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  • 1
    Electronic Resource
    Electronic Resource
    Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, LXXVII Synthese, Struktur und Reaktivität von Phosphametallacyclopropanen mit isolobalen ER- (E = N, P, As, Sb) und Fe(CO)4-Bausteinen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2171-2179 
    Details
    ISSN: 0009-2940
    Keywords: Phosphametallacyclopropanes ; Isolobal building blocks ; Lewis basic behavior ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal-Containing Heterocycles: Preparation, Properties, Reactions, LXXVII. - Synthesis, Structure and Reactivity of Phosphametallacyclopropanes with Isolobal ER (E = N,P,As,Sb) and Fe(CO)4 Building BlocksThe phosphidometallates \documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ Li_2 \left\{ {\left[ M \right]\dddot - PPh_2 } \right\} $\end{document} {[M] = (η5-C5H5)M-(CO)2}, resulting from the metal hydride complexes H[M]PPh2H [M = Cr (1), Mo (2), W (3)] by reduction with nBuLi, react with the geminal dihalides RECl2 to give the three-membered phosphametallacyclopropanes [ER = NC6F5 (M = Cr (1a), Mo (2a), W (3a)), PPh (M = Cr (1b), Mo (2b), W (3b)), PC6H11 (M = Cr (1c), Mo (2c), W (3c)), P-tBu (M = Cr (1d), Mo (2d), W (3d)), P(2,4,6-(tBu)3C6H2) (M = Cr (1e), Mo (2e), W (3e)), As(2,4,6-(tBu)3C6H2) (M = Cr (1f), Mo (2f), W (3f)), Sb-tBu (M = Cr (1g), Mo (2g))]. Reaction of Br2Fe(CO)4 with the corresponding dilithium compounds \documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ Li_2 \left\{ {\left[ M \right]\dddot - PPh_2 } \right\} $\end{document} affords the phosphido-bridged heterodimetallic complexes . According to X-ray structural analyses in 2a and 2f the P - E bond distances are shortened while the Mo - E bonds are significantly elongated compared to a single bond. (OC)5CrTHF is added to the Lewis basic E atom in 2b, 2d, and 2g with loss of THF to give P-tBu (4d), Sb-tBu (4g)]. By this reaction the antimony-containing ring 2g is kinetically stabilized. Because of the low basicity of the N atom in 2a no addition was observed. The ring skeleton of 4b and 4g, undergoes no change by Cr(CO)5 coordination as shown by X-ray structural analyses.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911241005
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  • 2
    Electronic Resource
    Electronic Resource
    Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, LXIII. Phosphamolybdacyclopropane mit Carben- und Phosphiniden-Bausteinen (1989)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 823-827 
    Details
    ISSN: 0009-2940
    Keywords: Phosphamolybdacyclopropanes ; Isolobal building blocks ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal-Containing Heterocycles: Preparation, Properties, Reactions, LXIII. - Phosphamolybdacyclopropanes with Carbene and Phosphinidene Building BlocksThe phosphidomolybdate (1) {[Mo] = (η5-C5H5)Mo(CO)2} reacts with the geminal dihalides RCHCl2 (2a-c) [R = H (a), Me (b), Ph (c)] and the organophosphorus chlorides RPCl2 (4b-d) [R = 2,4,6-(tBu)3C6H2 (d)] to give the three-membered phosphamolybdacyclopropanes (3a-c) and (5b-d), respectively. The activation parameters ΔG≠ for the rotation of the P-C unit are independent of the substituent R, based on temperature-dependent 1H-NMR spectra of 3a-c. According to an X-ray structural analysis 5c crystallizes in the triclinic space group P1 with Z = 4. Compared to a single bond the P—P distance (211 pm) in 5c is shorter. the complexes (OC)5MTHF are added to the Lewis basic phosphinidene phosphorus in 5c with loss of THF giving (6c-8c) [M = Cr (6), Mo (7), W (8)].
    Notes: Das Phosphidomolybdat (1) {[Mo] = (η5-C5H5)Mo(CO)2} reagiert mit den geminalen Dihalogeniden RCHCl2 (2a-c) [R = H (a), Me (b), Ph (c)] und Organophosphorchloriden RPCl2 (4b-d) [R = 2,4,6-(tBu)3C6H2 (d)] zu den dreigliedrigen Phosphamolybdacyclopropanen (3A-c) bzw. (5b-d). Aus temperaturabhängigen 1H-NMR-Spektren von 3a-c ergeben sich die Aktivierungsparameter ΔG≠ für die Rotation der P—C-Einheit, die unabhängig vom Substituenten R sind. 5c kristallisiert laut Röntgenstruktur-analyse in der triklinen Raumgruppe P1 mit Z = 4. Der P—P-Abstand in 5c ist mit 211 pm gegenüber einer Einfachbindung verkürzt. An den Lewis-basischen Phosphiniden-Phosphor in 5c addieren sich unter THF-Verlust die Komplexe (OC)5MTHF unter Bildung von (6c-8c) [M = Cr (6), Mo (7), W (8)].
