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  • 1
    Electronic Resource
    Electronic Resource
    Der thermische Zerfall des tBu2P—P=P(Me)tBu2Professor Rudolf Hoppe zum 75. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1769-1773 
    Details
    ISSN: 0044-2313
    Keywords: Phosphinophosphinidene-phosphorane tBu2P—P=P(Me)tBu2 ; formation of tBu2PMe and the phosphinophosphinidene tBu2P—P ; 2,4-Bis(di-tert-butylphosphino)-1,2,3,4-tetraphosphabicyclo[1.1.0]butane P4(PtBu2)2 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Thermal Decomposition of tBu2P—P=P(Me)tBu2The thermal decomposition of tBu2P—P=P(Me)tBu2 2 in C6H6 at 20°C is detectable after 10 h; tBu2PMe, (tBu2P)2PH and small amounts of the cyclotetraphosphanes P4(PtBu2)4 and P4(PtBu2)2 are formed. At 70°C (14 h) 83% of 2 are decomposed, and even 96% after 74 h. The main products are tBu2PMe (68%) and P4(PtBu2)4 (20%). With 2,3-dimethyl-1,3-butadiene as a trapping reagent tBu2PMe (62%) is still the main product, however, P4(PtBu2)4 is no longer found, but 1,2-bis(di-tert-butylphosphino)-4,5-dimethyl-1,2-diphosphacyclohexene-4 (22%) is formed instead. Also with cyclohexene tBu2PMe (78%) remains the major product besides P4(PtBu2)4 (9%) and small amounts of the trapping product 7-di-tert-butylphosphino-7-phosphabicyclo[4.1.0]heptane. Thus, the thermal decomposition of 2 at 70°C proceeds very similar to that of tBu2P—P=P(Br)tBu2 at -30°C and starts yielding and the phosphinophosphinidene tBu2P—P. In CH2Cl2 the decomposition of 2 includes the chlorination of the ylidic molecule.
    Notes: Die thermische Zersetzung von tBu2P—P=P(Me)tBu2 2 in C6H6 ist bei 20°C nach 10 h nachweisbar, wobei tBu2PMe, (tBu2P)2PH und geringe Mengen der Cyclotetraphosphane P4(PtBu2)4 und von P4(PtBu2)2 entstehen. Bei 70°C (14 h) sind 83% von 2 zerfallen, nach 75 h 97%. Hauptprodukte sind tBu2PMe (68%) und P4(PtBu2)4 (20%). In Anwesenheit des Abfangreagenzes 2,3-Dimethyl-1,3-butadien bleibt tBu2PMe (62%) Hauptprodukt, doch P4(PtBu2)4 wird nicht mehr gebildet, sondern es entsteht 1,2-Bis(di-tert-butylphosphino)-4,5-dimethyl-1,2-diphosphacyclohexen-4 (22%). Mit Cyclohexen ist tBu2PMe Hauptprodukt (78%) neben P4(PtBu2)4 (9%) und geringen Anteilen des Abfangproduktes 7-Di-tert-butylphosphino-7-phosphabicyclo[4.1.0]heptan. Damit entspricht der Zerfall von 2 bei 70°C weitgehend dem des tBu2P—P=P(Br)tBu2 bei -30°C und beginnt mit der Bildung von tBu2PMe und des Phosphinophosphinidens tBu2P—P. In CH2Cl2 läuft die Zersetzung von 2 über die Chlorierung und Zersetzung des Ylidgerüstes.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976231118
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  • 2
    Electronic Resource
    Electronic Resource
    Komplexchemie P-reicher Phosphane und Silylphosphane. XII. Bildung und Struktur von Li(THF)2[η2-(tBu2P)2P], Li(TMEDA)[η2-(tBu2P)2P], Li(THF)2[η2-(iPr2P)2P], Li(THF)2[η2-(Et2N)2P—P—PtBu2], Li(THF)2[η2-(tBu2P—P—PiPr2] und (tBu2P)2P—SiMe3Professor Kurt Dehnicke zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1564-1572 
    Details
