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  • 1
    Electronic Resource
    Electronic Resource
    Beiträge zur Chemie und Strukturchemie von Tris(diphenylphosphino)ethen und 1,1,4,4-Tetrakis(diphenylphosphino)-1,3-butadien (1989)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 1857-1861 
    Details
    ISSN: 0009-2940
    Keywords: Tris(diphenylphosphino)ethene derivatives ; 1,1,4,4-Tetrakis(diphenylphosphino)-1,3-butadiene derivatives ; Molybdenum complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry and Structures of Tris(diphenylphosphino)enthen and 1,1,4,4-Tetrakis(diphenylphosphino)-1,3-butadieneReaction of tris(diphenylphosphino)ethene (1), obtained by basecatalyzed hydrophosphorylation of Ph2PC≡CPPh2 with Ph2PH, with 2 equivalents of H3B · OC4H8 affords 1,1-bis(boranatodi-phenylphosphonio)-2-(diphenylphosphino)ethene (2). Methylation of 1 with MeI gives the monoquaternary salt 3, the molecular structure of which was determined by X-ray crystallography. A trisulfide 4 is available by treatment of 1 with elemental sulfur. - 1,1,4,4-Tetrakis(diphenylphosphino)-1,3-butadiene (5) was isolated as a byproduct in the synthesis of 1. 1,1,4,4-substitution was established by X-ray analysis of the tetrasulfide 6, obtained by treatment of 5 with elemental sulfur. Reaction of 5 with 2 equivalents of Mo(CO)6 yields the symmetrical, dinuclear complex 7.
    Notes: Das durch basenkatalysierte Addition von Ph2PH an Ph2PC≡CPPh2 erhaltene Tris(diphenylphosphino)ethen (1) reagiert mit 2 Äquivalenten H3B · OC4H8 zu 1,1-Bis(boranatodiphenylphosphonio)-2-(diphenylphosphino)ethen (2). Die Behandlung von 1 mit Iodmethan liefert neben nicht näher untersuchten Spaltprodukten das Monoquartärsalz 3, in dem die Oniumfunktion am mittleren der drei Phosphoratome auftritt. Die Kristallstruktur wurde röntgenographisch bestimmt. Bei Behandlung von 1 mit Schwefel entsteht das Trisulfid 4.  -  Bei der Darstellung von 1 wird als Nebenprodukt 1,1,4,4-Tetrakis(diphenylphosphino)-1,3-butadien (5) gebildet. Die Substitution in den 1,1,4,4-Positionen wurde ebenfalls durch Röntgenstrukturanalyse des Tetrasulfids 6 bestätigt, das durch Reaktion von 5 mit elementarem Schwefel darstellbar ist. 5, dessen Bildungsmechanismus noch nicht geklärt ist, reagiert mit 2 Äquivalenten Mo(CO)6 zum zweikernigen Molybdänkomplex 7.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19891221006
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  • 2
    Electronic Resource
    Electronic Resource
    Arsen(III)-, Antimon(III)- und Bismuth(III)-halogenid-Komplexe des [2.2.2]Paracyclophans: Vom lockeren van-der-Waals-Addukt zu stark gerichteten π-Komplexen mit zwei- und dreifacher externer η6-Koordination (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1089-1093 
    Details
    ISSN: 0009-2940
    Keywords: [2.2.2]Paracyclophane ligand ; (η6)π Complexes ; Arsenic(III) complexes ; Antimony(III) complexes ; Bismuth(III) complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Arsenic(III), Antimony(III), and Bismuth(III) Trihalide Complexes of [2.2.2]Paracyclophane: From Weak van der Waals Coordination to Strongly Directional π Complexation with Single or Double External η6 Coordination[2.2.2]Paracyclophane forms the adducts C24H24·AsCl3 (1), C24H24·(SbCl3)2·1/2 C6H6 (2), and C24H24·(BiCl3)3·C6H6 (3). For solutions in polar solvents NMR spectra indicate extensive dissociation and/or fluxionality. In the crystals adduct 1 features a weak addition of the AsCl3 molecule to one open side of a paracyclophane molecule with long intermolecular contacts approaching C3v symmetry. - Crystalline 2 shows SbCl3 coordination to two of the benzene rings of the hydrocarbon in a quasi-centered η6 mode, while one of the benzene rings remains uncoordinated. Chlorine-bridging between antimony atoms leads to tetrameric units (SbCI3)4 in the lattice. - In the bismuth compound 3 each benzene ring of the hydrocarbon is engaged in centroid (η6)π complexation, with the BiCl3 units crosslinked by chlorine bridges. The average of the Bi-ring distances (3.08,2.98, and 2.99 Å) is shorter than for the Sb-ring distances in 2 (3.047 and 3.050 Å), indicating stronger bonding. The crystal benzene is not coordinating.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240516
