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  • 1
    Publication Date: 1982-08-01
    Print ISSN: 0044-2313
    Electronic ISSN: 1521-3749
    Topics: Chemistry and Pharmacology
    Published by Wiley
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  • 2
    Publication Date: 1983-03-01
    Print ISSN: 0044-2313
    Electronic ISSN: 1521-3749
    Topics: Chemistry and Pharmacology
    Published by Wiley
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  • 3
    Publication Date: 1983-07-01
    Print ISSN: 0044-2313
    Electronic ISSN: 1521-3749
    Topics: Chemistry and Pharmacology
    Published by Wiley
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  • 4
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitrosyl Bromo Complexes of Rhenium: Re(NO)2Br3 and [Re(NO)2Br4]⊖; Crystal Structure of PPh4[Re(NO)2Br4] · 2 CCl4PPh4[Re(NO)2Br4] is prepared in the form of dark red-brown powder by the reaction of PPh4[Re(NO)2Cl4] with excess boron tribromide. From a solution of CH2Br2 and CCl4 it crystallizes with two moles CCl4, one of which splits off easily in vacuo. The reaction of aluminum tribromide in CH2Br2 solution leads to a slightly soluble red-brown Re(NO)2Br3 powder. The i.r. spectra indicate cis positions of the covalently bound NO ligands in both complexes. Re(NO)2Br3 is dimeric via bromo bridges.The crystal structure determination of PPh4[Re(NO)2Br4] · 2 CCl4 was solved by X-ray diffraction methods at - 115°C. The complex crystallizes in the monoclinic space group P21/c with four formula units per unit cell (4434 independent reflexions, R = 0.085). The unit cell dimensions are a = 1 092.3 pm, b = 2088.0 pm, c = 1 657.6 pm, β = 96.10°. The structure consists of P(C6H5)4⊖ cations, [Re(NO)2Br4]⊖ anions and intercalated CCl4 molecules. In the anion the NO groups are covalently bound to the Re atom like \documentclass{article}\pagestyle{empty}\begin{document}$ \mathop {{\rm RE}}\limits^ \ominus = \mathop {\rm N}\limits^ \oplus = {\rm O} $\end{document} and they are arranged in cis position to one another.
    Notes: PPh4[Re(NO)2Br4] entsteht als dunkelrotbraunes Pulver aus PPh4[Re(NO)2Cl4] mit überschüssigem Bortribromid. Aus Lösungen von CH2Br2 und CCl4 kristallisiert es unter Einschluß von zwei Mol CCl4, von denen i. Vak. eines leicht abgegeben wird. Mit Aluminiumtribromid läßt sich aus [Re(NO)2Br4]⊖ in CH2Br2-Lösung ein Bromidligand abspalten, wobei Re(NO)2Br3 als schwerlösliches, rotbraunes Pulver ausfällt. Die IR-Spektren ergeben Aufschluß über cis-ständige Nitrosylliganden, die kovalent an Rhenium gebunden sind. Re(NO)2Br3 ist über Bromobrücken dimerisiert.Die Kristallstruktur von PPh4[Re(NO)2Br4] · 2 CCl4 wurde mittels Röntgenbeugung bei - 115°C ermittelt. Der Komplex kristallisiert in der monoklinen Raumgruppe P21/c mit vier Formeleinheiten pro Elementarzelle (4434 unabhängige Reflexe, R = 0,085) und mit den Gitterabmessungen a = 1 092,3 pm, b = 2 088,0 pm, c = 1 657,6 pm und β = 96,10°. Die Struktur besteht aus P(C6H5)4⊖-Kationen, [Re(NO)2Br4]⊖-Anionen und eingelagerten CCl4-Molekülen. In den komplexen Anionen sind die Nitrosylliganden in gestreckter Koordination und in cis-Stellung zueinander orientiert.
