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  • 1
    Electronic Resource
    Electronic Resource
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 54 (1998), S. 1804-1807 
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 51 (1995), S. 1388-1390 
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 51 (1995), S. 562-565 
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 52 (1996), S. 1663-1666 
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 52 (1996), S. 818-820 
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 225-228 
    ISSN: 0044-2313
    Keywords: Polyiodide ; triiodide ; urotropinium triiodide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on Polyhalides. 17. Preparation and Crystal Structure of Urotropinium Triiodide, UrHI3Urotropinium triiodide C6H13N4I3 is formed by the reaction of equimolar amounts of urotropinium iodide and iodine in tBuOH as red-brown cube-like crystals melting at 402 K under decomposition. The compound crystallizes monoclinically in the space group P21/c with a = 952.0(3) pm, b = 1 160.2(6) pm, c = 1 149.9(4) pm, β = 92.22(3)° and Z = 4. The till now not described crystal structure (R = 0.027 for 1 860 observed reflexes) contains urotropinium ions UrH+ and slightly distorted triiodide ions I3-(d(I - I) = 292.3(1), 294.1(1) pm, ϕ(I - I - I) = 178.27(2)°) which are linked to ion pairs by a rather short contact (d(I … I) = 389.0(1) pm, ϕ(I - I … I) = 149.12(2)°).
    Notes: Urotropiniumtriiodid C6H13N4I3 fällt bei der Umsetzung äquimolarer Mengen Urotropiniumiodid und Iod aus tBuOH in rotbraunen würfelähnlichen Kristallen an, die bei 402 K unter Zersetzung schmelzen. Die Substanz kristallisiert in der monoklinen Raumgruppe P21/c mit a = 952,0(3) pm, b = 1 160,2(6) pm, c = 1 149,9(4) pm, β = 92,22(3)° und Z = 4. Die bisher nicht beschriebene Kristallstruktur (R = 0,027 für 1 860 beobachtete Reflexe) enthält Urotropiniumionen UrH+ und geringfügig verzerrte Triiodidionen I3-(d(I - I) = 292,3(1), 294,1(1) pm, ϕ(I - I - I) = 178,27(2)°), die über einen kurzen Kontakt Ionenpaare bilden (d(I … I) = 389,0(1) pm, ϕ(I - I … I) = 149,12(2)°).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 218-224 
    ISSN: 0044-2313
    Keywords: Polyiodides ; triiodide ; pentaiodide ; heptaiodide ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on Polyhalides. 16. Preparation and Crystal Structures of Bipyridiniumpolyiodides Bipy · HIn with n = 3, 5, and 7With simply protonated α,α′-Bipyridyl Bipy · H+ a triiodide Bipy · HI3, a pentaiodide Bipy · HI5 and a heptaiodide Bipy · HI7 may be prepared in the presence of iodide ions I- and dependent of the iodine I2 content.Bipyridiniumtriiodide C10H9N2I3 crystallizes at room temperature monoclinically in P21/n with a = 1 122.8(1) pm, b = 1 072.7(1) pm, c = 1 200.2(3) pm, β = 98.02(2)° and Z = 4. The crystal structure is built up from mixed cationic and anionic layers.Bipyridiniumpentaiodide C10H9N2I5 crystallizes at room temperature monoclinically in P21/c with a = 887.3(5) pm, b = 2 527.9(12) pm, c = 830.7(3) pm, β = 106.78(5)° and Z = 4. The crystal structure contains triiodide ions I3- till now uniquely connected by iodine molecules I2 in a trigonal planar way.Bipyridiniumheptaiodide C10H9N2I7 crystallizes at room temperature triclinically in P&1macr; with a = 713.1(3) pm, b = 1 007.9(3) pm, c = 1 464,8(4) pm, α = 81.07(3)°, β = 89.92(3)°, γ = 82.77(3)° and Z = 2. The crystal structure contains a V-shaped pentaiodide ion I5- completed by an iodine molecule I2 to a trigonal pyramidally shaped heptaiodide ion I7- and at the same time connected to a zigzag chain.
    Notes: Mit einfach protoniertem α,α′-Bipyridyl Bipy · H+ lassen sich in Gegenwart von Iodid I- und in Abhängigkeit vom Iodangebot I2 ein Triiodid Bipy · HI3, ein Pentaiodid Bipy · HI5 und ein Heptaiodid Bipy · HI7 fällen und einkristallin gewinnen.Bipyridiniumtriiodid C10H9N2I3 kristallisiert bei Raumtemperatur in der monoklinen Raumgruppe P21/n mit a = 1 122,8(1) pm, b = 1 072,7(1) pm, c = 1 200,2(3) pm, β = 98,02(2)° und Z = 4. Die Kristallstruktur wird aus im Wechsel kationisch und anionisch gemischten Schichten aufgebaut.Bipyridiniumpentaiodid C10H9N2I5 kristallisiert bei Raumtemperatur in der monoklinen Raumgruppe P21/c mit a = 887,3(5) pm, b = 2 527,9(12) pm, c = 830,7(3)pm, β = 106,78(5)° und Z = 4. Die Kristallstruktur enthält Triiodidionen I3-, die bisher einzigartig durch Iodmoleküle I2 trigonal planar zu zickzackartigen Ketten verknüpft werden.Bipyridiniumheptaiodid C10H9N2I7 kristallisiert bei Raumtemperatur in der triklinen Raumgruppe P&1macr; mit a = 713,1(3) pm, b = 1 007,9(3) pm, c = 1 464,8(4) pm, α = 81,07(3)°, β = 89.92(3)°, γ = 82,77(3)° und Z = 2. Die Kristallstruktur enthält ein V-förmiges Pentaiodidion I5-, das durch ein Iodmolekül I2 zu einem trigonal pyramidalen Heptaiodid I7- ergänzt und gleichzeitig zickzackartig verkettet wird.