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  • 3
    Electronic Resource
    Electronic Resource
    Preparation and Structure of Hexakis[(trialkylphosphane)aurio(I)]methanium(2+) Salts [(LAu)6C]2+(X-)2 with L=Et3P, iPr3P and X=BF4-, B3O3F4- (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 2705-2710 
    Details
    ISSN: 0009-2940
    Keywords: Auriophilicity ; Gold(I), phosphane complexes ; Methanium, hexaaurio(I) compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Hexaaurated carbon complexes of the type [(R3PAu)6C](BF4)2, R=Et (2a), iPr (2b) have been prepared by the reaction of the appropriate (phosphane)gold(I) chlorides R3PAuCl (1a and 1b) with tetrakis(dimethoxyboryl)methane, 13C-enriched at the central carbon atom, in the presence of excess of CsF in HMPT at room temperature. The products 2a and 2b are characterized by standard spectroscopic methods including direct detection of the interstitial C atoms by 13C-NMR spectroscopy. The crystal structure of the compound [(iPr3PAu)6C](B3O3F4)2 · 3 CH2Cl2 (3), obtained from partial (anion) hydrolysis has been determined. It contains dications with a central carbon atom surrounded by six (phosphane)gold(I) units. The edges of the CAu6 octahedron represent short Au-Au contacts (aprox. 3.0 Å), which strongly contribute to the formation and stability of these hypercoordinated species. Attempts to prepare a corresponding hexaauriomethanium dication starting from tBu3PAuCl (1c) failed owing to the bulkiness of the (tri-tert-butylphosphane)gold(I) unit. The X-ray structure analysis for 1c verifies an extremely crowded environment of the gold atom with small Au - P - C angles of only 107° leading to efficient shielding of the metal atom by methyl groups.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921251214
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  • 4
    Electronic Resource
    Electronic Resource
    A synthetic route to poly(silyl)methanes via poly(phenylsilyl)methanes and poly(bromosily)methanes (1989)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 2115-2119 
    Details
    ISSN: 0009-2940
    Keywords: CVD feedstock gases ; Poly(bromosilyl)methanes ; Poly(phenylsilyl)methanes ; Poly(silyl)methanes ; Silanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ein Syntheseweg zu Poly(phenylsilyl)methane und Poly(bromsilyl)methaneFür Di- und Tri(silyl)methan, aus denen durch Dampfphasenzersetzung (CVD) Kohlenstoff-haltiges amorphes Silicium (a-SiC:H) erhalten werden kann, wird eine ergiebige dreistufige Synthese beschrieben: Chlor(phenyl)silan und Di- oder Trihalogenmethane reagieren in guten Ausbeuten mit Magnesium in Tetrahydrofuran zu Bis- bzw. Tris(phenylsilyl)methan. Durch Behandlung mit wasserfreiem Bromwasserstoff können daraus fast quantitativ die Zwischenprodukte Bis- bzw. Tris(bromsilyl)methan erhalten werden, deren Hydrierung mit Lithiumaluminiumhydrid im Zweiphasensystem mit Phasentransferkatalysator die Zielverbindungen CH2(SiH3)2 bzw. CH(SiH3)3 ergibt. Wie diese Verbindungen wurden auch CH2(SiH2Ph)2, CH(SiH2Ph)3, CH2(SiH2Br)2, und CH(SiH2Br)3, durch spektroskopische Standardmethoden charakterisiert. Die Kristall- und Molekülstruktur von CH(SiH2Ph)3 wurde durch Einkristallröntgenbeugung ermittelt. Die für das Molekül gefundene kristallographische C3-Symmetrie wird unter Bezugnahme auf die Struktur anderer Spezies diskutiert, in denen drei Substituenten mit potentieller Cs-Symmetrie an ein tetraedrisches Zentrum gebunden sind.
