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  • 1985-1989  (11)
  • 1980-1984  (6)
  • 1910-1914  (1)
  • Chemistry  (18)
  • Inorganic Chemistry  (15)
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  • 1
    ISSN: 0009-286X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Additional Material: 2 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 12 (1988), S. 407-411 
    ISSN: 0142-2421
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The capability of optical measurements to elucidate adsorption as well as absorption phenomena is demonstrated by using oxygen interaction with copper films as an example. The films (thickness about 30 nm) deposited under UHV conditions on glass substrates show a polycrystalline structure with a marked (111) fibre texture. Gas doses were provided at 460 K while recording simultaneously the ellipsometric response (λ = 1152 nm) and the electrical resistivity. The optical properties of the clean films correspond to well-known bulk data. O2 adsorption causes the ellipsometric angles σΔ and σψ to change by 0.05° and 0.02°, respectively. At pressures of about 1 Pa oxygen begins to penetrate into the interior of the sample which manifests itself in a further drastic increase of σΔ = 30° and σψ = 5°.
    Additional Material: 6 Ill.
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  • 3
    ISSN: 0323-7648
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Basing on recent results of modelling discontinuous and continuous emulsion polymerization processes a mathematical model of the emulsion polymerization of butadiene with styrene is established. Partially the model can be applied to large-scale plants. Generally, however, its application requires particular adaption to large-scale conditions. Based on the kinetic concept a method for the continuous determination of the degree of activation at the inlet of the stirring vessel cascade is described.
    Notes: Ausgehend vom gegenwärtigen Stand der Modellierung von Emulsionspolymerisationen bei diskontinuierlicher und kontinuierlicher Prozeßführung wurde ein mathematisches Modell zur Anwendung bei der Butadien-Styren-Emulsions-polymerisation entwickelt. Es kann gezeigt werden, daß Teile des kinetischen Modells auf die technische Anlage übertragbar sind, generell aber zur Anpassung großtechnische Untersuchungen notwendig sind. Weiterhin wird aus den kinetischen Vorstellungen eine Methode zur kontinuierlichen Bestimmung des Aktivierungsgrades am Eingang der Rührkesselkaskade entwickelt und dargelegt.
    Additional Material: 10 Ill.
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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: Transition Metal Peroxofluoro Complexes. VIII. Crystal Structure of K2Ti(O2)F4. · 1/2H2O. Structural Comparison and Spectroscopic Data of the Compounds K2Ti(O)2F4 · xH2O (x = 1, 1/2, 0)The yellow hemihydrat K2Ti(O2)F4 · 1/2 H2O crystallizes monoclinic (space group C2/c, a = 1680.5(6), b = 653.2(1), c = 1224.3(4) pm, β = 115.8(1)°, Z = 8, Rw = 0.038 for 1113 independent reflections). It contains isolated, dinuclear, di(μ-fluoro)-bridged [Ti2(O2)2F8]4- anions, as known by orange coloured K2Ti(O2)F4 · H2O [1]. They are arranged in layers which are parallel to the (100) plane, whereas they are linked by hydrogen bonds forming infinite chains in K2Ti(O2)F4 · 1/2 H2O. Anhydrous K2Ti(O2)F4 - even yellow - crystallizes monoclinic with a = 828.9(2), b = 1107.6(2), c = 1303.9(3) pm, β = 92.29(2)°. I.r. and Raman spectra of all compounds are listed and interpreted. On the basis of the UV spectra the different colours of some titaniumperoxofluoro compounds are discussed in relation to the titanium-peroxid bonding.
    Notes: Das gelbe Hemihydrat K2Ti(O2)F4 · 1/2H2O kristallisiert monoklin (Raumgruppe C2/c, a = 1680,5(6), b = 653,2(1), c = 1224,3(4) pm, β = 115,8(1)°, Z = 8, Rw = 0,038 für 1113 unabhängige Reflexe). Es enthält isolierte, zweikernige, di(μ-fluoro)-verbrückte [Ti2(O2)2F8]4--Anionen, wie sie vom orangefarbenen K2Ti(O2)F4 · H2O her schon bekannt sind [1]. Während sie dort jedoch über Wasserstoffbrücken zu Ketten verknüpft sind, sind sie im K2Ti(O2)F4 · 1/2 H2O in Schichten parallel zur (100) Ebene angeordnet. Das ebenfalls gelbe wasserfreie K2Ti(O2)F4 kristallisiert monoklin mit den Gitterkonstanten a = 828,9(2), b = 1107,6(2), c = 1303,9(3) pm, β = 92,29(2)°.IR- und Raman-Spektren aller drei Verbindungen K2Ti(O2)F4 · xH2O (x = 0, 1/2, 1) werden aufgeführt und interpretiert. Auf der Grundlage der UV-Spektren werden die unterschiedlichen Farben verschiedener Titanperoxofluoroverbindungen im Zusammenhang mit ihren Bindungsverhältnissen diskutiert.
