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  • Inorganic Chemistry  (25)
  • 1,3-diphosphorinances  (1)
  • 1-phosphabicyclo[3.3.1]nonanes  (1)
  • 1-phosphabicyclo[4.3.0]nonanes  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Zur Aminomethylierung der Heterocycloalkanone-(3) (1968)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 101 (1968), S. 1052-1055 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Die Aminomethylierung der Heterocycloalkanone-(3) Thiophanon-(3), Tetrahydrothio-pyranon-(3) und Chromanon-(3) findet im sauren Medium bevorzugt in 4-Stellung und nicht an der dem Heteroatom benachbarten Methylengruppe statt. Die Struktur der Amin-Eliminierungsprodukte aus Mannich-Basen-Hydrochloriden von 2-Äthoxycarbonyl-tetra-hydrothiopyranon-(3) und 2-Äthoxycarbonyl-thiophanon-(3) weist ebenfalls auf eine Substitution in 4-Stellung hin.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19681010341
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  • 2
    Electronic Resource
    Electronic Resource
    Reaction of Cyclic Thioureas with 2-Benzylidenecycloalkanones (1987)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 120 (1987), S. 1449-1450 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: BF3. OEt2-catalyzed reaction of cyclic thioureas (1) with 2-benzylidenecycloalkanones (2) afforded tricyclic 1,3-thiazines (3, 4). The progress of the reactions was found to depend on the ring size of both 1 and 2.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19871200827
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  • 3
    Electronic Resource
    Electronic Resource
    Zur Konfiguration der 1,3-Dichlor-2-methyl-1-propene (1983)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 116 (1983), S. 522-526 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Configuration of the 1,3-Dichloro-2-methyl-l-propenesDetermination of the configurations of 1,3-dichloro-2-methyl-1-propenes (1) was performed by 1H and 13C NMR spectroscopy using the isomer pairs of 1,3-dichloro-1-propenes (2), 1-chloro-2-methyl-1-propene-3-ols (3) and 1-chloro-1-propene-3-ols (4) as reference compounds. The chemical shifts, vicinal coupling constants, relative LIS value and NOE effects were in an unambiguous agreement with the (Z)-configuration of the lower-boiling isomer of 1.
    Notes: Die Konfigurationen von 1,3-Dichlor-2-methyl-1-propenen (1) werden mittels 1H- und 13C-NMR-Spektroskopie zugeordnet. Als Vergleichssubstanzen dienten die Isomeren von 1,3-Dichlor-1-propen (2), 1-Chlor-2-methyl-1-propen-3-ol (3) und 1-Chlor-1-propen-3-ol (4). Die chemischen Verschiebungen, vicinalen Kopplungskonstanten, relativen LIS-Werte und NOE-Effekte stehen mit der (Z)-Konfiguration des niedriger siedenden Isomeren von 1 eindeutig im Einklang.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19831160213
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  • 4
    Electronic Resource
    Electronic Resource
    1,4,7,10,13,16,19,22-Octaazacyclotetracosane-1,4,7,10,13,16,19,22-octaacetic Acid (H8OTEC) and 1,4,7,10,14,17,20,23-Octaazacyclohexacosane- 1,4,7,10,14,17,20,23-octaacetic Acid (H8OHEC): Synthesis and Characterization of Two Large Macrocyclic Polyamine Polycarboxylic Ligands and Some of Their Copper(II) and Lanthanide(III) Complexes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 267-277 
