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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1599-1608 
    ISSN: 0044-2313
    Keywords: Cyclophosphazenes ; [3]ferrocenophanes ; 1,1′-ferrocene-dichalcogenato compounds ; NMR spectra ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Ferrocenol and 1,1′-Ferrocendiol with Cyclotriphosphazenes, P3N3F6 and P3N3Cl6The hexahalogeno-cyclotriphosphazenes, P3N3X6 (X = F (1 a), Cl (1 b)), react with ferrocenol (FcOH) in a molar ratio 1 : 1 to give the ferrocenoxy derivatives, FcO[P3N3X5] (X = F (3 a), Cl (3 b)); in an analogous manner the tetrameric ring P4N4Cl8 (2 b) is converted to FcO[P4N4Cl7] (4 b). Abkürzungen: Fc = Ferrocenyl, (C5H5)Fe(C5H4-); fc = 1,1′-ferrocendiyl, Fe(C5H4-)2; rc = 1,1′-ruthenocendiyl, Ru(C5H4-)2. Fluorphosphazene werden mit a, Chlorphosphazene mit b gekennzeichnet. With 1,1′-ferrocenediol, (fc(OH) 2), the cyclo triphosphazenes react in a molar ratio 1 : 1 to produce fcO 2[P 3 N 3 X 4] (X = F ( 5 a), Cl ( 5 b)). According to the x-ray structure analysis, the 1,1′-ferrocenediolato group in 5 a , b is bound to two different phosphorus atoms. On the contrary, the 1,1′-ferrocenedithiolato- and 1,1′-ferrocenediselenolato units in fcS 2[P 3 N 3 X 5] (X = F ( 6 a), Cl ( 6 b)) and fcSe 2[P 3 N 3 X 5] (X = F ( 7 a), Cl ( 7 b)) are attached to only one phosphorus atom, and spirocyclic 1,3-dichalcogena-2-phospha-[3]ferrocenophanes are formed. All new products have been characterized on the basis of their 1 H, 13 C and 31 P NMR as well as EI mass spectra. The molecular structures of 5 a , b and 6 a have been determined by x-ray structure analyses.
    Notes: Die Hexahalogen-cyclotriphosphazene, P3N3X6 (X = F (1 a), Cl (1 b)), reagieren mit Ferrocenol, FcOH, im Molverhältnis 1 : 1 unter Bildung der Ferrocenoxy-Derivate FcO[P3N3X5] (X = F (3 a), Cl (3 b)); der tetramere Ring P4N4Cl8 (2 b) bildet in analoger Weise FcO[P4N4Cl7] (4 b). 1,1′-Ferrocendiol, fc(OH)2, setzt sich mit P3N3X6 im Molverhältnis 1 : 1 zu fcO2[P3N3X4] (X = F (5 a), Cl (5 b)) um; nach der Röntgenstrukturanalyse ist der 1,1′-Ferrocendiolato-Rest in 5 a, b an zwei verschiedene Phosphoratome gebunden. Dagegen werden die 1,1′-Ferrocendithiolat- und 1,1′-Ferrocendiselenolat-Reste in fcS2[P3N3X4] (X = F (6 a), Cl (6 b)) bzw. fcSe2[P3N3X4] (X = F (7a), Cl (7 b)) jeweils nur an ein Phosphoratom angekoppelt, so daß spirocyclische 1,2-Dichalkogena-2-phospha[3]ferrocenophane entstehen. Alle neuen Produkte wurden anhand ihrer 1H-, 13C- und 31P-NMR-Spektren und der EI-Massenspektren charakterisiert; für 5 a, b und 6 a wurde die Molekülstruktur durch Röntgenstrukturanalyse bestimmt.
    Additional Material: 3 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 545-553 
    ISSN: 0044-2313
    Keywords: Cyclotetraphosphazenes ; [3]ferrocenophanes ; NMR spectra ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,1′-Ferrocene Dichalcogenato Derivatives of Octachloro-cyclotetraphosphazeneMononuclear 1,1′-ferrocenedichalcogenato derivatives of octachloro-cyclotetraphosphazene, fcE2[P4N4Cl6] (E = O (12), S (13), Se (14), have been prepared and characterized by 1H, 13C and 31P NMR spectroscopy as well as mass spectrometry.1) The molecular structures of 12--14 were determined by X-ray crystallography. While the 11′-ferrocene diolato complex, fcO2[P4N4Cl6] (12), possesses a 1,3-transannular bridged structure, the dithiolato and diselenolato analogues, 13 and 14, are spiro compounds containing 1,3-dichalcogena-2-phospha-[3]ferrocenophane rings. According to their temperature-dependent NMR spectra, 13 and 14 are nonrigid molecules above room temperature in solution.
    Notes: Es wurden einkernige 1,1′-Ferrocendichalkogenato-Derivate des Oktachlor-cyclotetraphosphazens, fcE2[P4N4Cl6] (E = O (12), S (13), Se (14), dargestellt und mit Hilfe der 1H-, 13C- und 31P-NMR-Spektroskopie sowie der Massenspektrometrie charakterisiert.1) Die Molekülstrukturen von 12-14 wurden durch Röntgenstrukturanalysen bestimmt. Während der 1,1′-Ferrocendiolato-Komplex, fcO2[P4N4Cl6] (12), eine 1,3-transannular verbrückte Struktur besitzt, sind die Dithiolato- und Diselenolato-Analoga, 13 und 14, Spiroverbindungen mit l,3-Dichalkogena-2-phos pha-[3]ferrocenophan-Ringen. Entsprechend den temperaturabhängigen NMR-Spektren sind 13 und 14 oberhalb Raumtemperatur in Lösung nichtstarre Moleküle.
    Additional Material: 1 Ill.
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