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  • Articles  (27)
  • Inorganic Chemistry  (21)
  • Physical Chemistry  (6)
  • Gas chromatography
  • Wiley-Blackwell  (27)
  • 1975-1979  (27)
  • 1975  (27)
  • 1
    Electronic Resource
    Electronic Resource
    Crystal chemistry and synthesis of Ternary Silicates and Germanates containing alkali (Na+, K+) and alkaline earth (Ca2+, Sr2+, Ba2+) cations (1975)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 411 (1975), S. 163-172 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallchemie der ternären Silicate und Germanate mit Alkali (Na+, K+)- und Erdalkali (Ca2+, Sr2+, Ba2+)-KationenDie Darstellung von neuen ternären Silicat- und Germanat-Phasen mit großen Alkali- und Erdalkalikationen wird beschrieben. Sie wurden durch Festkörperreaktion von Mischungen der Carbonate bzw. Oxalate mit SiO2 bzw. GeO2 oder durch Schmelzen und anschließende Rekristallisation des Glases erhalten.Vertreter der kubischen M4+M2+X3O9-Familie sind Na4CaSi3O9 und die isostrukturellen Verbindungen K4CaGe3O9, K4SrGe3O9, K4CaSi3O9 und K4SrSi3O9. K4BaSi3O9 ist pseudokubisch; die Symmetrie des Na4SrSi3O9 ist unbekannt. Zur rhomboedrischen M8+M2+X10O25-Familie gehören K8CaSi10O25, K8SrSi10O25 und K8BaSi10O25.Na2CaGe2O6 und Na2SrGe2O6 sind isostrukturell, aber strukturell nicht mit Na2BaSi2O6 verwandt. Na2Ba2Ge2O7 und Na2Ba2Si2O7 sind strukturell ähnlich.
    Notes: The synthesis of new ternary silicate and germanate phases containing large alkali and alkaline-earth cations is described. They are made by solid-state reaction of mixtures of carbonates or oxalates with SiO2 or GeO2, or by fusion and subsequent recrystallization of the glass.Representatives of the cubic M4+M2+X3O9 family include Na4CaSi3O9 and the isostructural compounds K4CaGe3O9, K4SrGe3O9 and K4SrSi3O9. K4BaSi3O9 is pseudocubic: the symmetry of Na4SrSi3O9 is unknown. The rhombohedral M8+M2+X10O25 family includes K8CaSi10O25, K8SrSi10O25 and K8BaSi10O25.Na2CaGe2O6 and Na2SrGe2O6 are isostructural but both are structurally unrelated to Na2BaSi2O6. Na2Ba2Ge2O7 and Na2Ba2Si2O7 are structurally similar.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19754110211
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  • 2
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    Electronic Resource
    Abfangreaktionen kurzlebiger Radikale, XII Über die radikalische substitution am Schwefel: Induzierter Zerfall von (Thio)Carbonyldisulfiden (1975)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 1339-1345 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Short-Life Radicals, XII. Free Radical Substitution at the Sulfur Atom: The Induced Degradation of (Thio)Carbonyl DisulfidesDibenzoyl, diacetyl, bis(thiobenzoyl) disulfide (1, 2, 7), and benzoyl 4-tolyl disulfide (11) are degradated by hydrides R3SnH at 60°C about 103 times faster than in the spontaneous degradation. The products and following reactions have been established. In all cases, SH2 mechanisms are found, with attack of stannyl radicals at the (acyl bound) sulfur atom. In the case of 1, 2 and 11, ΔHspont.≠ is 35 or 34 ± 2 kcal/mole at 150°C.
    Notes: Dibenzoyl-, Diacetyl-, Bis(thiobenzoyl)disulfid (1, 2, 7) und Benzoyl(4-tolyl)disulfid (11) werden durch Hydride R3SnH bei 60°C im Verhältnis zum Spontanzerfall etwa um den Faktor 103 rascher abgebaut. Produkte und Folgereaktionen werden sichergestellt. Es liegen jeweils SH2-Mechanismen mit Angriff von Stannyl-Radikalen am (acylseitigen) Schwefel vor. Bei 1, 2 und 11 ist ΔH spont.≠ = 35 bzw. 34 ± 2 kcal/mol bei 150°C.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19751080439
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  • 3
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    Electronic Resource
    Abfangreaktionen kurzlebiger Radikale, XIV Zur Kinetik der SH2-Reaktion am Schwefel (1975)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 1355-1363 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Short-Life Radicals, XIV. Kinetics of the SH2 Reaction at the Sulfur AtomThe kinetics of the radical chain reactions of dibenzoyl (1), diacetyl (2), benzoyl-4-tolyl (3), and tetramethylthiuram disulfide (4), resp., with R′3SnH have been determined. In the case of 1 (90°C), both reactions, RS + R′3SnH →Ka RSH + R′3Sn; and R′3Sn + RSSR →Kb R′3SnSR + RS; are rate determining, v = 2.0 · 10-4 [RSSR]1[R′3SnH]1/2. The spontaneous splitting RSSR → 2RS is chain generating (its degree at 60°C is estimated), the hetero recombination RS + R′3Sn → R′3SnSR is the main termination step. The effect of the initiator AIBN has been measured (60°C), v = 4.6 · 10-4 [AIBN]1/2[RSSR]1/2[R′3SnH]1/2. ka = kb = 9 · 103 liters/mole·s. In the case of 2-4, similar behaviour has been found.  -  For dibenzoyl peroxide, ka (≈kb) = 6 · 104 liters/mole·s has been calculated at 50°C.