    Additional Material: 3 Ill.
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  • 5
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Acyl- and Alkylidenephosphines. XXX. Molecular and Crystal Structure of 1H-1,3-Benzazaphosphole1H-1,3-Benzazaphosphole synthesized by Issleib and coworkers [2], crystallizes in the orthorhombic space group Pna21 with following dimensions of the unit cell Determined at a temperature of measurement of -80 ± 3°C: a = 828.6(2); b = 557.1(1); c = 1433.5(4) pm; Z = 4. An X-ray Structure Determination (Rg = 0.061) shows the molecule to be characterized by a rather narrow C—P=C angle of 88.2(4)° as well as a shortened single {180.7(7)} and a typical double bond {169.5(9) pm} between the carbon atoms and the twofold coordinate phosphorus. All the other bond lengths differ only scarcely from corresponding values of the homologues benzimidazole 2a [3, 4] and 1H-1,3-benzazarsole 2c [5]. In spite of the fact that all three solids crystallize in the same space group, only the heterocycles 2b and 2c are isotypic; intermolecular hydrogen bonds as found in 2a, are no longer present in the heavier homologues.
    Notes: Das Von Issleib u. Mitarb. [2] dargestellte 1H-1,3-Benzazaphosphol 2b kristallisiert orthorhombisch in der Raumgruppe Pna21 mit folgenden, bei einer Meßtemperatur Von -80 ± 3°C bestimmten Abmessungen der Elementarzelle: a = 828,6(2); b = 557,1(1); c = 1433,5(4) pm; Z = 4. Nach den Ergebnissen einer Röntgenstrukturanalyse (Rg = 0,061) weist das Molekül bei einem C—P=C-Winkel Von nur 88,2(4)° eine auf 180,7(7) pm Verkürzte Einfach- und eine mit 169,5(9) pm typische Doppelbindung zwischen Den Kohlenstoffatomen und Dem zweifach koordinierten Phosphoratom auf. Die übrigen Bindungslängen weichen kaum Von Den für die Homologen Benzimidazol 2a [3, 4] und 1H-1,3-Benzazarsol 2c [5] publizierten Werten ab. Obwohl bei allen drei Kristallstrukturen die gleiche Raumgruppe auftritt, sind nur die Heterocyclen 2b und 2c zueinander isotyp; die für Verbindung 2a charakteristischen intermolekularen Wasserstoffbrücken bilden sich bei Den schwereren Homologen nicht mehr aus.
    Additional Material: 4 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 537 (1986), S. 175-188 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Peroxofluoro Complexes. VII. Peroxofluorokryolithes A3Ti(O2)F5 (A = K, Na) and K2NaTi(O2)F5. Crystal Structure of K3Ti(O2)F5Peroxofluorokryolithes A3Ti(O2)F5 (A = K, Na) and K2NaTi(O2)F5 were prepared at pH 4.5-6 by adding H2O2 and AOH/AF to solutions of TiO2 in hydrofluoric acid or aqueous solutions of TiF4. In the range of pH 3-4.5 exist phases of peroxofluoro-kryolithes with variations in stoichiometrie. A single crystall X-ray structure analysis of K3Ti(O2)F5 (Fm3m, a = 883.6(1) pm) yielded a disordered kryolithstructure (R = 0.020, RW = 0.017). Na3Ti(O2)F5 was found to crystallize in two monoclinic low-temperature - and one cubic high-temperature modifications. K2NaTi(O2)F5 crystallizes cubic (Fm3m) with a = 847.8(1) pm. Vibrational spectra have been measured and thermal behavior was studied by DTA/DTG and high-temperature guinier. At pH 9.5 K3Ti(O2)2F3 has been synthesized
    Notes: Peroxofluorokryolithe A3Ti(O2)F5 mit A = K, Na und K2NaTi(O2)F5 wurden aus flußsauren TiO2- oder wäßrigen TiF4-Lösungen, H2O2 und AOH/AF zwischen pH 4,5 und 6 hergestellt. Zwischen pH 3 und 4,5 existieren Peroxofluorokryolithphasen. Die Bestimmung der Kristallstruktur von K3Ti(O2)F5 (Fm3m, a = 883,6(1) pm) führte zu einem Kryolithfehlordnungsmodell, in dem auch die Alkaliionen statistisch fehlgeordnet sind (R = 0,020, RW = 0,017). Von Na3Ti(O2)F5 wurden zwei monokline Normaltemperatur- und eine kubische Hochtemperaturmodifikation aufgefunden. K2NaTi(O2)F5 kristallisiert kubisch (Fm3m) mit a = 847,8(1) pm. Die Schwingungsspektren wurden aufgenommen und das thermische Verhalten mittels DTA/DTG und Heizguinieraufnahmen untersucht. Bei pH 9,5 wurde die Verbindung K3Ti(O2)2F3 synthetisiert.