    Additional Material: 2 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 502 (1983), S. 35-44 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Rhenium Trichloride Dinitrosyl with Triphenyl Phosphane. Crystal Structure of [ReCl3(NO) (NPPh3) (OPPh3)]Triphenyl phosphane reacts with ReCl3(NO)2 in dichloro methane solution forming the phosphaneiminato complex [ReCl3(NO)(NPPh3)(OPPh3)], which is characterized by it's i.r. spectrum and by 31P nuclear magnetic resonance. The crystal structure was determined by the aid of X-ray diffraction data (3 133 independent reflexions, R = 3.9%). The complex crystallizes monoclinic in the space group P21/n with four formula units per unit cell. The lattice dimensions are a = 1114, b = 1825, c = 1931 pm, β 96.6°. In the complex the rhenium atom has the coordination number six, the ligands being three chlorine atoms, the linear bonded Nitrosyl group, the O atom of the triphenyl phosphane oxide, which is coordinated trans to the NO ligand, and the N atom of the phosphaneiminato group. The ReN and PN bond lengths of the (NPPh3)⊖ ligand (186 and 163 pm, resp.) indicate double bond character; in contrast to other phosphaneiminato complexes of transition metals with linear array M=N=P, in [ReCl3(NO)(NPPh3)(OPPh3)] the Re—N—P bond angle is only 139°.
    Notes: Triphenylphosphan reagiert in Dichlormethanlösung mit ReCl3(NO)2 unter Bildung des Phosphaniminatokomplexes [ReCl3(NO)(NPPh3)(OPPh3)], der mittels des IR-Spektrums und des 31P-Kernresonanzspektrums charakterisiert wird. Die Kristallstruktur wurde mit Hilfe von Röntgenbeugungsdaten ermittelt (3133 unabhängige Reflexe, R = 3,9%). Der Komplex kristallisiert in der monoklinen Raumgruppe P21/n mit vier Formeleinheiten pro Elementarzelle. Die Gitterkonstanten sind a = 1114, b = 1825, c = 1931 pm, β 96,6°. In dem Komplex ist das Rheniumatom sechsfach von drei Chloratomen, von dem in gestreckter Anordnung gebundenen Nitrosylliganden, von dem in trans-Position zur NO-Gruppe koordinierten O-Atom des Triphenyl-phosphanoxidmoleküls und von dem N-Atom des Triphenylphosphaniminatoliganden umgeben. Die ReN- und die PN-Bindungsabstände des (NPPh3)⊖-Liganden entsprechen mit 186 bzw. 163 pm etwa Doppelbindungen; im Gegensatz zu anderen Phosphaniminatokomplexen von Übergangsmetallen mit gestreckter Gruppe M=N=P beträgt im [ReCl3(NO)(NPPh3)(OPPh3)] der ReNP-Bindungswinkel nur 139°.
    Additional Material: 3 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 498 (1983), S. 131-138 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: {ReCl2(NO)2[Sb(C6H5)3]2}; Preparation, Crystal Structure, Infrared and 121Sb Mössbauer SpectrumThe title compound yields from treatment of ReCl3(NO)2 with excess Sb(C6H5)3 in a dichloromethane suspension forming green crystals. The structure of {ReCl2(NO)2[Sb(C6H5)3]2} was solved by X-ray methods; the complex crystallizes in the triclinic space group P1 with three formula units per unit cell (9522 undependent, observed reflexions, R = 5.0%). The lattice constants are a = 1251, b = 1414, c = 1671 pm, α = 66.2, β = 83.0, γ = 89.1°. The Rhenium atom is coordinated octahedrally by two NO groups, two Cl atoms, which are in cis-position to one another and two antimony atoms of the SbPh3 ligands, which are in trans positions. The NO and Cl ligands are statistically disordered in the equatorial plane. The I.R. spectrum as well as the 121Sb-Mössbauer spectrum, the latter obtained at 4.2 K, are recorded.
    Notes: Die Titelverbindung entsteht bei der Einwirkung von überschüssigem Triphenylantimon auf ReCl3(NO)2 in Dichlormethan-Suspension in Form grüner Kristalle. {ReCl2(NO)2[Sb(C6H5)3]2} kristallisiert nach Röntgenbeugungsmessungen triklin in der Raumgruppe P1 mit drei Formeleinheiten pro Elementarzelle (9 522 unabhängige, beobachtete Reflexe, R = 5,0%). Die Gitterabmessungen sind a = 1251, b = 1414, c = 1671 pm; α = 66,2, β = 83,0, γ = 89,1°. In dem Komplex ist das Re-Atom oktaedrisch von zwei cis-ständigen Nitrosylgruppen, zwei cis-ständigen Chlorliganden und von den beiden Antimonatomen der zueinander trans-ständigen Triphenyl-antimongruppen umgeben. Nitrosyl- und Chlorliganden sind statistisch fehlgeordnet. Das IR-Spektrum und das bei 4,2 K registrierte 121Sb-Mößbauer-Spektrum werden mitgeteilt.
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