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  • 1
    Electronic Resource
    Electronic Resource
    A method for measuring sedimentation and diffusion of macromolecules in capillary tubes by total intensity and quasi-elastic light-scattering techniquesPresented in part at the Symposium on New Generation Instrumentation in Rheology, Rheology Society, Cincinnati, Ohio, January 1973, by M. H. Birnboim. (1975)
    New York : Wiley-Blackwell
    Biopolymers 14 (1975), S. 419-430 
    Details
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Light scattered from a macromolecular solution in a capillary tube is used to determine both the sedimentation and translational diffusion coefficients. The capillary tube is spun in a preparative centrifuge, removed, and placed in a light-scattering photometer equipped with a scanning mechanism. The intensity distribution of scattered light along the tube represents the concentration profile in the tube and provides the measure of boundary migration. The sedimentation coefficient is determined from this measure and the applied centrifugal field. The diffusion coefficient is obtained from a time-autocorrelation analysis of fluctuations in intensity of light scattered from any fixed point of the profile. These coefficients were obtained for two monodisperse systems, R17 bacteriophage and 28s ribosomal rat liver RNA. The molecular weights obtained from ratios of these coefficients are in good agreement with literature values. In the sedimentation analysis, deviations from linearity between boundary displacement and applied field were found to be less than 1%. This precision confirms that the boundary is stable for the capillary geometry even in the absence of a preformed density gradient. The sedimentation coefficients of identical samples were also measured with the Spinco Model E analytical ultracentrifuge; results of the two methods agree to within 4%.As a consequence of the capillary tube geometry and light-scattering detection, sedimentation coefficients can be obtained from sample volumes of less than 100 μl. This detection techniques is thus far demonstrated to be at least an order of magnitude more sensitive than Schlieren optics, thereby useful when uv absorption is not applicable. For diffusion measurements there are also several inherent advantages. The diffusion coefficient is obtained from the identical sample, and scanning provides the capability to measure D from various parts of the sedimentation profiles and thereby directly explore concentration dependence, homogeneity, and integrity of the sample. The capillary tube with a layer of silicone oil over the sample and centrifugation provides an effective method to cleanse the solution and trap all dust.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bip.1975.360140214
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  • 2
    Electronic Resource
    Electronic Resource
    Di- und Polyaminozucker, XXI. Synthese von Derivaten der 2,4-Diamino-2,3,4-tridesoxy-D-ribo-hexose (1975)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 3397-3411 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Di-and Polyamino Sugars, XXI. Synthesis of Derivatives of 2,4-Diamino-2,3,4-trideoxy-D-ribo-hexoseStarting with D-glucose the title compound has been synthesized as its di-N-acetyl. -trifluoroacetyl and N,N′-bis(2,4-dinitrophenyl) derivative. The free sugar could not be obtained in a pure state.
    Notes: Die Titelverbindung wurde, ausgehend von D-Glucose, in Form ihres Di-N-acetyl-, -trifluoracetyl- und ihres N,N′-Bis(2,4-dinitrophenyl)-Derivates erhalten. Reindarstellung des freien Zuckers gelang nicht.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19751081031
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  • 3
    Electronic Resource
    Electronic Resource
    Heterocyclische Siebenring-Verbindungen, XVI. Synthese gezielt 3,5-substituierter 4-Phenyl-1-benzothiepine (1975)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 3596-3610 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Heterocyclic Seven-membered Ring Compounds, XVI. Synthesis of 3,5-Substituted 4-Phenyl-1-benzothiepins4-Phenyl-1-benzothiepins 7 and 8 are synthesized starting from their 5-methoxy-2,3-dihydro-precursor 2; using the 2,5-dihydro-intermediate 12 yields the 4-phenyl-1-benzothiepins 13 and 14. The 1-benzothiepin 17 can be obtained from the diketone 1 directly. The 3-cyano-substituted compound 22 is prepared from its 2,5-dihydro-precursor 21. Some ring-contraction and ring-cleavage reactions of the heterocyclic seven-membered ring-system are described.