    Additional Material: 6 Ill.
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  • 8
    ISSN: 0044-2313
    Keywords: Tris(fluorophenyl)antimony and -bismuth compounds ; bismuth tris(2,6-difluorobenzoate) ; preparations ; crystal structure of tris(2,6-difluorophenyl)bismuth ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Properties of Some New Tris(fluorophenyl)antimony and -bismuth Compounds. Crystal Structure of Tris(2,6-difluorophenyl)bismuth(2,6-F2C6H3)3Bi, (2,4,6-F3C6H2)3Bi, and (2,6-F2C6H3)3Sb are prepared via Grignard reactions with BiBr3 and SbBr3, respectively. The syntheses and properties of the new compounds and the crystal structure of (2,6-F2C6H3)3Bi are described. From the reaction of BiBr3 with Ag(OCOC6H3F2) the bismuth benzoate Bi(OCOC6H3F2)3 is formed in 83% yield. Attempts to prepare (2,6-F2C6H3)3Bi by decarboxylation of the bismuth benzoate failed.
    Notes: (2,6-F2C6H3)3Bi, (2,4,6-F3C6H2)3Bi und (2,6-F2C6H3)3Sb werden durch Grignard-Reaktionen mit BiBr3 bzw. SbBr3 dargestellt. Die Synthesebedingungen und die Eigenschaften der neuen Verbindungen sowie die Kristallstruktur von (2,6-F2C6H3)3Bi werden beschrieben. Bi(OCOC6H3F2)3 entsteht in 83% Ausbeute aus BiBr3 und Ag(OCOC6H3F2); die präparative Darstellung von (2,6-F2C6H3)3Bi durch Decarboxylierung des Bismutbenzoats gelingt nicht.
    Additional Material: 3 Ill.
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  • 9
    ISSN: 0044-2313
    Keywords: Arylxenon trifluoromethanesulfonates ; electrophilic aromatic substitution ; xenontrifluoroacetate trifluoromethanesulfonate ; NMR spectra ; X-ray crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die direkte Synthese von Arylxenontrifluormethansulfonaten durch elektrophile SubstitutionBei der Reaktion von Xenonbis(trifluoracetat) mit Trifluormethansulfonsäure wird die neue, hochreaktive, unsymmetrische Xenon-Sauerstoff-Verbindung CF3COOXeOSO2CF3 erzeugt. Benzolderivate mit elektronenziehenden Substituenten wie F, CF3, Cl und NO2 werden von diesem Intermediat unter Bildung von Arylxenontrifluormethansulfonaten elektrophil angegriffen. Über diese Eintopfsynthese wurden Trifluormethansulfonate mit den Kationen [Xe(2,4,6-F3C6H2)]+, [Xe(2-F-5-NO2C6H3)]+, [Xe(2-F-5-CF3C6H3)]+ und [Xe(3,5-(CF3)2C6H3)]+ synthetisiert. Alle Verbindungen wurden durch ihre NMR-, Massen- und Schwingungsspektren charakterisiert.Zusätzlich wurden mehrere neue Arylxenontrifluormethansulfonate als Produkte der Umsetzungen von 1,3-F2C6H4 und weiteren desaktivierten Benzolen mit Xenon(trifluoracetat)trifluormethansulfonat anhand der 129Xe-NMR-Spektren identifiziert.Fluorsubstituenten in ortho-Position zu Xenon erhöhen signifikant die thermische Stabilität der Arylxenontrifluormethansulfonate.Die Molekülstruktur von [Xe(2,6-F2C6H3)][OSO2CF3] wurde durch eine Einkristallröntgenstrukturanalyse bestimmt. Die Arylxenoneinheit koordiniert schwach mit einem Sauerstoffatom des CF3SO3-Anions. Die Verbindung kristallisiert in der triklinen Raumgruppe mit a = 880.9(3) pm, b = 1093.9(5) pm, c = 1209.8(5) pm, α = 89.04(4)°, β = 74.23(3)°, γ = 86.03(3)°, Z = 4.
    Notes: The reaction of xenonbis(trifluoroacetate) and trifluoromethanesulfonic acid (triflic acid) gave the new, highly reactive unsymmetrical xenon-oxo species CF3COOXeOSO2CF3. Benzene derivates, containing electron withdrawing substituents such as -F, -CF3, -Cl or -NO2 were electrophilic attacked by this intermediate to yield arylxenon trifluoromethanesulfonates. Via this one-pot synthesis trifluoromethanesulfonates with the cations [Xe(2,4,6-F3C6H2)]+, [Xe(2-F-5-NO2C6H3)]+, [Xe(2-F-5-CF3C6H3)]+ and [Xe(3,5-(CF3)2C6H3)]+ were prepared. All compounds were characterized by their NMR, mass, and vibrational spectra.Additionally, several new arylxenon trifluoromethanesulfonates were detected by 129Xe-NMR spectroscopy as products of the reaction of 1,3-F2C6H4 and further deactivated benzenes with xenontrifluoroacetate trifluoromethane sulfonate.Fluoro substituents in ortho position to xenon significantly increase the thermal stability of the arylxenon trifluoromethanesulfonates obtained.The molecular structure of [Xe(2,6-F2C6H3)][OSO2CF3] was determined by single crystal diffraction methods. The arylxenon unit is weakly coordinated by one oxygen atom of the CF3SO3 anion. The salt crystallizes in the triclinic space group P1, a = 880.9(3) pm, b = 1093.9(5) pm, c = 1209.8(5) pm, α = 89.04(4)°, β = 74.23(3)°, γ = 86.03(3)°, Z = 4.
    Additional Material: 7 Ill.
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