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  • 1
    Electronic Resource
    Electronic Resource
    Struktur und Reaktionen von 2,2′-Oxybis[2,2-dimethyl-4,4,5,5-tetrakis(trifluormethyl)-1,3,2λ5-dioxaphospholan]Professor Alfred Roedig zum 70. Geburtstag gewidmet. (1981)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1981 (1981), S. 1035-1043 
    Details
    ISSN: 0170-2041
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure and Reactions of 2,2′-Oxybis[2,2-dimethyl-4,4,5,5-tetrakis(trifluoromethyl)-1,3,2λ5-dioxaphospholane]The structure of the title compound 3 has been determined by X-ray diffraction. 3 was found to crystallize in the monoclinic system (space group P21/c). Two crystallographically independent molecules are observed in the crystal lattice which differ with regard to the P - O - P angle [147.3(3)° and 150.8(3)°, respectively]. Formation of 3 has been observed in the reaction of the chlorophosphorane Me2P(pfp)Cl (2; pfp = perfluoropinacolyl) with NaHCO3, and of the siloxyphosphorane Me2P(pfp)OSiMe3 (1) with Me2P(= O)Cl. Cleavage of 3 with methanol furnishes the previously known compound Me2P(pfp)OMe (5) and the acyclic phosphinic acid ester Me2P(= O)OC(CF3)2C(CF3)2OH (4b). Reaction of 3 with water leads to exclusive formation of 4b; the isomeric hydroxyphosphorane Me2P(pfp)OH (4a) has not been observed.
    Notes: Die Struktur der monoklin (Raumgruppe P21/c) kristallisierenden Titelverbindung 3 wurde durch Röntgenstrukturanalyse bestimmt (Abb. 1-3). Im Kristallgitter werden zwei kristallographisch unabhängige Moleküle beobachtet, die sich in der Groβe des P - O - P-Winkels unterscheiden [147.3(3)° bzw. 150.8(3)°]. 3 bildet sich bei der Umsetzung des Chlorphosphorans Me2P(pfp)Cl (2; pfp = perfluorpinakolyl) mit NaHCO3 sowie aus dem Siloxyphosphoran Me2P(pfp)OSiMe3 (1) mit Me2P(= O)Cl. Die Spaltung von 3 mit Methanol liefert die bereits bekannte Verbindung Me2P(pfp)OMe (5) und den acyclischen Phosphinsäureester Me2P(= O)OC(CF3)2C(CF3)2OH (4b). Die Umsetzung von 3 mit H2O führt ausschließlich zu 4b; die Bildung des isomeren Hydroxyphosphorans Me2P(pfp)OH (4a) wird nicht beobachtet.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.198119810609
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  • 2
    Electronic Resource
    Electronic Resource
    Verbindungen mit dem 1,3,5,2-Triazaphosphorinan-Grundgerüst: Synthese und Koordinationschemie neuartiger, N,N,N′-Trimethylethylendiamin-substituierter Verbindungen mit drei-und vierfach koordiniertem Phosphor (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 1265-1270 
    Details
    ISSN: 0009-2940
    Keywords: 1,3,5-Trimethylbiuret ; Ethylenediamine, N,N,N′-trimethyl- ; Iron complexes ; Chromium complexes ; Molybdenum complexes ; 1,3,5,2-Triazaphosphorinanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Compounds with the 1,3,5,2-Triazaphosphorinane Skeleton: Synthesis and Coordination Chemistry of Novel N,N,N′-Trimethylethylenediamine-Substituted Compounds with Three-and Four-Coordinate PhosphorusSubstitution of chlorine for the N,N,N′-trimethylethylenediamine group in the 1,3,5-trimethylbiuret derivative 2 produced 4. The reaction of the 1,3,5,2-triazaphosphorinane 4 with sulfur furnished the expected P(=S) derivative 5. Reaction of 4 with methyl iodide led to the formation of the ammonium iodide 6 by methylation of the nitrogen atom of the terminal NMe2 group while the phosphorus atom of 4 remained unaffected. The structure of 6 was confirmed by a single-crystal X-ray structure analysis. In the unusual reaction of 4 with Br2 the bromodimethylammonium-bromophosphonium dibromide 7 was formed. The reaction of 4 with Fe2(CO)9 furnished the expected Fe(CO)4 complex 8 while with (C7H8)Cr(CO)4 (C7H8=norbornadiene) 9 was obtained. In 9, norbornadiene is replaced by one molecule of 4, which is coordinated by phosphorus and the nitrogen atom of the NMe2 group. In the reaction of 4 with C7H8Mo(CO)4 (C7H8=norbornadiene) the complexes 10a and 10b were formed. In 10a, the P(III) atom of 4 is coordinated to Mo; the second coordination site at Mo(CO)4 is occupied by the nitrogen atom of the terminal NMe2 group. In 10b, the nitrogen atoms of the PN(Me) and of the NMe2 grouping are coordinated to Mo, with formation of a five-membered ring.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260602
