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  • 1
    Electronic Resource
    Electronic Resource
    Die Kristallstrukturen von Kalium-, Rubidium- und Cäsium-trifluororthocarbonat mit einer Bemerkung zum Bariumsulfat-Typ1 (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 321-327 
    Details
    ISSN: 0009-2940
    Keywords: Trifluororthocarbonates of potassium, rubidium, cesium ; Phase transitions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Crystal Structures of Potassium, Rubidium, and Cesium Trifluororthocarbonate and a Remark Concerning the Barium Sulfate Type1)Crystals of potassium, rubidium, and cesium trifluororthocarbonate (9a, 9b, and 9c) have been grown by Ostwald ripening in CH3CN applying a COF2 pressure of 3 bar. According to X-ray single-crystal structure analysis, 9a, 9b, and 9c belong to the baryte-structure family with an pseudotetrahedral anion being dynamically disordered at room temperature. All of the title compounds undergo a phase transition into a monoclinic, completely ordered low-temperature form, which has been refined for 9c. The C - O bond seems to be shortened by polar interactions. The results obtained with 9a, 9b, and 9c at room temperature indicate that the type of disorder found in 9 might be generally present in baryte-type compounds.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240212
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  • 2
    Electronic Resource
    Electronic Resource
    Synthesewege zu neuen ionischen Ozoniden (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 1383-1388 
    Details
    ISSN: 0009-2940
    Keywords: Phase-transfer catalysis ; Ozonides, ionic ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthetic Routes to New Ionic OzonidesNew synthetic routes to tetraorganylammonium ozonides involving exchange reactions with alkali metal ozonides were investigated. The previously reported reaction between tetraalkylammonium hyperoxides R4N+O2- (R = Me, Et) and alkali metal ozonides in liquid ammonia is severely hampered by the difficult synthesis of these hyperoxides; they are unknown for other quaternary ammonium cations. A similar reaction between the easily accessible chlorides of trialkylbenzylammonium ions and KO3 yields mixed ozonides/chlorides due to some solubility of KCl in liquid ammonia. The new compounds BzlMe3N+ (O3-)0.6Cl-0.4 (3), BzlEt3N+ (O3-)0.8Cl0.2- (4) and Bzl(nBu)3N+(O3-)0.5Cl0.5- (5) were prepared by this route. - The by far superior route to new ozonides utilizes macroreticular cation exchange resins in liquid ammonia. Batch equilibration between an excess of the appropriate ionic form of the resin and CsO3 produced Me3PhN+O3- (6), BzlMe3N+O3- (7), Bzl(nBu)3N+O3- (8), and (nPr)4N+ O3- (9) in almost quantitative yield. Compounds 4, 6, and 7 were studied by single-crystal X-ray analysis; the shortening of the ozonide bond length and the widening of the bond angle in comparison to the alkali metal ozonides as well as the possibility of C-H…O hydrogen bonding are discussed. Thermal stabilities were determined by DTA/TG methods, rapid decomposition starts at 59-79°C for 3, 6, and 7 and at 28-56°C for the remaining new ozonides which contain detachable β-H atoms.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250613
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  • 3
    Electronic Resource
    Electronic Resource
    Notiz/Note P4O7 und P4O6S, Vergleich der Molekül- und Kristallstrukturen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1711-1714 
    Details
    ISSN: 0009-2940
    Keywords: 2,4,6,8,10-Hexaoxa-1,3,5,7-tetraphosphatricyclo[3.3.1.1]decane 1-sulfide, molecular and crystal structure ; P4O6 derivatives ; Calculations, SCF, for P4O7 and P4O6S ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: P4O7 and P4O6S, Comparison of Molecular and Crystal StructureSingle crystals of P4O6S were grown for the first time. By X-ray diffraction the space group (P21/c), the unit cell [α = 813.5(1), b = 938.3(1), c = 993.1(1) pm; β = 90.27(1)°], and the crystal and molecular structure have been determined. As compared to P4O7, the geometry of the P4O6 cage remains virtually unchanged upon substitution of the terminal oxygen atom by a sulfur atom. Calculated charge distributions clearly confirm the experimental results. With the exception of P(1), to which the additional chalcogen atom is attached, the effective charges at all other atoms seem not to be affected by an exchange of the terminal oxygen atom by a sulfur atom.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240807
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  • 4
    Electronic Resource
    Electronic Resource
    Chirale dreilagige und kondensierte [2.2]Cyclophane Synthese, Struktur, Chiroptik (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 169-176 
    Details
    ISSN: 0009-2940