    Details
    ISSN: 0009-2940
    Keywords: Macrocyclic ligands ; Lanthanides ; Copper ; Polyamines ; Polycarboxylic acids ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The optimized synthesis of two new macrocyclic polyamine polycarboxylic ligands, 1,4,7,10,14,17,20,23-octaazacyclohexacosane-1,4,7,10,14,17,20,23-octaacetic acid (H8OHEC) (10) and 1,4,7, 10,13,16,19,22-octaazacyclotetracosane-1,4,7,10, 13,16,19,22-octaacetic acid (H8OTEC) (12), is presented. The key step in the synthesis of both is the high yield carboxymethylation of the corresponding macrocyclic amines using tert-butyl bromoacetate followed by acidic hydrolysis of the acetate protecting groups. The molecular structures of the intermediates 1,4,7,10,14,17,20,23-octaazacyclohexacosane (OHEC-amine) (8), and octa-tert-butyl 1,4,7,10,13,16,19,22- octaazacyclotetracosane-1,4,7,10,13,16,19,22-octaacetate (OTEC-ester) (11) are determined by X-ray crystal structure analysis. OHEC-amine 8 reacts with 2 equiv. of CuSO4 yielding the dinuclear complex [Cu2(OHEC-amine)](SO4)2 (13). Complex 13 crystallizes with 16 molecules of water. 13 · 16 H2O contains two copper atoms, which are coordinated in a strongly distorted octahedral fashion by four nitrogen atoms, one oxygen atom from the sulfate dianion and one oxygen atom from a water molecule. The new ligands 10 and 12 are fully characterized by 1D- and 2D-NMR spectroscopy. Both ligands form dinuclear lanthanide(III) chelates (Ln=Y, Sm, Eu, Gd, Yb, Lu), which are stable and highly water soluble. With lanthanum(III) only mononuclear complexes are formed.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300221
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  • 5
    Electronic Resource
    Electronic Resource
    1,5-Diphosphabicyclo[3.3.1]nonanFrau Professor Marianne Baudler zum 70. Geburtstage am 27. April 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 594 (1991), S. 66-76 
    Details
    ISSN: 0044-2313
    Keywords: Organophosphorus compounds, bicyclic hydrophosphorylation, intramolecular ; methylenebisphosphines ; 1,3-diphosphorinances ; 1,5-diphosphabicyclo[3.3.1]nonanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,5-Diphosphabicyclo [3.3.1]nonane1,5-Diphosphabicyclo[3.3.1]nonane 8 has been obtained by free-radical cyclization of CH2=CHCH2(H)PCH2P(H)CH2CH=CH2 6 and 1-allyl-1,3-diphosphorinane 7. For the synthesis of 6 and 7 the chlorophosphine Cl2PCH2PCl2 1 is used as a starting material, which can be converted into Me2N(Cl)PCH2P(Cl)NMe2 3 by reaction with (Me2N)2PCH2P(NMe2)2 2. Treatment of 3 with two equivalents of allyl lithium and cleavage of the PN bonds in CH2=CHCH2(Me2N)PCH2P(NMe2)CH2CH=CH2 4 with diluted HCl affords CH2=CHCH2(H)(O)PCH2P(O)(H)CH2CH=CH2 5. Phenylsilane is used for the first time as a reducing agent to obtain a secundary phosphine like 6 from the secundary phosphine oxide (5). Prolonged heating increases the yield of the byproduct 7 in the mixture of 6 and 7. Reactions of the trivalent phosphorus in 8 with CS2, CH3I, POCl3, NO, sulfur, and KSeCN, respectively, delivers the corresponding derivatives 9-17. The compounds decribed are characterized by 1H, 13C, 31P, 77Se n.m.r., i.r., and m.s. data.