    Additional Material: 2 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 575 (1989), S. 197-201 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Peroxofluoro Complexes. IX. Crystal Structure of Ba3[Ti(O2)F5]2 · 2 H2OThe pale yellow hydrat Ba3[Ti(O2)F5]2 · 2 H2O crystallizes tetragonal (space group P42/mbc, a = 1 248.5(3), c = 812.2(2) pm; Z = 4; R = 0.026 for 404 independent reflections). It contains isolated [Ti(O2)F5]3- anions. Thermal decomposition leads directly to α-Ba3Ti2O2F10, which is isotypic to α-Ba3Al2F12.
    Notes: Das hellgelbe Hydrat Ba3[Ti(O2)F5]2 · 2 H2O kristallisiert tetragonal (Raumgruppe P42/mbc, a = 1 248,5(3), c = 812,2(2) pm; Z = 4; R = 0,026 für 404 unabhängige Reflexe) und enthält isolierte [Ti(O2)F5]3--Anionen. Die thermische Zersetzung führt direkt zum α-Ba3Ti2O2F10, das isotyp zum α-Ba3Al2F12 kristallisiert.
    Additional Material: 2 Ill.
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  • 8
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Peroxofluoro Complexes. VI. Preparation, Vibrational Spectra, and Crystal Structure of (NH4)3Zr(O2)F5. A New Disorder Model for Ammonium Peroxopentafluoro Metallates(IV) with Elpasolite Structure(NH4)3Zr(O2)F5 has been prepared from solution and characterized by the i.r. and raman spectra. The disordered crystal structure was determined: space group Fm3m, Z = 4, a = 944.01(8) pm, Rw = 0.014 for 162 reflections. A new disorder model - revised with respect to former proposals made for the isotypic Ti compound - allows now to derive unambiguously the geometry of the complex anions: d(O—O) = 157(1), d(Zr—O) = 206.3(9), d(Zr—F), average 203.8 pm. An analogous treatment of the disorder for (NH4)3Ti(O2)F5 also led to a significant improvement of the results (Rw = 0.019, d(O—O) = 151(2), d(Ti—O) = 197(1), d(Ti—F), average 191.6 pm).
    Notes: (NH4)3Zr(O2)F5 wurde aus Lösung dargestellt, IR- und Raman-spektroskopisch charakterisiert, und die fehlgeordnete Kristallstruktur bestimmt: Raumgruppe Fm3m, a = 944,01(8) pm, Z = 4, Rw = 0,014 für 162 Reflexe. Ein neues, gegenüber früheren Vorschlägen für die isotype Ti-Verbindung verbessertes Fehlordnungsmodell erlaubt nun die widerspruchsfreie Ableitung der Gestalt der komplexen Anionen: d(O—O) = 157(1), d(Zr—O) = 206,3(9), d(Zr—F) = 203,8 pm (gemittelt). Analoge Behandlung der Fehlordnung führte auch bei (NH4)3Ti(O2)F5 zu einer deutlichen Verbesserung früherer Resultate (Rw = 0,019, d(O—O) = 151(2), d(Ti—O) = 197(1), d(Ti—F) gemittelt 191,6 pm).
    Additional Material: 2 Ill.
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  • 9
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Trichloronitro Methane with Iron Carbonyls. Crystal Structure of (PPh4)2[Fe2OCl6] · 2 CH2Cl2Trichloronitro methane reacts with Fe2(CO)9 or Fe3(CO)12 forming NO[FeOCl2] which is composed of Nitrosyl ions and polymeric [FeOCl2]⊖. The reaction of NO[FeOCl2] with POCl3 affords Fe(O2PCl2)3; with tetraphenyl phosphoniumchloride it forms the complex (PPh4)2[Fe2OCl6] which is soluble in CH2Cl2. The oxochloro ferrates are characterized by the aid of 57Fe-Mössbauer spectra and by i.r. spectra.A single crystal of (PPh4)2[Fe2OCl6] · 2 CH2Cl2 was used to carry out a structural investigation by means of X-ray diffraction data (space group P1, Z = 1, a = 1157.2(2), b = 1363.8(3), c = 1140.3(2) pm, α = 109.22(1)°, β = 95.23(1)°, γ = 67.24(2)°, R = 0.052 for 3814 reflexions with F0 〉 3σ). The [Cl3Fe—O—FeCl3]2⊖-anion is found to have a centre of symmetry and thus, in accordance with the i.r. spectra, contains a linear bridge. High thermal parameters of the bridging oxygen atom and the chlorine ligands, however, allow interpretations as orientation disorder of slightly bent anions.