    Notes: A three-step synthesis is presented for di- and tri(silyl)methane, two feedstock gases for the chemical vapour deposition of amorphous hydrogenated silicon/carbon alloys (a-SiC:H). Chloro(phenyl)silane and di- or trihalomethanes react with magnesium in tetrahydrofuran to give high yields of bis- and tris(phenylsilyl)methane, respectively. The two products can be converted into bis- and tris(bromosilyl)methane by treatment with anhydrous hydrogen bromide. Bromide/hydride substitution in these precursors is accomplished with lithium aluminum hydride in a two-phase system using a phase-transfer catalyst. The compounds CH2(SiH2Ph)2, CH(SiH2Ph)3, CH2(SiH2Br)2, CH(SiH2Br)3, CH2(SiH3)2, and CH(SiH3)3 have been characterized by standard spectroscopic methods, and the crystal and molecular structure of CH(SiH2Ph)3 has been determined by single-crystal X-ray diffraction. The molecule adopts a conformation with crystallographic C3 symmetry. This result is discussed with regard to the structure of related molecules with three substituents of potential Cs symmetry at a tetrahedral center.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19891221111
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  • 5
    Electronic Resource
    Electronic Resource
    Gold(I) Complexes of Primary Phosphanes: Pair Formation through Au…Au Interactions (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 285-287 
    Details
    ISSN: 0009-2940
    Keywords: Phosphanes, primary / Gold complexes / Gold-gold interactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (CO)AuCl reacts with (2,4,6-trialkylphenyl)phosphanes 1a-d (alkyl = Me, Et, iPr, tBu) to give the 1:1 complexes 2a-d. The crystal structure of 2d shows pairs of molecules with Au…Au contacts of 3.440(1) Å.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901230210
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  • 6
    Electronic Resource
    Electronic Resource
    Syntheses and Molecular Structures of an Isoelectronic Series of (2-Hetero-)1,3-Diphosphabenzenes (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1525-1530 
    Details
    ISSN: 0009-2940
    Keywords: 1,3-Diphosphabenzene derivatives ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Syntheses, NMR spectra, and X-ray molecular structures of three (2-hetero-)1,3-diphosphabenzenes are reported which constitute an isoelectronic triade of compounds with BH2, CH, and N bridging units between the two phosphorus atoms. The remaining three carbon atoms of the rings are part of a 2-methallylic system. The 2-borataheterocycle 3 has been prepared by the reaction of CH2 = C(CH2)PPh2)2 (1) with Me2S—BH2Br to give an intermediate 2 still containing the exocyclic olefinic bond. Treatment of 2 with a base, deprotonation of one ring CH2 group, and proton migration from the other one to the olefinic CH2 group afford the 5-methyl-1λ5-phospha-3-phosphonia-2-boratabenzene 3. The PBP unit is tilted by 144.0(2)° against the planar C3P2 part of the ring. A heterocyclic precursor 4 for the carbon analog is generated from 1 and CH2I2, which on reaction with a strong base yields the diphosphabenzene 5 with a fully planar ring skeleton. For the synthesis of the aza analog 7, CH2=C(CH2Cl)2 is treated with HN(PPh2)2 to give the precursor 6, which can be deprotonatad at nitrogen and carbon with a base. In the crystals of 7, two independent molecules of very similar structure are present. The molecules show planar heterocycles.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240708
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  • 7
    Electronic Resource
    Electronic Resource