    Notes: Die 5-Methoxy-2,3-dihydro-Vorstufe 2 wird in die 4-Phenyl-1-benzothiepine 7 und 8 übergeführt; aus der 2,5-Dihydro-Vorstufe 12 werden die 4-Phenyl-1-benzothiepine 13 und 14 dargestellt. Das 1-Benzothiepin 17 wird direkt aus dem Siebenring-Diketon 1 erhalten. Das 3-cyan-substituierte 1-Benzothiepin 22 erhält man aus der 2,5-Dihydro-Vorstufe 21. Es werden einige Ringverengungsbzw. Ringspaltungsreaktionen des heterocyclischen Siebenring-Systems beschrieben.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19751081121
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  • 4
    Electronic Resource
    Electronic Resource
    Eine moderne Strömungsapparatur für kinetische Messungen an thermischen Umlagerungen in der Gasphase: Thermolysekinetik neuer Kleinringverbindungen (1977)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 2545-2560 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Modern Flow Reactor for Kinetic Measurements of Gasphase Thermal Rearrangements: Thermolysis Kinetics of Some New Small Ring CompoundsAn apparatus with a laminar flow reactor is introduced, which serves for kinetic measurements in the gas phase using rather small amounts (5-10mg) of compounds. Test runs for the well studied vinylcyclopropane rearrangement and the retro-Diels-Alder reaction of dicyclopentadiene demonstrate the reliability of the results thus obtained.  -  The thermolytic rearrangements of the following compounds were studied with this device: diademane (1), dispiro[2.0.2.4]deca-7,9-diene (3) including the formation of o-ethylstyrene (4) and tetrahydronaphthalene 5, 3,3,4,4-tetramethyl-1,5-hexadiene (6), 1,4-bis(cyclopropylidene)butane (8), dispiro[cyclopropane-1,2′-bicyclo[2.2.0]hexane-3′,1″-cyclopropane] (10), 2,2,3,3-tetramethylbicyclo[2.2.0]hexane (11) and 2,2-dimethylbicyclo[2.2.0]hexane-3-spirocyclopropane (12). All these reactions followed first order rate laws with the following Arrhenius relationships: ln(k1) = 33.6 - 31600/RT, ln(k3) = 34.2 - 35500/RT, ln(k4) = 33.6 - 35100/RT, ln(k5) = 33.6 - 36000/RT, ln(k6) = 29.1 - 33300/RT, ln(k8) = 22.0 - 26200/RT, ln(k10) = 32.0 - 35200/RT, ln(k11) = 32.0 - 40900/RT, ln(k12) = 32.3 - 39400/RT. The kinetic isotope effects of 1.4 and 1.1 (at 175°C) for the formation of 4 and 5 respectively and the difference Ea4 - Ea5 ≈ 0.1-0.9 kcal/mol strongly favor a mechanism, by which 3 rearranges via a 1,6-diradical to yield 4 and 5 by intramolecular disproportionation and recombination, respectively.
