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  • 1
    Electronic Resource
    Electronic Resource
    [Mo(NPPh3)4]2+ [MoNCl3(NPPh3)]2- · C7H8, ein Phosphaniminato-Komplex mit einem Dikation von Molybdän(VI) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 507-512 
    Details
    ISSN: 0044-2313
    Keywords: Phosphoraneiminato Complex of Molybdenum ; Synthesis ; IR Spectrum ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Mo(NPPh3)4]2+ [MoNCl3(NPPh3)]2- · C7H8, a Phosphoraneiminato Complex with a Dication of Molybdenum(VI).The title compound was prepared by the reaction of MoNCl3 with Me3SiNPPh3 in acetonitrile solution. Red single crystals separated upon addition of toluene. They were characterized by IR spectroscopy and by an X-ray structure determination. (Space group P1, Z = 2, 6918 observed unique reflections, R = 0.059. Lattice dimensions at 20°C: a = 1 181.4, b = 2 021.4, c =2 409.7pm; α = 65.87°, β = 101.09°, γ= 78.97°). In the dication [Mo(NPPh3)4]2+ the molybdenum atom is surrounded in a tetrahedral fashion by the four nitrogen atoms of the phosphorane iminato ligands. The MoN and PN bond lengths correspond well with double bonds. In the two anions [MoNCl3(NPPh3)]-, which occur in different conformations, the molybdenum atoms are fivefold coordinated by the terminal nitride ligand Mo≡N: in axial positions and by the three chlorine atoms and the nitrogen atom of the (NPPh3)- ligand in the equatorial positions.
    Notes: Die Titelverbindung entsteht in Form leuchtend roter Einkristalle bei der Einwirkung von Me3SiNPPh3 auf MoNCl3 in Acetonitrillösung nach Zugabe von Toluol. Sie wird durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P1, Z = 2, 6918 beobachtete unabhängige Reflexe, R = 5,9%. Gitterabmessungen bei 20°C: a = 1 181,4; b = 2 021,4; c = 2 409,7pm; α = 65,87°; β = 101,09°; γ= 78,97°. In dem Dikation [Mo(NPPh3)4]2+ ist das Molybdänatom tetraedrisch von den vier N-Atomen der Phosphaniminatoliganden umgeben mit MoN- und PN-Abständen, die Doppelbindungen entsprechen. Die beiden symmetrieunabhängigen Anionen [MoNCl3(NPPh3)]- besitzen verschiedene Konformationen. In ihnen sind die Molybdänatome fünffach von dem terminalen Nitridoliganden Mo≡N: in axialer Position und von den drei Chloratomen und dem N-Atom des Phosphaniminatoliganden Äquatorial koordiniert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190312
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  • 2
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur einer neuen Modifikation von Tetraselentetranitrid, Se4N4 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1011-1015 
    Details
    ISSN: 0044-2313
    Keywords: New modification of Se4N4 ; Synthesis ; IR Spectrum ; 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 a New Modification of Tetraselenium Tetranitride, Se4N4β-Se4N4 has been prepared by the reaction of selenium dioxide with the phosphane imine Me3SiNPMe3 in acetonitrile, forming red-brown crystal needles. The crystal structure analysis shows a new modification, the IR spectrum of which differs only slightly from the known α-form of Se4N4 (space group C2/c).β-Se4N4: Space group P21/n, Z = 4, structure solution with 1 667 observed unique reflections, R = 0.054. Lattice dimensions at -50°C: a = 881.8(2), b = 738.7(2), c = 899.6(2) pm, β = 93.58(1)°. Just as the α-form β-Se4N4 forms cage molecules without symmetry and intramolecular Se—Se contacts of 273.2 and 274.0 pm. There are strong Se…N-interactions between the Se4N4 molecules.
    Notes: β-Se4N4 entsteht in Form rotbrauner Kristallnadeln bei der Reaktion von Selendioxid mit dem Phosphanimin Me3SiNPMe3 in Acetonitrillösung. Die Kristallstruktur-analyse ergab das Vorliegen einer neuen Modifikation, deren IR-Spektrum sich nur wenig von der bekannten α-Form des Se4N4 (Raumgruppe C2/c) unterscheidet.β-Se4N4: Raumgruppe P21/n, Z = 4, Strukturlösung mit 1 667 beobachteten unabhängigen Reflexen, R = 0,054. Gitterkonstanten bei -50°C: a = 881,8(2); b = 738,7(2); c = 899,6(2) pm, β = 93,58(1)°. β-Se4N4 bildet wie die α-Form Käfigmoleküle, die ohne Symmetrie sind und zwei intramolekulare Se—Se-Kontakte von 273,2 und 274,0 pm ausbilden. Zwischen den Molekülen bestehen starke Se…N-Wechselwirkungen.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200610
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  • 3
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur des Selenyl-Phosphaniminato-Komplexes SeO(NPPh3)2 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1171-1174 
    Details
    ISSN: 0044-2313
    Keywords: Selenium ; Phosphorane Iminato Complex of Selenium ; Synthesis ; IR Spectrum ; 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 the Selenyl-Phosphoraneiminato Complex SeO(NPPh3)2SeO(NPPh3)2 has been prepared from SeO2 and Me3SiNPPh3 in a SeO2 suspension in acetonitrile, forming colourless crystals. The compound is characterized by IR spectroscopy and by a crystal structure determination. Space group P1, Z = 2, structure solution with 5 344 observed unique reflections, R = 0.064. Lattice dimensions at -40°C: a = 931.6, b = 947.6, c = 1 762 pm, α = 77.50°, β = 81.78°, γ = 79.23°. The compound forms monomeric molecules in which the selenium atom is ϕ-tetrahedrally surrounded with bond lengths SeO = 161.7 pm and SeN = 179.9 and 181.6 pm.
    Notes: SeO(NPPh3)2 entsteht in Form farbloser Kristalle bei der Reaktion einer Suspension von SeO2 mit Me3SiNPPh3 in Acetonitril. Die Verbindung wird durch das IR-Spektrum und durch eine Kristallstrukturanalyse charakterisiert. Raumgruppe P1, Z = 2, Strukturlösung mit 5 344 beobachteten unabhängigen Reflexen, R = 0,064. Gitterkonstanten bei -40°C: a = 931,6; b = 947,6; c = 1 762 pm, α = 77,50°, β = 81,78°, γ = 79,23°. Die Verbindung bildet monomere Moleküle, in denen das Selenatom verzerrt ϕ-tetraedrisch umgeben ist mit Abständen SeO = 161,7 pm und SeN = 179,9 und 181,6 pm.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210709
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