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  • 3
    Electronic Resource
    Electronic Resource
    2-{[2-(Dimethylamino)ethyl]methylamino}-1,3,2-benzodioxaphosphol als Ligand in Übergangsmetallkomplexen  -  Kristall- und Molekülstruktur eines Tetracarbonylchrom-Komplexes (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 301-307 
    Details
    ISSN: 0009-2940
    Keywords: Ethylenediamine, N,N,N′-trimethyl- ; Transition-metal complexes, P - N coordination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 2-{[2-(Dimethylamino)ethyl]methylamino}-1,3,2-benzodioxaphosphole as a Ligand in Transition-Metal Complexes. Crystal and Molecular Structure of a Tetracarbonyl Chromium DerivativeComplexes of the zerovalent transition metals chromium, molybdenum, iron, and platinum react with the title phosphorus-(III)-compound 3 to give a range of different products: in the coordination compounds 4 and 5, 3 functions as a bidentate ligand, coordinating to the metal through the phosphorus and the nitrogen atom of the dimethylamino group. The structure of 4 was confirmed by a single-crystal X-ray analysis, showing a ligand “bite” angle of 91.0, 91.4° in two independent molecules. In the compounds 7 - 9, involving Mo, Fe, and Pt as a central atom, 3 coordinates solely through P(III). For the platinum(O) complex 9 31P-NMR spectroscopy revealed a dynamic behaviour at room temperature.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250205
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  • 4
    Electronic Resource
    Electronic Resource
    N,N-Dimethylharnstoff-verbrückte Diphosphorverbindungen; Struktur eines Spirophosphorans mit λ5-Phosphor als BrückengliedHerrn Professor Leopold Horner zum 70. Geburtstag gewidmet. (1982)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1982 (1982), S. 167-181 
    Details
    ISSN: 0170-2041
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N,N′-Dimethylurea-bridged Diphosphorus Compounds; Structure of a Spirophosphorane with λ5-Phosphorus as a Bridging AtomReaction of N,N′-dimethyl-N,N′-bis(trimethylsilyl)urea with MePCl2 yields the chloro-substituted diphosphine 1. With excess hexafluoroacetone 1 reacts with loss of one equivalent of MePCl2 and formation of the spirophosphorane 3 whose structure has been determined by X-ray diffraction. The geometry at phosphorus is approximately trigonal-bipyramidal. A spirophosphorane analogous to 3 is obtained by reaction of 1 with tetrachloro-o-benzoquinone (TOB). Dehalogenation of 1 furnishes the diphosphine 7 which reacts quantitatively with one equivalent of TOB to give the λ3-λ5P-diphosphorus compound 10. Attempted further oxidation of 10 with TOB at the λ3P atom leads to cleavage of the P-P bond with formation of 4 and a further spirophosphorane 9 which results, formally, from the oxidative addition of two equivalents of TOB to a PMe unit. Formation of 4 and 9 is also observed upon reaction of 7 with more than one equivalent of TOB. In the reaction of 1 with Me2NSiMe3 the P-P-bonded compound 11 is obtained, containing one λ3-and one λ4-phosphorus atom directly bonded.
    Notes: Durch Umsetzung von N,N′-Dimethyl-N,N′-bis(trimethylsilyl)harnstoff mit MePCl2 ist das Chlor-substituierte Diphosphin 1 zugänglich. 1 reagiert mit überschüssigem Hexafluoraceton unter Abspaltung von MePCl2 zum Spirophosphoran 3, dessen Struktur durch Röntgen-Struktur-analyse bestimmt wurde. Am Phosphor liegt annähernd trigonal-bipyramidale Geometrie vor. - Durch Umsetzung von 1 mit Tetrachlor-o-benzochinon (TOB) wird ein zu 3 analoges Phosphoran 4 erhalten. Enthalogenierung von 1 liefert das Diphosphin 7, das mit einem Äquivalent TOB quantitativ zur λ3P - λ5P-Diphosphorverbindung 10 umgesetzt werden kann. Der Versuch, 10 am λ3-Phosphor mit TOB weiter zu oxidieren, führt zur Spaltung der P-P-Bindung unter Bildung von 4 und eines weiteren Spirophosphorans 9, das formal durch oxidative Addition von zwei Äquivalenten TOB an eine PMe-Einheit entsteht. 4 und 9 werden auch bei der Umsetzung von 7 mit mehr als einem Äquivalent TOB erhalten. Reaktion von 1 mit Me2NSiMe3 liefert quantitativ die Diphosphorverbindung 11, die je ein λ3- und λ4-Phosphoratom in direkter Bindung enthält.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.198219820117
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