    Notes: Für kinetische Messungen in der Gasphase wird eine Apparatur mit laminarem Strömungsreaktor vorgestellt, die mit sehr geringen Substanzmengen (5-10mg) auskommt. Testmessungen an der eingehend untersuchten Vinylcyclopropanumlagerung und der Retro-Diels-Alder-Reaktion des Dicyclopentadiens beweisen die Verläßlichkeit der gewonnenen Daten.  -  Mit der Apparatur wurden die Thermolysen von Diademan (1), Dispiro[2.0.2.4]deca-7,9-dien (3) einschließlich Bildung von o-Ethylstyrol (4) und Tetrahydronaphthalin (5), 3,3,4,4-Tetramethyl-1,5-hexadien (6), 1,4-Bis(cyclopropyliden)butan (8), Dispiro[cyclopropan-1,2′-bicyclo[2.2.0]hexan-3′,1″-cyclopropan] (10), 2,2,3,3-Tetramethylbicyclo[2.2.0]hexan (11) und 2,2-Dimethylbicyclo[2.2.0]-hexan-3-spirocyclopropan (12) untersucht. Alle Reaktionen verlaufen nach Zeitgesetzen erster Ordnung und ergeben die folgenden Arrhenius-Beziehungen: ln(k1) = 33.6 - 31600/RT, ln(k3) = 34.2 - 35500/RT, ln(k4) = 33.6 - 35100/RT, ln(k5) = 33.6 - 3600/RT, ln(k6) = 29.1 - 33300/RT, ln(k8) = 22.0 - 26200/RT, ln(k10) = 32.0 - 35200/RT, ln(k11) = 32.0 - 40900/RT, ln(k12) = 32.3 - 39400/RT. Die kinetischen Isotopieeffekte von 1.4 und 1.1 bei der Bildung von 4 bzw. 5 (gemessen bei 175°C) und die gefundene Differenz Ea4 - Ea5 ≈ 0.1-0.9 kcal/mol sprechen für einen Umlagerungsmechanismus von 3 über ein 1,6-Diradikal, das intramolekular disproportioniert und rekombiniert zu 4, bzw. 5.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19771100713
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  • 5
    Electronic Resource
    Electronic Resource
    Phosphorhaltige Kohlenhydrate, XVII: Untersuchung der Hydrierung ungesättigter Glycosylphosphonate. Anomerer Effekt und A-Wert der Dimethylphosphono-Gruppe (1978)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 111 (1978), S. 3325-3335 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorus-containing Carbohydrates, XVII: Studies on the Hydrogenation of Unsaturated Glycosylphosphonates. Anomeric Effect and A-Value of the Dimethylphosphono GroupBy hydrogenation unsaturated glycosylphosphonates of type 1 give rise to the formation of 2,3-dideoxyglycosylphosphonates 2 and 2,3,4-trideoxyglycosylphosphonates 3. Their product ratio depends on configuration and conformation of the educts 1a-f. 1H and 13H and 13C NMR data permit an assigment of the anomers of the hydrogenated glycosylphosphonates. For the one-bond coupling constant between 13C-1 and 31P the correlation 1JC, Peq 〉 1JC, Pax is valid, which exhibits a difference of 19-23 Hz. The unsaturated glycosylphosphonates show deviations from Hudson's isorotation rule. In dimethyl cis-4-methyl-1-cyclohexanephosphonate (9) the A-value of the dimethylphosphono group has been determined to 8.34 kJ/mol. The ratio of conformers in 3a leads to an anomeric effect of the dimethylphosphono group of 2.33 kJ/mol.
    Notes: Ungesättigte Glycosylphosphonate vom Typ 1 liefern bei der Hydrierung außer 2,3-Didesoxyglycosylphosphonaten 2 auch 2,3,4-Tridesoxyglycosylphosphonate 3. Das Produktverhältnis ist von Konfiguration und Konformation der Ausgangsprodukte 1a-f abhängig. 1H- und 13C-NMR-Daten erlauben eine Anomerenzuordnung der hydrierten Glycosylphosphonate. Für die 13C-31P-Direktkopplung an C-1 gilt 1JC, Peq 〉 1JC, Pax mit einer Differenz von 19-23 Hz. Die ungesättigten Glycosylphosphonate zeigen Abweichungen von der Hudsonschen Regel. Am Dimethyl-cis-4-methyl-1-cyclohexanphosphonat (9) wurde der A-Wert der Dimethylphosphono-Gruppe zu 8.34 kJ/mol bestimmt. Aus der Konformerenverteilung bei 3a ergibt sich der anomere Effekt der Dimethylphosphono-Gruppe zu 2.33 kJ/mol.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19781111006
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  • 6
    Electronic Resource
    Electronic Resource
    Darstellung, chemische Eigenschaften und thermische Umlagerung von Spiro[3.4]octa-5,7-dien (1977)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 2561-2573 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Chemical Properties and Thermal Rearrangement of Spiro[3,4]octa-5,7-dieneThe synthesis of spiro[3.4]octa-5,7-diene (2) was achieved along two routes starting from spiro-[3.4]octan-5-one (5). In both cases the last step was a dehydrohalogenation of the halospiro-[3.4]octenes 8b/9b and 11, respectively, which had to be carried out at room temperature, because 2 dimerizes about as fast as cyclopentadiene. It also underwent addition of maleic anhydride and 2-chloroacryloyl chloride to yield 13 and 14a respectively. 14a could be degraded to the bicyclo[2.2.1]hept-2-en-5-on-7-spirocyclobutane (15a), which served as a precursor to the hydrocarbon 17. Above 90°C 2 isomerizes to a mixture of bicyclo[3.3.0]octadienes 18a and 18b. This reaction followed a first order kinetics in the gas phase with the Arrhenius equation ln(k) = 31.7 - 29200/RT. These kinetic parameters are interpreted in terms of a sigmatropic [1,5]-alkyl shift.