    Notes: Die Kinetik der Radikalketten-Reaktionen von Dibenzoyl- (1), Diacetyl- (2), Benzoyl-4-tolyl- (3) bzw. Tetramethylthiuram-disulfid (4) mit R′3SnH wird bestimmt. Bei 1 (90°C) sind die beiden Reaktionen RS + R′3SnH →Ka RSH + R′3Sn und R′3Sn + RSSR →Kb R′3SnSR + RS geschwindigkeitsbestimmend, v = 2.0 · 10-4 [RSSR]1[R′3SnH]1/2. Kettenstart ist der Spontanzerfall RSSR → 2RS (sein Ausmaß bei 60°C wird abgeschätzt), wichtigster Kettenabbruch die Hetero-Rekombination RS + R′3Sn → R′3SnSR. Der Einfluß des Starters AIBN wird gemessen, v = 4.6 · 10-4 [AIBN]1/2[RSSR]1/2[R′3SnH]1/2 (60°C). ka = kb = 9 · 103 Liter/mole·s. Für 2-4 sind die Verhältnisse analog.  -  Bei Dibenzoylperoxid ist ka (≈kb) = 6 · 104 Liter/mol·s bei 50°C.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19751080441
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  • 4
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    Elektrochemische Synthesen, III. Elektrosynthesen mit Isobutyraldehyd (1975)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 3292-3302 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Electrochemical Syntheses, III. Electrosyntheses with IsobutyraldehydeElectrochemically induced catalytic trimerisations of isobutyraldehyde are observed upon electrolysis in aprotic media. Anodically 2,4,6-triisopropyl-1,3,5-trioxane (1) is produced, whilst cathodically two configurational isomeres of 2,6-diisopropyl-5,5-dimethyl-1,3-dioxane-4-ol (2) are formed, their relative amounts depending on the nature of the electrolyte. 2,4,6-Triisopropyl-1,3,5-triazine (4) along with some 2,4-diisopropyl-1,3,5-triazine (5) is obtained by the oxidation of isobutyraldehyde in ammonia-saturated methanol. The addition of formamide to the electrolyte increases the yield of 5. Only 4 is produced in ammonia-saturated acetonitrile. The formation of 4 and 5 is assumed to proceed by way of the cyclisation of imidoesters as primary oxidation products in methanol solution and by the electro-oxidation of 2,4,6-triisopropylhexahydro-1,3,5-triazine (3) in acetonitrile solution.
    Notes: Elektrochemisch induzierte katalytische Trimerisierungen von Isobutyraldehyd werden bei der Elektrolyse in aprotischen Medien beobachtet. Anodisch entsteht 2,4,6-Triisopropyl-1,3,5-trioxan (1), kathodisch zwei Konfigurationsisomere von 2,6-Diisopropyl-5,5-dimethyl-1,3-dioxan-4-ol (2), deren Verhältnis von der Art des Elektrolytsystems abhängt. In ammoniakalischem Methanol entsteht bei der Oxidation von Isobutyraldehyd neben 2,4,6-Triisopropyl-1,3,5-triazin (4) 2,4-Diisopropyl-1,3,5-triazin (5). Der Zusatz von Formamid zum Elektrolyten erhöht den Anteil an 5. In ammoniakalischem Acetonitril entsteht nur 4. Als Mechanismus wird in Methanol eine Cyclisierung von primär gebildeten Imidoestern, in Acetonitril die Elektrooxidation von 2,4,6-Triisopropylhexahydro-1,3,5-triazin (3) angenommen.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19751081020
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  • 5
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    Electronic Resource
    Abfangreaktionen kurzlebiger Radikale, XIII Über die radikalische Substitution am Schwefel: Thioverbindungen mit zwei verschiedenen reaktiven Heteroatomen (1975)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 1346-1354 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Short-Life Radicals, XIII. Free Radical Substitution at the Sulfur Atom: Thio Compounds Having Two Different Reactive Hetero AtomsTetramethylthiuram disulfide (1), „dixanthogene“ (6), trithioperoxycarbonic acid O-ethyl ester-SS-p-tolyl ester (8) (ΔHspont.≠ = 32 ± 2 kcal/mol) and tuluenesulfenic acid ethyl ester (12) are degradated in a radical way by hydrides R3SnH, working very quickly compared with the spontaneous degradation. Products and following reactions have been established. The only or main primary reaction is the attack of stannyl radicals at the (acyl bound) sulfur atom (SH2 reaction). They do not react with N in 1 or O in 12, but react with O in 8 and, rather strongly, in the O-ethyl S-stannyl dithiocarbonate 5, intermediate from 6 and 8, giving fragmentation.
