PF3One of the products from the reaction between ClPF2 or PF3 and H2C=P(F)[N(CH3)2]2 (2) is tris{[bis(dimethylamino)difluorophosphoranyl]methyl}phosphane, 3. With sulfur, 3 forms the corresponding phosphane sulfide 4. The structures of the new compounds are elucidated by their n.m.r. spectra in double and triple resonance mode and by their mass spectra.
    Notes: Eines der Produkte aus der Reaktion zwischen ClPF2 oder PF3 und H2C=P(F)[N(CH3)2]2 (2) ist Tris{[bis(dimethylamino)difluorphosphoranyl]methyl}phosphan, 3. Mit Schwefel reagiert 3 zum entsprechenden Phosphansulfid 4. Die Strukturen der neuen Verbindungen werden durch NMR-Mehrfachresonanzexperimente und ihre Massenspektren belegt.
    Additional Material: 2 Ill.
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