    Keywords: Caesium effect / Chiroptical properties / Circular dichroism / Cyclophanes, multilayered ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chiral Triple-Layered and Condensed [2.2]Cyclophanes - Synthesis, Structure, Chiroptical PropertiesThe helical title compounds 1-5 are obtained using a simple one-step cyclisation reaction with yields reaching or increasing those obtained by application of organometallic methods in [2.2]phane syntheses. The formation of the triple-layered phanes 1 leads with high selectivity only to the “up-down” isomers with fixed conformation, as shown by X-ray crystallography and by the detection of strong NOEs of the inner hydrogen atoms. For studies on structure-chiroptic relation-ships a systematic sequence of helical [2.2]phanes with larger arene systems is synthesized. Enrichment of enantiomers is achieved by HPLC on (+)-PTrMA; the kinetics of racemisation and the CD spectra are discussed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901230129
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  • 5
    Electronic Resource
    Electronic Resource
    Nitro- und Allyloxy-substituierte helicale [2.2]Metacyclophane: Synthese, Circulardichroismus und Röntgen-Kristallstrukturanalysen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1585-1590 
    Details
    ISSN: 0009-2940
    Keywords: Charge transfer ; Circular dichroism ; Helical molecules ; [2.2]Metacyclophanes ; Structure-chiroptic relationships ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Nitro- and Allyloxy-Substituted Helical [2.2]Metacyclophanes: Synthesis, Circular Dichroism and Crystal StructuresThe preparations of the title compound 3a, intraannularly nitro-functionalized, of the extraannularly substituted reference compound 3b, and of the sulfone 4 are described. Enantiomeric resolution of these helical phanes was accomplished on (+)-PTrMA and cellulose tris(3,5-dimethylphenyl)carbamate by HPLC. Racemization of the enantiomers of 3b is faster than that of the previously reported extraannularly substituted phanes. The crystal structure of 3a as well as that of the allyl ether 3d show severe distortions of the benzene rings; the CD spectrum of 3a is pointing at an intramolecular charge-transfer complex, an effect that cannot be evaluated from the CD spectrum of 3b.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240719
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  • 6
    Electronic Resource
    Electronic Resource
    Zur Existenz des Hexahydroxoperiodonium-Ions  -  Kristallzüchtung und Strukturanalyse von α- und β-H6IO6HSO4Herrn Professor Otto J. Scherer zum 60. Geburtstag gewidmet. (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 2415-2419 
    Details
    ISSN: 0009-2940
    Keywords: Periodic acid, protonation of ; Hexahydroxoiodine(VII) cation ; Hexahydroxoiodine(VII) hydrogensulfate, bimorphism of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: On the Existence of the Hexahydroxoiodine(VII) Cation - Crystal Growth and Structure Analysis of α- and β-H6IO6HSO4*Periodic acid H5IO6 dissolves at 50°C in 90-97% H2SO4 to give the hexahydroxoiodine(VII) cation H6IO6+. Depending on the concentration of the sulfuric acid, two modifications of H6IO6HSO4 can selectively and reproducibly be precipitated. The crystal structures determinations prove the existence of H6IO6+ in the solid state. The crystal structures and Raman spectra of α-H6IO6HSO4 (1a) and β-H6IO6HSO4 (1b) are discussed and compared. The temperature-dependent behaviour of 1a and 1b is studied by means of DTA, temperature-dependent X-ray powder diffraction, and Raman spectroscopy.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931261112
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  • 7
    Electronic Resource
    Electronic Resource
    Ein einfacher Weg zu Silicium in oktaedrischer Sauerstoffkoordination (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 1213-1218 
    Details
    ISSN: 0009-2940
    Keywords: Silicon ; Octahedral oxygen coordination ; Phosphorus ; NMR, 1H MAS ; NMR, 29Si MAS ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A Simple Route to Silicon in Octahedral Oxygen CoordinationSyntheses and crystal structures of three new compounds Rb2SiP4O13 (1), Cs2H2Si(P2O7)2 (2), and BaH2Si(P2O7)2 (3) containing silicon in an octahedral oxygen coordination are reported. The structures have been determined by X-ray structure analyses. All three compounds are constituted of silicophosphate polyanions. The NMR chemical shifts of silicon and hydrogen are measured.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941270706
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  • 8
    Electronic Resource
    Electronic Resource
    Verbesserte Darstellung, Kristallzüchtung und Strukturanalyse von P4O6S2 und P4O6S3Professor Hartmut Bärninghausen zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 281-286 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphosphorus hexaoxide disulfide and trisulfide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Improved Syntheses, Crystal Growth, and Crystal Structure Determination of P4O6S2 and P4O6S3Syntheses and single crystal growths of the title compounds are described. Both compounds crystallize in the space group P21/c (P4O6S2: a = 11.293(4); b = 6.457(3); c = 11.588(4) Å; β = 90.29(2)°, 2 450 diffractometer data, Rw = 0.035/P4O6S3: a = 15.611(5); b = 8,303(3); c = 9.697(4) Å; β = 127.12(2)°, 2 481 diffractometer data, Rw = 0.034). The structural data for the series P4O6Sn (n = 1 - 4) thus completed are compared to their oxide analogues P4O6On (n = 1 - 4). The changes in the geometry of the P4O6-cage in course of its successive oxidation are discussed.