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19891220505
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  • 3
    Electronic Resource
    Electronic Resource
    Phosphaniminato-Komplexe des Schwefels. Synthese und Kristallstrukturen von [SO(Cl)(NPPh3)], [SO2(Cl)(NPPh3)] und [SCl(NPPh3)2]ClProfessor Egon Uhlig zum 65. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1986-1991 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes of Sulfur ; Syntheses ; IR Spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorane Iminato Complexes of Sulfur. Synthesis and Crystal Structures of [SO(Cl)(NPPh3)], [SO2(Cl)(NPPh3)], and [SCl(NPPh3)2]ClThe title compounds have been prepared by the reaction of Me3SiNPPh3 with SOCl2, SO2Cl2, and SCl2, respectively. They form colourless, moisture sensitive crystals, which were characterized by IR spectroscopy and by crystal structure determinations.[SO(Cl)(NPPh3)]: Space group P21/n, Z = 4, structure determination with 2 434 observed unique reflections, R = 0.047. Lattice dimensions at 19°C: a = 1 304.8, b = 996.5, c = 1 339.5 pm, β = 93.75°. The compound forms monomeric molecules with a remarkably long S—Cl bond of 234.2 pm and distances SN and PN of 154.6 and 161.6 pm, respectively, which agree with double bonds.[SO2(Cl)(NPPh3)]: Space group P21/n, Z = 4, structure solution with 2 872 observed, unique reflections, R = 0.047. Lattice dimensions at 20°C: a = 956.9, b = 1 909, c = 1 002.0 pm, β = 106.06°. The compound forms monomeric molecules with distances S—Cl of 207.1 pm, SN of 154.5 pm, and PN of 161.6 pm.[SCl(NPPh3)2]Cl: Space group P21/c, Z = 4, structure solution with 5 224 observed, unique reflections, R = 0.042. Lattice dimensions at 20°C: a = 1 108.6, b = 1 603.8, c = 1 840.5 pm, β = 99.98°. The compound forms ions [SCl(NPPh3)2]+ and Cl-. In the cation the sulfur atom is ϕ-tetrahedrally coordinated with a long S—Cl distance of 248.5 pm and SN bond lengths of 154.5 and 156.0 pm.
    Notes: Die Titelverbindungen entstehen durch Umsetzung von Me3SiNPPh3 mit Thionylchlorid, Sulfurylchlorid bzw. Schwefeldichlorid als farblose, feuchtigkeitsempfindliche Kristalle, die wir durch die IR-Spektren und durch Kristallstrukturanalysen charakterisiert haben.[SO(Cl)(NPPh3)]: Raumgruppe P21/n, Z = 4, Strukturlösung mit 2 434 unabhängigen beobachteten Reflexen, R = 0,047. Gitterabmessungen bei 19°C: a = 1 304,8; b = 996,5; c = 1 339,5 pm, β = 93,75°. Die Verbindung bildet monomere Moleküle mit einer auffällig langen S—Cl-Bindung von 234,2 pm und Abständen SN und PN von 154,6 bzw. 161,6 pm, die Doppelbindungen entsprechen.[SO2(Cl)(NPPh3)]: Raumgruppe P21/n, Z = 4, Strukturlösung mit 2 872 unabhängigen beobachteten Reflexen, R = 0,047. Gitterabmessungen bei 20°C: a = 956,9; b = 1 909; c = 1 002,0 pm, β = 106,06°. Die Verbindung bildet monomere Moleküle mit Abständen S—Cl von 207,1 pm, SN von 154,5 pm und PN von 161,6 pm.[SCl(NPPh3)2]Cl: Raumgruppe P21/c, Z = 4, Strukturlösung mit 5 224 unabhängigen beobachteten Reflexen, R = 0,042. Gitterabmessungen bei 20°C: a = 1 108,6; b = 1 603,8; c = 1 840,5 pm, β = 99,98°. Die Verbindung bildet Ionen [SCl(NPPh3)2]+ und Cl-. Im Kation ist das Schwefelatom ϕ-tetraedrisch koordiniert mit einem langen S—Cl-Abstand von 248,5 pm und SN-Bindungslängen von 154,5 und 156,0 pm.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946201125
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  • 4
    Electronic Resource