    Fusing Cyclopentadiene and Ferrocene by Two Silyl Bridges Stereochemically Well-Defined Building Blocks for High-Nuclear Metallocenes (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1531-1539 
    Details
    ISSN: 0009-2940
    Keywords: Ferrocenes ; Cyclopentadienes, disilyl- ; Silatropic rearrangement ; Lithium cyclopentadienides ; Metallocene, trinuclear, mixed-metal ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tetrahydro-4,4,8,8-tetramethyl-4,8-disila-s-indacenyl anion (LH) reacts with or without cyclopentadienyl anion (Cp-) and Fe2Cl4(THF)3 to give the mixed ferrocenes CpFe(LH) and (LH)2Fe in 50 and 63% yield, respectively. Near room temperature and in solution CpFe(LH) exists as a pair of enantiomers (syn-3a/b). According to an X-ray analysis both enantiomers are present in a single crystal. Compound 3 consists of a ferrocene linked to a cyclopentadiene by two Me2Si groups such that the acidic Cp proton points towards the iron. Temperature-dependent NMR spectra show that syn-3a and syn-3b are non-rigid molecules which are interconverted by 1,2-silatropic bond shifts (Ea = 49.2 ± 2.9 kJmol-1). Three more isomers (anti-3a, anti-3b, and the spiro derivative 3c), though present only in low concentration, are engaged in the rearrangement. (LH)2Fe is also non-rigid and exists as a pair of diastereomers (4a and 4b). The isomers of 3 and 4 undergo hydrolysis (e.g., syn-3a/3b gives [(Me2SiOSiMe2)Cp]FeCp (5) among others) and deprotonation. The latter yields CpFe(L-) (7) and (L-)2Fe (8), which are characterized by NMR spectroscopy. 7 forms crystals with [Li(TMEDA)]+ as counterion, and an X-ray analysis shows that lithium and iron are located at opposite sides of the strongly folded ligand L. The reaction of 7 with CrCl2(THF) gives the trinuclear stacked metallocene 9 in 47% yield. 9 has two unpaired electrons which are located essentially in the center of the molecule.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240709
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  • 8
    Electronic Resource
    Electronic Resource
    Hexacoordinated Group-14 Elements with Phosphorus Donor Ligands: Syntheses and Structures of Cl2E[C(PMe2)2(SiMe3)]2 (E = Si, Ge, Sn) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 671-676 
    Details
    ISSN: 0009-2940
    Keywords: Hexacoordination ; Silicon ; Germanium ; Tin ; Phosphinomethanide Ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The group-14 tetrahalides ECl4 (E = Si, Ge, Sn) react with two equivalents of Li[C(PMe2)2(SiMe3)] to give the trans-hexacoordinated complexes Cl2E[C(PMe2)2(SiMe3)]2, which were characterized spectroscopically and by structure determinations in the solid state. The complexes were found to crystallize with or without tetrahydrofuran (THF) molecules, depending on the presence or absence of this solvent. In the case of the silicon complex, the structures of both crystal forms were determined, showing slightly different molecular structures of the complexes in the solid state. Without cocrystallized THF, Cl2Si[C(PMe2)2(SiMe3)]2 has no crystallographically imposed molecular symmetry, while in the presence of THF its crystallographic symmetry is C2h (2/m). The tin and germanium complexes were crystallized either with and without THF molecules, respectively, their crystal structures being isotypic with the respective ones of the silicon complex. In all cases, small amounts of the cis-hexacoordinated isomers were also observed in solution, but only in the case of the silicon complex, it was isolated in pure form. It rearranges to the trans isomer at ambient temperature. trans-Cl2Si[C(PMe2)3]3, trans-Cl2Si[C(PPh2)2(SiMe3)]2 and cis-Me2-Si[C(PMe2)2(SiMe3)]2 were likewise obtained.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290613
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  • 9