    Notes: Tetramethylthiuramdisulfid (1), „Dixanthogen“ (6), Trithioperoxykohlensäure-O-äthylester-SS-p-tolylester (8) (ΔHspont.≠ = 32 ± 2 kcal/mol) und Toluolsulfensäure-äthylester (12) werden von Hydriden R3SnH radikalisch abgebaut, sehr schnell im Vergleich zum Spontanzerfall. Produkte und Folgereaktionen werden sichergestellt. Primärreaktion ist hauptsächlich oder alleinig der Angriff von Stannyl-Radikalen am (acylseitigen) Schwefel (SH2-Reaktion). Diese reagieren nicht mit N in 1 und O in 12, offenbar aber mit O in 8 und insbesondere im Dithiokohlensäure-O-äthylester-S-stannylester 5, Zwischenprodukt aus 6 und 8, unter Fragmentierung.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19751080440
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  • 6
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    Kinetics and mechanisms of substitution reactions with sulfur-containing nucleophiles in aqueous acid solutions. I - rates of reactions of some tetrahalopalladate (II) anions with thiourea and selenourea (1975)
    New York, NY : Wiley-Blackwell
    International Journal of Chemical Kinetics 7 (1975), S. 87-98 
    Details
    ISSN: 0538-8066
    Keywords: Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The activation energy parameters for the reaction of PdX42- (X=Cl-, Br-) in aqueous halide acid solution with thiourea (tu) and selenourea (seu) have been determined. High rates of reaction parallel low enthalpies and appreciable negative entropy of activation. The rate law in each case simplifies to kobs=k[L] where L=tu or seu, and only ligand-dependent rate constants are observed at 25°C. The ligand-dependent rate constants for the first identifiable step in the PdCl42- + X system is (9.1±0.1) × 103 M-1 sec-1 and (4.5±0.1) × 104 M-1 sec-1 for X=tu and seu, respectively, while for the PdBr42- + X system it is (2.0±0.1) × 104 M-1 sec-1 and (9.0±0.1) × 104 M-1 sec-1 for X=tu and seu, respectively.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/kin.550070110
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  • 7
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    On the fast addition reactions of BH3 (1975)
    New York, NY : Wiley-Blackwell
    International Journal of Chemical Kinetics 7 (1975), S. 633-636 
    Details
    ISSN: 0538-8066
    Keywords: Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/kin.550070412
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  • 8
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    N. Methyl-N-diäthoxyphosphorylamido-Derivate des Hexachlorocyclotriphosphazatriens. I. Die Reaktion von Hexachlorocyclotriphosphazatrien mit dem Natriumsalz des N-Methylamidophosphorsäurediäthylesters (1975)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 415 (1975), S. 51-56 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N-Methyl-N-Diethoxyphosphorylamido Derivatives of Hexachlorocyclotriphosphazatriene. I. The Reaction of Hexachlorocyclotriphosphazatriene with Sodium N-Methylamidophosphoric Acid Diethyl Ester.The reaction of hexachlorocyclotriphosphazatriene with the sodium salt of 0, 0-diethyl-N-methylamido-phosphate in the molar ratios 1:1, 1:2, and 1:3 gives a mixture of partially substituted compounds. The N-methyl-N-diethoxyphosphorylamidoderivatives, N3P3Cl6-n[NCH3P(O)(OC2H5)]n (n = 1, 2, 3) were isolated in a pure form by preparative column chromatography. Compounds with a higher degree of substitution are not formed. The compounds are characterized by their molecular weights, elementary analysis, and TLC-Rf values.