    Notes: Trichlornitromethan reagiert mit den Eisencarbonylen Fe2(CO)9 bzw. Fe3(CO)12 unter Bildung von NO[FeOCl2], das aus Nitrosylionen und polymerem [FeOCl2]⊖ aufgebaut ist. NO[FeOCl2] setzt sich mit POCl3 zu Fe(O2PCl2)3 um; mit Tetraphenylphosphoniumchlorid entsteht der in CH2Cl2 lösliche Komplex (PPh4)2[Fe2OCl6]. Die Oxochloroferrate werden mit Hilfe der 57Fe-Mößbauer-Spektren und der IR-Spektren charakterisiert.An einem Einkristall von (PPh4)2[Fe2OCl6] · 2 CH2Cl2 wurde eine Röntgen-Strukturanalyse durchgeführt (Raumgruppe P1, Z = 1, a = 1157,2(2), b = 1363,8(3), c = 1140,3(2) pm, α = 109,22(1)°, β = 95,23(1)°, γ = 67,24(2)°, R = 0,052 für 3814 Reflexe mit F0 〉 3σ). Danach besitzt das [Cl3Fe—O—FeCl3]2⊖-Anion ein Symmetriezentrum und ist somit  -  in Übereinstimmung mit den IR-Spektren  -  linear gebaut. Große thermische Schwingungsparameter des Brückensauerstoffatoms wie der Cl-Liganden lassen jedoch auch die Möglichkeit einer Orientierungsfehlordnung leicht gewinkelter Anionen zu.
    Additional Material: 4 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 520 (1985), S. 139-150 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Acyl- and Alkylidenephosphines. XXVII. Molecular and Crystal Structure of Methyl-[(N-phenyl, N-trimethylsilyl)thiocarbamoyl]trimethylsilylphosphine.Methyl[(N-phenyl, N-trimethylsilyl)thiocarbamoyl]trimethylsilylphosphine 1a formed via an addition of methylbis(trimethylsilyl)phosphine to phenyl isothiocyanate [1], crystallizes in the monoclinic centrosymmetric space group P21/n with following dimensions of the unit cell determined at a temperature of measurement of -80±3°C: a=1041.2(4);b=1706.9(12);c=1001.1(6)pm; β=106.41(4)°; Z = 4. An X-ray structure determination (Rw = 0.039) confirms the constitution of the compound as already derived from its nmr spectra. One trimethylsilyl group is bound to the phosphorus atom, whereas the other is connected with the sp2-hybridized nitrogen atom. Characteristic rounded bond lenghts and angles are: P—Si 231, P—CH3 184, P—C(S) 187, C=S 167, N—C(S) 137, and N—Si 181 pm as well as P—C—S 122°, P—C—N 117°, and S—C—N 121°.
    Notes: Das durch Addition von Methylbis (trimethylsilyl) phosphan an Phenylisothiocyanat gebildete [1] Methyl[N-phenyl, [N-trimethylsilyl] thiocarbamoyl thiocarbamoyl]trimethylsilylphosphan 1a kristallisiert monoklin in der zentrosymmetrischen Raumgruppe P21/n mit folgenden, bei einer Meßtemperatur von -80±3°C bestimmten Abmessungen der Elementarzelle: a=1041,2(4); b=1706,9(12); c=1001,1(6) pm; β-106,41(4)°; Z = 4. Die Röntgenstrukturanalyse (w = 0,039) bestätigt die bereits aus den NMR-Spektren abgeleitete Konstitution der Verbindung mit an Phosphor- und sp2-hybridisiertes Stickstoffatom gebundenen Trimethylsilyl-Gruppen. Charakteristische gerundete Bindungslängen und - winkel sind: P—Si 231, P—CH3 184, P—C(S) 187, C=S 167, N—C(S) 137 und N—Si 181pm sowie P—C—S 122°, P—C—N 117° und S—C—N 121°.
    Additional Material: 4 Ill.
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