    Notes: 1,5-Diphosphabicyclo[3.3.1]nonan 8 wird durch radikalische Cyclisierung von CH2=CHCH2(H)PCH2P(H)CH2CH=CH2 6 und 1-Allyl-1,3-diphosphorinan 7 erhalten. Ausgangsmaterial für die Synthese von 6 und 7 ist Cl2PCH2PCl2 1, das mit (Me2N)2PCH2P(NMe2)22 quantitativ zu Me2N(Cl)PCH2P(Cl)NMe2 3 reagiert. Die Umsetzung von 3 mit zwei Äquivalenten Allyllithium zu CH2=CHCH2(Me2N)PCH2P(NMe2)CH2CH=CH2 4 und Abspaltung der Me2N-Schutzgruppen mit verdünnter Salzsäure liefert CH2=CHCH2(H)(O)PCH2P(O)(H)CH2CH=CH2 5. Dessen Reduktion zu 6 gelingt mit C6H5SiH3. Daneben entsteht 7, das durch längeres Erhitzen angereichert werden kann. Reaktionen des dreibindigen Phosphors in 8 mit CS2, CH3I, POCl3, NO, Schwefel und KSeCN führen zu den Derivaten 9-17. Die Verbindungen werden durch 1H-, 13C-, 31P- und 77Se-NMR-sowie IR- und MS-Daten charakterisiert.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915940108
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  • 6
    Electronic Resource
    Electronic Resource
    Cis- und trans-1-Phosphabicyclo[4.4.0]decanProfessor Rudolf Hoppe zum 65. Geburtstage am 29. Oktober 1987 gewidmet (1987)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 553 (1987), S. 136-146 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cis- and trans-1-Phosphabicyclo[4.4.0]decaneA mixture of cis-(5a) and trans-1-phosphabicyclo [4.4.0] decane 5b has been prepared by free-radical cyclization of (CH2 = CH—CH2—CH2)2CH—PH2 10. The isomers could be separated in a pure state. Stereostructures have been assigned by 13C n.m.r. at 153 - 302 K. Equilibration of 5a and 5b by u.v. irradiation gave ⊲G°35 ≍ 0 kJ ° mol-1 · Activation parameters for ring inversion of “cis” stereoisomer 5a and its “cis” P-sulfid 17a are found to be ΔG° = 41.9 kJ · mol-1 and 39.7 kJ · mol-1, respectively. Treatment of 5a and 5b with H2O2, sulfur, selenium, HSO3F, CH3I, CS2, and Ni(CO)4, respectively, yield the corresponding derivatives. 1H, 13C, 31P, 77Se n.m.r. and i.r. data are reported.
    Notes: Durch radikalische Cyclisierung von (CH2=CH—CH2—CH2)2CH—PH2 10 wird eine Mischung von cis- (5a) und trans-1-Phosphabicyclo[4.4.0]decan (5b) erhalten. Nach Trennung in die reinen Stereoisomeren konnten die Strukturen durch 13C-NMR-Spektren bei 153 - 302 K zugeordnet werden. Gleichgewichtseinstellungen 5a ⇌ 5b durch UV-Bestrahlung ergaben bei 35°C einen ⊲G°-Wert nahe Null. Die Aktivierungsparameter für die Ringinversion von 5a und seinem Sulfid 17a betragen ⊲G = 41,9 kJ · mol-1 bzw. 39,7 kJ · mol-1. Umsetzungen von 5a und 5b mit H2O2, Schwefel, Selen, HSO3F, CH3I, CS2 und Ni(CO)4 führten zu den entsprechenden Derivaten. Werte der 1H-, 13C-, 31P- und 77Se-NMR-Spektren sowie IR-Daten der LNi(CO)3 (L = 5a, 5b) werden mitgeteilt.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19875531016
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  • 7
    Electronic Resource
    Electronic Resource
    Isomerisierung bei der Komplexbildung von 3-Acetyl-tetramsäure: Struktur und magnetische Eigenschaften des CuII- und NiII-Komplexes von 2,7-Bis(1′, 5′, 5′-trimethylpyrrolidin-2′, 4′-dion-3′ -yl)-3, 6-diazaocta-2, 6-dien (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 614 (1992), S. 87-94 
    Details
    ISSN: 0044-2313
    Keywords: Chelating agent: CuII and NiII complex ; complexation ; relaxation times ; 13C-n. m. r. ; magnetic properties ; X-ray analysis ; structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Isomerization at the Complexation of 3-Acetyltetramic Acid: Structure and Magnetic Properties of the CuII- and NiII-Complex of 2,7-Bis (1′, 5′, 5′ -trimethylpyrrolidin-2′,4′ -dion-3′ -yl)-3,6-diazaocta-2,6-dien2,7-Bis(1′, 5′, 5′ -trimethylpyrrolidin-2′, 4′ -dion-3′ -yl)-3,6-diazaoctadien formes CuII and NiII complexes with different constitutions (because of the Z/E isomerization). Results of X-ray analysis of N,N′ -ethylenbis(1′, 5′, 5′ -trimethylpyrrolidin-2′, 4′ -dion-3′ -acetiminato)nickel(II) 1 respectively -copper(II) 2 shows, that the complexing agent in 1 occurs in the E-form, whereas the ligand of the CuII complex forms the Z-form. Magnetic susceptibility and shift effects of the 13C-NMR signals point to a weak paramagnetism of the NiII complex. ESR-spectra are obtained from 2 only. Furthermore, the CuII complex reduces the relaxation times T1 and T2 of 1H and 17O nuclei spins from water. From the temperature dependence of the shortening of the relaxation times an activation energy is calculated which describes the reorientation of the copper complex in the “water matrix”.