    Notes: Darstellung und Einkristallzucht der Titelverbindungen werden beschrieben. Beide Verbindungen kristallisieren in der Raumgruppe P21/c (P4O6S2: a = 11,293(4); b = 6,457(3); c = 11,588(4) Å; β = 90,29(2)°, 2 450 Diffraktometerdaten, Rw = 0,035/P4O6S3: a = 15,611(5); b = 8,303(3); c = 9.697(4) Å; β = 127,12(2)°, 2 481 Diffraktometerdaten, Rw = 0,034). Durch die neu gelösten Strukturen werden die Daten für das System P4O6Sn (n = 1 - 4) komplettiert und können mit denen der analog aufgebauten Oxide P4O6On (n = 1 - 4) verglichen werden. Die Veränderungen der Molekülgeometrie des zentralen P4O6-Käfigs im Zuge der schrittweisen Oxidation werden diskutiert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190210
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  • 9
    Electronic Resource
    Electronic Resource
    Modifizierte Darstellung und Kristallstrukturbestimmung von β-Na2CS3Professor Dietrich Mootz zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1203-1208 
    Details
    ISSN: 0044-2313
    Keywords: β-Sodium thiocarbonate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Modified Synthesis and Crystal Structure Determination of β-Na2CS3.β-Na2CS3 has been synthesized via a novel route from Na2S and CS2, and its crystal structure has been determined using single crystal techniques (for crystallographic informations see “Inhaltsübersicht”). Structural relations between Li2CO3 and β-Na2CS3 are discussed. The ionic conductivities are 3 · 10-11S cm-1 and 1.3 · 10-2S cm-1 at 50°C and 250°C, respectively.
    Notes: In der Literatur als β-Na2CS3 beschriebenes Natriumthiocarbonat wurde auf einem neuen Wege aus Na2S und CS2 dargestellt und die Kristallstruktur aufgeklärt (C2/c; a = 1 003,6(1) pm, b = 633,7(1) pm, c = 855,5(1) pm, β = 108,05(1)°, Z = 4,1582 unabhängige Reflexe, R = 0,034). Strukturbeziehungen zu Li2CO3 werden diskutiert. Die Ionenleitfähigkeiten betragen 3 · 10-11S cm-1 und 1,3 · 10-2S cm-1 bei 50°C bzw. 250°C.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190709
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  • 10
    Electronic Resource
    Electronic Resource
    Zur Existenz des Tetrahydrogenorthoperiodations Die Kristallstruktur von LiH4IO6 · H2O (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 805-808 
    Details
    ISSN: 0044-2313
    Keywords: Lithiumtetrahydrogenorthoperiodate monohydrate ; crystal structure ; tetrahydrogenorthoperiodate Ion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Existence of the Tetrahydrogenorthoperiodate Ion. The Crystal Structure of LiH4IO6 · H2OThe crystal structure of LiH4IO6 · H2O has been determined (P1; a = 564.74(12), b = 574.41(13), c = 970.4(6) pm, α = 101.37(2), β = 96.37(2), γ = 114.72(2)°; Z = 2; 5 731 independent reflections; R = 0.038). All hydrogen-atoms were localized from difference fourier map and refined without applying constraints. Thus the existence of the tetrahydrogenorthoperiodate-ion in the solid state is proved, unambigously. The crystal structure is discussed and compared to other alkaliorthoperiodates.
    Notes: Die Kristallstruktur von LiH4IO6 · H2O wurde bestimmt (P1; a = 564,74(12), b = 574,41(13), c = 970,4(6) pm, α = 101,37(2), β = 96,37(2), γ = 114,72(2)°; Z = 2; 5 731 unabhängige Reflexe, R = 0,038). Alle Wasserstofflagen konnten aufgefunden und frei verfeinert werden und beweisen erstmals die Existenz des Tetrahydrogenorthoperiodations im Festkörper. Die Kristallstruktur wird diskutiert und mit denjenigen anderer Alkaliorthoperiodate verglichen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200508
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