    Electronic Resource
    Phosphaniminato-Komplexe des Schwefels. Synthese und Kristallstrukturen von [O3SS(NPPh3)2] · CH3CN, [SO(NPPh3)2] und [SCl(NPMe3)2]ClProfessor Dirk Reinen zum 65. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 531-536 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes of Sulfur ; Syntheses ; IR Spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorane Iminato Complexes of Sulfur. Syntheses and Crystal Structures of [O3SS(NPPh3)2] · CH3CN, [SO(NPPh3)2], and [SCl(NPMe3)2]ClThe title compounds have been prepared by the reaction of Me3SiNPPh3 with SO2 and SOCl2, respectively, and by the reaction of Me3SiNPMe3 with S2Cl2. They form colourless, moisture sensitive crystals, which were characterized by IR spectroscopy and by crystal structure determinations.[O3SS((NPPh3)2)] · CH3CN: Space group Pca21, Z = 4, structure solution with 4016 observed unique reflections, R = 0.050. Lattice dimensions at -60°C: a = 1865.1, b = 1168.4, c = 1569.0 pm. The compound has a zwitterionic structure with a S—S bond length of 218.2 pm and bond lengths S—N of 161.2 and P—N of 160.1 pm.[SO(NPPh3)2]: Space group P21/c, Z = 4, structure solution with 2854 observed unique reflections, R = 0.113. Lattice dimensions at -50°C: a = 1173.1, b = 1585.6, c = 1619.2 pm, b̃ = 98.13°. The compound forms monomeric molecules, in which the positions of S and N atoms are disordered in two positions. The bond lengths are S—N 166 pm and P—N 163 pm in average.[SCl(NPMe3)2]Cl: Space group P1, Z = 2, structure solution with 2416 observed unique reflections, R = 0.038. Lattice dimensions at 20°C: a = 613.2, b = 1030.3, c = 1111.4 pm, α = 88.48°, b̃ = 88.01°, γ = 83.10°. The compound forms ions [SCl(NPMe3)2]+ and Cl-. In the cation the sulfur atom is φ-tetrahedrally coordinated with a long S—Cl distance of 246.9 pm and bond lengths S—N of 155.3 pm and P—N of 164.3 pm in average.
    Notes: Die Titelverbindungen entstehen durch Umsetzung von Me3SiNPPh3 mit Schwefeldioxid bzw. mit Thionylchlorid und von Me3SiNPMe3 mit Dischwefeldichlorid als farblose, feuchtigkeitsempfindliche Kristalle, die wir durch die IR-Spektren und durch Kristallstrukturanalysen charakterisiert haben.[O3SS(NPPh3)2)] · CH3CN: Raumgruppe Pca21, Z = 4, Strukturlösung mit 4016 unabhängigen beobachteten Reflexen, R = 0,050. Gitterabmessungen bei -60°C: a = 1865,1; b = 1168,4; c = 1569,0 pm. Die Verbindung hat eine zwitterionische Struktur mit einer S—S-Bindungslänge von 218,2 pm und Abständen S—N von 161,2 pm und P—N von 160,1 pm.[SO(NPPh3)2]: Raumgruppe P21/c, Z = 4, Strukturbestimmung mit 2854 unabhängigen beobachteten Reflexen, R = 0,113. Gitterabmessungen bei -50°C: a = 1173,1; b = 1585,6; c = 1619,2 pm, b̃ = 98,13°. Die Verbindung hat eine monomere Molekülstruktur, deren S- und N-Atomlagen in zwei Positionen fehlgeordnet sind. Die Bindungslängen betragen im Mittel für S—N 166 pm und für P—N 163 pm.[SCl(NPMe3)2]Cl: Raumgruppe P1, Z = 2, Strukturlösung mit 2416 unabhängigen beobachteten Reflexen, R = 0,038. Gitterabmessungen bei 20°C: a = 613,2; b = 1030,3; c = 1111,4 pm, α = 88,48°; b̃ = 88,01°; γ = 83,10°. Die Verbindung besteht aus Ionen [SCl(NPMe3]2+ und Cl-. Im Kation ist das Schwefelatom φ-tetraedrisch koordiniert mit einem S—Cl-Abstand von 246,9 pm und mittleren Bindungslängen S—N von 155,3 pm und P—N von 164,3 pm.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210405
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