    Notes: Die Synthese von Spiro[3.4]octa-5,7-dien (2) gelingt ausgehend von Spiro[3.4]octan-5-on (5) auf zwei Wegen. Bei beiden wird in der letzten Stufe eine Dehydrohalogenierung eines Halogenspiro[3.4]octens 8b/9b bzw. 11 bei Raumtemperatur vorgenommen, weil 2 bei höheren Temperaturen ähnlich schnell dimerisiert wie 1,3-Cyclopentadien. Ebenso addiert es leicht Maleinsäureanhydrid und 2-Chloracryloylchlorid zu 13 bzw. 14a. 14a läßt sich zum Bicyclo[2.2.1]hept-2-en-5-on-7-spirocyclobutan (15a) abbauen, aus dem der Kohlenwasserstoff 17 zugänglich ist. Oberhalb von 90°C isomerisiert 2 zu einem Gemisch der Bicyclo[3.3.0]octadiene 18a und 18b. Die Kinetik dieser Reaktion in der Gasphase zeigt einen Verlauf erster Ordnung und folgt dem Arrhenius-Ansatz ln(k) = 31.7 - 29200/RT. Daraus ist für den Mechanismus auf eine konzertierte [1,5]-Alkylverschiebung zu schließen.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19771100714
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  • 7
    Electronic Resource
    Electronic Resource
    Optisch aktive, aromatische Spirane, 5. Stereochemie von Metallocenen, 39. Eine universelle Methode zur Darstellung, Konfigurationsermittlung und Bestimmung der enantiomeren Reinheit chiraler 2,2′-Spirobiindane (1977)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 1403-1420 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Optically Active, Aromatic Spiranes, 5. Stereochemistry of Metallocenes, 39. An Universal Method for the Preparation, and Determination of the Absolute Configuration and Enantiomeric Purity of Chiral 2,2′-SpirobiindanesFrom optically active tricarbonyl(1-oxoindane)chromium complexes 1 of known configuration and enantiomeric purity by reaction with phthalaldehydic esters 2 and hydrogenation of the benzal derivatives 4 chiral key compounds 5 and 6 for the preparation of 2,2′-spirobiindan-1,1′-diones are obtained. Cyclization of 6 yields diastereomers (cis- and trans-7) which after mild removal of Cr(CO)3 afford the enantiomeric biindanones 8 from which 2,2′-spirobiindanes 9 are accessible. Chiralities and enantiomeric purities of all spiranes can easily be deduced from those of the indanones 1. This universal principle is presented for several methyl- and methoxy-2,2′-spirobiindan-1,1′-diones and -biindanes.
    Notes: Aus optisch aktiven Tricarbonyl(1-oxoindan)chrom-Komplexen 1 bekannter Konfiguration und enantiomerer Reinheit werden durch Umsetzung mit Phthalaldehydsäureestern 2 und Hydrierung der Benzalderivate 4 chirale Schlüsselverbindungen 5 bzw. 6 zur Darstellung von 2,2′-Spirobiindan-1,1′-dionen erhalten. Ringschluß von 6 führt zu Diastereomeren (cis- und trans-7), die nach schonender Abspaltung von Cr(CO)3 die enantiomeren Biindanone 8 liefern, aus denen die 2,2′-Spirobiindane 9 zugänglich sind. Chiralität und enantiomere Reinheit aller Spirane folgen aus jenen der eingesetzten Indanone 1. Dieses universelle Prinzip wird anhand einiger Methyl- und Methoxy-2,2y-spirobiindan-1,1′-dione und -biindane präsentiert.