    Notes: Die Reaktion von Hexachlorocyclotriphosphazatrien mit dem Natriumsalz des N-Methylamidophosphorsäurediäthylesters führt bei Raumtemperatur in den Molverhältnissen 1:1, 1:2 und 1:3 zu einem Gemisch partiell substituierter Verbindungen. Mit Hilfe der präparativen Säulenchromatographie konnten die N-Methyl-N-diäthoxyphosphorylamido-Derivate, N3P3Cl6-n[NCH3P(O)(OC2H5)2]n (n = 1, 2, 3); in reiner Form isoliert werden. Verbindungen höheren Substitutionsgrades wurden nicht erhalten. Die Verbindungen wurden durch ihre Molmassen, Elementaranalysen und die dünnschichtchromatographischen Rf-Werte charakterisiert und gesichert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19754150108
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  • 9
    Electronic Resource
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    The thermal expansion and high temperature transformation of GeSe (1975)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 411 (1975), S. 90-96 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die thermische Ausdehnung und die Hochtemperaturumwandlung des GeSeDie thermische Ausdehnung des GeSe wurde röntgenographisch mittels einer 190 mm Unicam Hochtemperaturkamera von Zimmertemperatur bis zum Schmelzpunkt von 670 ± 5°C untersucht. Die thermische Ausdehnung der kristallographischen Achsen ist linear mit einer betonten Änderung der Ausdehnungskoeffizienten aller Achsen oberhalb 400°C. Die relativen Änderungen der Achsen deuten an, daß sich die Struktur mit zunehmender Temperatur kubischer Symmetrie nähert. Die Umwandlung des GeSe von der rhombischen zur NaCl-Struktur erfolgt bei einer Temperatur von 651 ± 5°C. Die Gitterkonstante des kubischen GeSe ist a0 = 5,730 ± 0,003 Å bei der Temperatur 656°C. Die kubische Modifikation des GeSe ist bis zum Schmelzpunkt stabil.
    Notes: The thermal expansion of GeSe has been studied above room temperature up to the melting point of 670 ± 5°C by X-ray diffraction techniques using a 190 mm Unicam high temperature camera. The thermal expansion of the crystallographic axes is linear with a distinct change of the expansion coeffients for all axes above 400°C. The relative changes of the axes indicate a rearrangement of the structure towards cubic symmetry with increasing temperature. The transformation of GeSe from the orthorhombic to a normal NaCl-type structure is observed at 651 ± 5°C. The lattice parameter of the cubic form of GeSe is a0 = 5.730 ± 0.003 Å at 656°C. The GeSe lattice remains cubic up to the melting point.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19754110110
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  • 10
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    Electronic Resource
    N-Methyl-N-Diäthoxyphosphorylamideo-Dervite des Hexachlorocyclotriphosphazatriens. II. Die Ammonolyse der N-Methyl-N-deäthoxyphosphorylamido-chlorcocyclotriphosphazatriene (1975)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 416 (1975), S. 169-173 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N-Methyl-N-Diethoxyphosphorylamido Derivatives of Hexachlorocyclotriphosphazatriene. II. Ammonoloyses of N-Methyl-N-Diethoxyphosphorylamido-ChlorocyclotriphosphazatrienesMonokis-[N-methyl-N-diethroxyphosphorylamido]-pentachloro-cyclotriphospha-zatriene and 2, 4-bis-[N-methyl-N-diethoxyphosphorylamido]-2, 4, 6, 6-tetrachloro-cyclotriphosphazatriene react with gaseous ammonia at room temperature to the corresponding diamino compounds, N3P3CL4-n[NCH3P(O)(OC2H5)2]n(NH2)2, (n = 1, 2). Total Exchange of the chlorine in the N-Methyl-Ndiethoxyphosphorylamido-derivatives, N3P3CL6-n[NCH3P(O)(OC2H5)2]n, (n = a, 2, 3), takes place during the reaction with liquid ammonia. Aminophosphazenes of the type N3P3[NCH3P(O)(OC2H5)2]n(NH2)6-n, (n = 1, 2, 3), are formed. The described aminocyclotriphosphazatrienes are characterized by their melting points, elementary analyses, molecular weights and the TLC-Rf-values.
    Notes: Monokis-[N-methyl-N-diäthoxyphorylamido]-pentachloro-cyclotriphosphazatrien und 2, 4-Bis-[N-methyl-N-diäthoxyphosphorylamido]-2,4,6,6-tetrachlorocyclotriphosphazatrien reagieren mit gasförmigem Ammoniak bei Raumtemperatur zu den entsprechenden diaminoverbindungen, N3P3CL4-n[NCH3P(O)(OC2H5)2]n(NH2)2, (n = 1, 2). Vollständiger Austausch des Chlors in den N-Methyl-N-diäthoxyphosphorylamido-Derivaten, S3P3CL6-n[NCH3P(O). (OC2H5)2]n, (n = 1, 2, 3). findet bei der Umsetzung mit flüssigem ammonial Statt. Es werden dabei Aminocyclophosphazene des Typs N3P[NCH33P(O)(OC2H5)2]n(NH2)6-n, (n = 1. 2. 3) gebildet, Die beschriebenen Aminocyclophosphazatriene werden durch ihre Schmelzpunkte, Elementaranalysen, Molmassen und die dünnschichtchromatographischen Rf-Werte charakterisiert.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19754160208
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