    ISSN: 0044-2313
    Keywords: Li(THF)2[η2-(tBu2P)2P] ; Li(TMEDA)[η2-(tBu2P)2P] ; Li(THF)2[η2-(iPr2P)2P] ; Li(THF)2[η2-(Et2N)2P—P—PtBu2] ; Li(THF)2[η2-(tBu2P—P—PiPr2)] ; (tBu2P)2P—SiMe3 ; crystal structures ; 1H, 31P, 7Li-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation and Structure of Li(THF)2[η2-(tBu2P)2P], Li(TMEDA)[η2-(tBu2P)2P], Li(THF)2[η2-(iPr2P)2P], Li(THF)2[η2-(Et2N)2P—P—PtBu2], Li(THF)2[η2-(tBu2P—P—PiPr2] and (tBu2P)2P—SiMe3The formation and crystal structures of the compounds (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA)[η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 and Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 are reported. Compounds 3-6 are formed by reacting the corresponding silylated triphosphanes with nBuLi: 2 and 3 result from (tBu2P)2P—SiMe3 1, 4 from (iPrP)2P—SiMe3, 5 from (Et2N)2P—P(SiMe3)—PtBu2 and 6 from tBu2P—P(SiMe3)—PiPr2. 1 crystallizes in the orthorhombic space group P212121 (no. 19) with a = 910.87(7) pm, b = 1132.5(1) pm, c = 2373.5(2) pm (determined at 90 K). The structure determination of 2 was performed at 293 K and 200 K, respectively. 2 crystallizes in the monoclinic space group P21/n (no. 14) with a = 1069.7(3) pm, b = 1802.5(3) pm, c = 1604.0(7) pm, β = 98.11(2)° (200 K); 3 also in P21/n (no. 14) with a = 904.3(2) pm, b = 1936.4(5) pm, c = 1653.2(3) pm, β = 94.52(1)° (200 K). 4 crystallizes monoclinically in C2/c (no. 15) with a = 1650.0(5) pm, b = 945.6(3) pm, c = 1779.8(5) pm, β = 108.81(2)° (200 K); 5 in P21/n (no. 14) with a = 939.4(5) pm, b = 1736.8(6) pm, c = 1943.3(7) pm, β = 98.17(4)° (200 K). All compounds contain Z = 4 molecules in the unit cell.The 1H, 31P and 7Li NMR spectra of 2-6 are discussed.
    Notes: Es wird über die Verbindungen (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA) · [η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 und Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 berichtet. Letztere bilden sich durch Umsetzung der entsprechenden silylierten Triphosphane mit nBuLi: 2 und 3 aus (tBu2P)2P—SiMe3 1, 4 aus (iPr2P)2P—SiMe3, 5 aus (Et2N)2—P · (SiMe3)—PtBu2, 6 aus tBu2P—P(SiMe3)—PiPr2.1 kristallisiert orthorhombisch in P212121 (Nr. 19) mit a = 910,87(7) pm, b = 1132,5(1) pm, c = 2373,5(2) pm (bei 90 K bestimmt). Die Strukturbestimmung von 2 erfolgte bei 293 K und 200 K. 2 kristallisiert monoklin in P21/n (Nr. 14) mit a = 1069,7(3) pm, b = 1802,5(3) pm, c = 1604,0(7) pm, β = 98,11(2)° (200 K), 3 ebenfalls in P21/n (Nr. 14) mit a = 904,3(2) pm, b = 1936,4(5) pm, c = 1653,2(3) pm, β = 94,52(1)° (200 K). 4 kristallisiert monoklin in C2/c (Nr. 15) mit a = 1650,0(5) pm, b = 945,6(3) pm, c = 1779,8(5) pm, β = 108,81(2)° (200K), 5 in P21/n (Nr. 14) mit a = 939,4(5) pm, b = 1736,8(6) pm, c = 1943,3(7) pm, β = 98,17(4)° (200 K). Alle fünf Verbindungen enthalten jeweils vier Formeleinheiten in der Elementarzelle.Es wird über die Untersuchung der 1H-, 31P- und 7Li-NMR-Spektren der Verbindungen 2-6 berichtet.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220920
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