    Notes: 2,7-Bis(1′, 5′, 5′ -trimethylpyrrolidin-2′, 4′ -dion-3′ -yl)-3,6-diazaocta-2,6-dien bildet aufgrund der Z/E-Isomerisierung als Ligand CuII- und NiII- Komplexe unterschiedlicher Konstitution. Die Ergebnisse der Röntgenstrukturanalyse von N,N′ -Ethylen-bis- (1′, 5′, 5′ -trimethylpyrrolidin-2′, 4′ -dion-3′ -acetimina-to)-Nickel-(II) 1 bzw. -Kupfer-(II) 2 zeigen, daß bei 1 der Ligand in der E-Form hingegen beim Kupferkomplex in der Z-Form vorliegt. Die magnetische Suszeptibilität und die Verschiebungseffekte der Ligandensignale in den 13C-NMR-Spektren deuten einen schwachen Paramagnetismus des Nickelkomplexes an. EPR-Spektren konnten nur vom Kupferkomplex 2 erhalten werden. Des weiteren verkürzt 2 die Relaxationszeiten T1 und T2 der Kernspinzustände von 1H und 17O des Wassers. Aus der Temperaturabhängigkeit der Relaxationszeitverkürzung wird eine Aktivierungsenergie berechnet, die zur Beschreibung der Reorientierung des Kupferkomplexes in der „Wassermatrix“ dient.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926140816
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  • 8
    Electronic Resource
    Electronic Resource
    5-Hydroxy-1-phosphabicyclo[3.3.1]nonanProfessor Heinrich Nöth zum 65. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 989-992 
    Details
    ISSN: 0044-2313
    Keywords: Bicyclic organophosphorus compounds ; intramolecular hydrophosphorylation ; 1-phosphabicyclo[3.3.1]nonanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 5-Hydroxy-1-phosphabicyclo[3.3.1]nonaneA new approach to 1-phosphabicyclo[3.3.1]nonane compounds involves free-radical cyclization of 4-trimethylsilyloxy-4-phosphinomethyl-hepta-1.6-diene synthesized by the reaction of 2.2-diallyl-oxirane with KPH2 followed by trimethylsilylation. Trimethylsilyl groups are easily cleaved in boiling methanol forming 5-hydroxy-1-phosphabicyclo[3.3.1]nonanes. Silylated and desilylated bicyclic compounds are characterized by n.m.r. and i.r. data.