    Electronic Resource
    Electronic Resource
    CH2=PPh und CH2=AsPh als Liganden an Rhodium Kristall- und Molekülstruktur von C5Me5Rh(η2-CH2PPh)(CO) und C5Me5(CO)Rh(AsPh)3 (1989)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 1061-1066 
    Details
    ISSN: 0009-2940
    Keywords: Phospha- and arsaalkene rhodium complexes ; Metalla heterocycle containing RhAs3 ; Rhodium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: CH2=PPH and CH2=AsPh as Ligands Coordinated to Rhodium. Crystal and Molecular Structure of C5Me5Rh(η2-CH2PPh)(CO) and C5Me5(CO)Rh(AsPh)3C5Me5RhCH2I(CO)I (1) reacts with excess LiPHPh or LiAsHPh to give the complexes C5Me5Rh(η2-CH2EPh)(CO) (2: E = P; 3: E = As). The C—P bond length of the coordinated phosphaalkene in 2 is 174.0(4) pm and thus ca. 10 pm shorter than that of a C—P single bond. On standing in solution, the new heterocycle C5Me5(CO)Rh(AsPh)3 (4) is formed from 3. The X-ray analysis of 4 shows that the bonding distances and angles in the central nonplanar RhAs3 four-membered ring are very similar to thos in cyclo-(AsCF3)4.
    Notes: C5Me5RhCH2I(CO)I (1) reagiert mit überschüssigem LiPHPh oder LiAsHPh zu den Komplexen C5Me5Rh(η2-CH2EPh)(CO) (2: E = P; 3: E = As). Der C—P-Abstand des koordinierten Phosphaalkens in 2 ist mit 174.0(4) pm um ca. 10 pm kürzer als der einer C—P-Einfachbindung. Beim Stehenlassen in Lösung entsteht aus 3 teilweise der Heterocyclus C5Me5(CO)Rh(AsPh)3 (4), von dem die Struktur bestimmt wurde. Die Bindungsabstände und -winkel in dem zentralen, nicht planaren RhAs3-Vierring sind denen in cyclo-(AsCF3)4 sehr ähnlich.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19891220608
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  • 10
    Electronic Resource
    Electronic Resource
    π-Complexes of p-Block Elements: Synthesis and Structures of Adducts of Arsenic and Antimony Halides with Alkylated Benzenes (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 1221-1226 
    Details
    ISSN: 0009-2940
    Keywords: π-Complexes of p-block elements ; Arene complexes ; Arsenic complexes ; Antimony complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,2,4,5-Tetramethyl-and pentamethylbenzene from stable 1:2 complexes with SbCl3 of the type (C6H6-Men) · 2SbCl3(1,2) with an inverse sandwich structure. The compounds crystallize isotypically and are isostructural to the (hexamethylbenzene)antimony and -bismuth complexes.They are thus built of tetrameric chlorine-bridged Sb4Cl12 units, which are crosslinked at the metal centers with four other tetramers by double-sided arene coordination (X-ray structure analysis of 1). The Sb atoms, which are in a distorted trigonal bipyramidal environment, show a slight deviation from a centric (η6) coordination. The same stoichiometry and the same structural principle are found for the complex (C6Me6 · 2 AsCl3 (4), which is obtained from solutions of hexamethylbenzene and AsCl3 in toluene. In 4 the arsenic atoms are η6-coordinated to the hexamethylbenzene ring from both sides (X-ray analysis). Treatment of AsBr3 with hexamethylbenzene leads to a product of the composition 5 (C6Me6) · AsBr3. Reaction of hexaethylbenzene with AsCl3 in petroleum ether leads to the formation of the 1:2 complex (C6Et6) · 2 AsCl3 (5), built of discrete inverse sandwich units, which are arranged in strings parallel to the crystallographic c axis. From solutions of AsCl3 (AsBr3), SbCl3 (SbBr3) and hexaethylbenzene in petroleum ether ternary compounds are isolated with an As:Sb ratio of 1:5.2 and 1:1.86, respectively. Single crystal X-ray structure determinations failed as a consequence of severe disorder.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901230602
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