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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 962-966 
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes ; Sulfur Compounds ; 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. Crystal Structures of [S(NPEt3)3]Cl, [S(NPEt3)2]CI2 and [Me3SiOSO2NPPh3]The ionic phosphorane iminato complexes [S(NPEt3)3]Cl and [S(NPEt3)2]Cl2 are obtained as colourless, moisture sensitive crystals after reaction of Me3SiNPEt3 with disulfur dichloride from acetonitrile solutions. Both complexes, as well as the molecular complex [Me3SiOSO2NPPh3]. which is known from literature data, were characterized by crystal structure determinations.
    Notes: Die ionisch aufgebauten Phosphaniminato-Komplexe [S(NPEt3)3]Cl und [S(NPEt3)2]Cl2 entstehen als farblose, feuchtigkeitsempfindliche Kristalle nach Reaktion von Me3SiNPEt3 mit Dischwefeldichlorid in Acetonitrillösung. Beide Komplexe werden ebenso wie die literaturbekannte Molekülverbindung [Me3SiOSO2NPPh3] durch Kristallstrukturanalysen charakterisiert.
    Additional Material: 3 Ill.
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  • 2
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes ; Copper(II) ; Synthesis ; Magnetic Behaviour ; EPR Spectrum ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Cu4(NPMe3)3(O2C—CH3)5] - a Tetrameric Phosphorane Iminato Complex of Copper(II). Synthesis, Crystal Structure, Magnetic Behaviour, and EPR SpectrumThe title compound and the corresponding benzoate complex [Cu4(NPMe3)3(O2C—C6H5)5] have been prepared by reactions of copper(II)acetate and copper(II)benzoate, respectively, with Me3SiNPMe3 in dichloromethane. Both complexes are characterized by IR spectroscopy. The acetate complex is additionally characterized by the measurement of the magnetic susceptibility, by its EPR spectrum, and by a crystal structure determination.[Cu4(NPMe3)3(O2C—CH3)5] · CH2Cl2: Space group I41/a, Z = 16, structure solution with 7 960 independent reflections, R = 0.044. Lattice dimensions at -70°C: a = b = 3 670.6; c = 1 091.9 pm. The structure consists of four Cu atoms which are arranged at the corners of a distorted tetrahedron with Cu…Cu distances between 290 and 318 pm. Three of the faces of the tetrahedron are linked by μ3-N atoms of the phosphorane iminato groups. Three of the acetate ligands form chelates, the other two are monofunctionally coordinated. Three of the copper atoms have a planar surrounding, the forth Cu atom has a (4 + 1) coordination.
    Notes: Die Titelverbindung sowie der entsprechende Benzoat-Komplex [Cu4(NPMe3)3(O2C—C6H5)5] wurden durch Reaktion von Kupfer(II)acetat bzw. von Kupfer(II)benzoat mit Me3SiNPMe3 in Dichlormethan hergestellt und durch ihre IR-Spektren charakterisiert. Der Acetatkomplex wurde zusätzlich durch die Messung der magnetischen Suszeptibilität, des EPR-Spektrums und durch eine Kristallstrukturanalyse charakterisiert.[Cu4(NPMe3)3(O2C—CH3)5] · CH2Cl2: Raumgruppe I41/a, Z = 16, Strukturlösung mit 7 960 unabhängigen Reflexen, R = 0,044. Gitterkonstanten bei -70°C: a = b = 3 670,6; c = 1 091,9 pm. Die Struktur besteht aus vier Cu-Atomen, die ein verzerrtes Tetraeder bilden mit Cu…Cu-Abständen zwischen 290 und 318 pm. Drei der Tetraederflächen sind durch μ3-N-Atome dreier NPMe3--Gruppen überbrückt, drei der Acetatliganden sind chelatartig gebunden, während zwei Acetatgruppen monofunktionell koordinieren. Drei der Cu-Atome haben planare Umgebung, das vierte hat eine (4 + 1)-Koordination.
    Additional Material: 5 Ill.
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