    Additional Material: 8 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19771100424
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  • 8
    Electronic Resource
    Electronic Resource
    Beiträge zur Chemie des Indols, VIII. Decarboxylierungen einiger 1-Alkyl-2-carboxy-3-indolessigsäuren sowie Synthese eines 5-Thiocyanato-2,3-dihydroindols (1975)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 3538-3542 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Not mentioned2a-d, easily produced from the N-alkyl-N-phenylhydrazines 1a-d and 2-oxoglutaric acid, are decarboxylated to the compounds 4a-d in high yields. 2a is reduced to the 2,3-dihydro compound 3a and reacts via the amide 5a to the 5-thiocyanato derivative 6a.
    Notes: Contributions to the Chemistry of Indole, VIII. Decarboxylations of Some 1-Alkyl-2-carboxy-3-indolacetic Acids and Synthesis of a 5-Thiocyanato-2,3-dihydroindole-d, leicht darstellbar aus N-Alkyl-N-phenylhydrazin und 2-Oxoglutarsäure, werden mit hoher Ausbeute zu 4a-d decarboxyliert. 2a wird zum Dihydroindol 3a reduziert und über das Amid 5a zum 5-Thiocyanatoderivat 6a umgesetzt.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19751081115
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  • 9
    Electronic Resource
    Electronic Resource
    The Inversion of the Amino Group in Vinylamine, a Flexible Model TreatmentA preliminary account of this work was given at the meeting of the Swiss Chemical Society in Geneva, October 9, 1976. (1978)
    New York, NY : Wiley-Blackwell
    Helvetica Chimica Acta 61 (1978), S. 1418-1426 
    Details
    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Flexible model results for the —NH2 inversion in vinylamine are compared with microwave data published by Lovas et al. [3]. The information available on the spacing of inversion levels is found to be sufficient to rule out a planar equilibrium structure. Shifts of rotational constants upon excitation of the inversion are calculated for two predicted paths of motion derived from PRDDO geometry optimization results obtained by MiiIler & Brown [2]. Partial geometry optimization yields a path inconsistent with experiment but the path obtained from complete optimization produces shifts in excellent agreement with the observed shifts. A potential energy function compatible with experimental data on spacing of inversion levels is calculated from the observed inertia defects. The inversion angle at equilibrium is slightly smaller than the angle predicted from PRDDO calculations, and the barrier to inversion, ΔV = 1.08 ± 0.07 kcal/mol, is approximately half the PRDDO value.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/hlca.19780610426
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  • 10
    Electronic Resource
    Electronic Resource
    Enhydrazine, 131) Einige Produkte aus 3-Hydroxy-1-methyl-5-pyrazolcarbonsäure- methylester und 1-Benzyl-3-hydroxypyrazol (1976)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 109 (1976), S. 268-273 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Enehydrazines, 131) Some Products from Methyl 3-Hydroxy-1-methyl-5-pyrazolecarboxylate and 1-Benzyl-3-hydroxypyrazoleSome esters and ethers of the 3-pyrazolones 1a, 2c and6a are Prepared. They are derived from the tautomeric 3-hydroxypyrazole forms in which the free starting compounds mostly occur. Some substitutions in 4-position are likewise described.
    Notes: Es werden einige Ester und Äther der 3-Pyrazolone 1a, 2c und 6a dargestellt, die sich von der tautomeren 3-Hydroxypyrazol-Form herleiten, in der auch die freien Ausgangsverbindungen vorliegen. Einige Substitutionen in 4-Stellung der 3-Hydroxypyrazole werden ebenfalls beschrieben.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19761090127
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