    Notes: Die Reaktion von 2,2-Diallyl-oxiran mit KPH2 zu 4-Hydroxy-4-phosphinomethyl-hepta-1,6-dien, das nach Bildung des Trimethylsilylethers radikalisch cyclisiert wird, stellt einen neuen Zugang zum 1-Phosphabicyclo[3.3.1]nonan-System dar. Die Titelverbindung wird durch Abspaltung der Trimethylsilylgruppe in siedendem Methanol gebildet. Die silylierten und entsilylierten bicyclischen Verbindungen werden durch NMR- und IR-Daten charakterisiert.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190605
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  • 9
    Electronic Resource
    Electronic Resource
    γ-anti-Effekt an 1-Phosphabicyclo[3.3.1]nonan-Derivaten mit Substituenten am Phosphor. Synthese und Struktur von Pentacarbonyl(1-phosphabicyclo[3.3.1]nonan)chrom (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 127-134 
    Details
    ISSN: 0044-2313
    Keywords: γ-anti effect ; 1-phosphabicyclo 3.3.1 nonane derivatives ; pentacarbonylchromium complex ; structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: γ-Anti Effect in 1-Phosphabicyclo[3.3.1]nonane Derivatives with Substituents at Phosphorus. Synthesis and Structure of Pentacarbonyl(1-phosphabicyclo[3.3.1]nonane) ChromiumIn 1-phosphabicyclo[3.3.1]nonane derivatives of the composition C8H15P(X) the CC-conformation always dominates. Changes in the chemical shifts of the bridge-head carbon atom C(5) in the 13C-NMR spectrum are only originated by the electronic influence of the substituent X at the phosphorus centre. Based on a homogeneous interpretation of the electronic interactions and with regard to Pearsons's definition of electronegativity the electronegativities of substituents at the phosphorus atom X = Cr(CO)5, Fe(CO)4, and Ni(CO)3 are estimated. These groups are placed in antiperiplanar orientation to the carbon atom C(5).The molecular structure of (1-phosphabicyclo[3.3.1]-nonane) Cr(CO)5 3 was elucidated by X-ray diffraction analysis. The molecule features the 1-phosphabicyclononane ligand in the CC-conformation, which has a nearly undistorted Cr(CO)5 unit coordinated to the phosphorus atom (d Cr—P = 2.368(1) Å).
    Notes: Bei 1-Phosphabicyclo[3.3.1]nonan-Derivaten C8H15P(X) dominiert stets die CC-Konformation. Änderungen der chemischen Verschiebung des C(5)-Brückenkopfatoms im 13C-NMR-Spektrum werden alleine durch den elektronischen Einfluß des Substituenten X am Phosphoratom hervorgerufen. Auf der Grundlage einer einheitlichen Interpretation der elektronischen Wechselwirkungen und unter Anwendung des Elektronegativitätsbegriffs von Pearson konnte die Elektronegativität der in antiperiplanarer Position zu C(5) stehenden Phosphorsubstituenten X = Cr(CO)5, Fe(CO)4, Ni(CO)3 abgeschätzt werden.Die Molekülstruktur von (1-Phosphabicyclo[3.3.1]-nonan) Cr(CO)5 (3) wurde mittels Röntgenbeugung ermittelt. Das Molekül zeigt das Bild eines 1-Phosphabicyclo[3.3.1]nonans in der CC-Konformation, an dessen Phosphoratom eine nahezu unverzerrte Cr(CO)5 Einheit (d Cr—P = 2,368(1) Å) koordiniert ist.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926100121
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  • 10
    Electronic Resource
    Electronic Resource
    NMR-spektroskopische Untersuchungen an Fluoro-diaza-diphosphetidinen und Fluoro-λ5-monophosphazenen (1987)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 544 (1987), S. 225-231 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N.M.R. Investigations of Fluorodiazadiphosphetidines and Fluoro-λ5-monophosphazenesThe 19F and 31P n.m.r. data of 37 fluorodiazadiphosphetidines [RR′PF—NC6H4X]2, and 62 fluoro-λ5-monophosphazenes, RR′PF=NC6H4X, are submitted. In the case of tetrafluorodiazadiphosphetidines, [RPF2—NC6H4X]2, an intramolecular exchange of the fluorine atoms at phosphorus has to be concluded from the n.m.r. data. The influence of the substituents R and X on the n.m.r. parameters is discussed using simple models of molecular structure.
    Notes: Es werden die 19F- und 31P-NMR-Daten von 37 Fluorodiazadiphosphetidinen, [RR′PF—NC6H4X]2, und 62 Fluoro-λ5-monophosphazenen, RR′PF=NC6H4X, mitgeteilt. Aus ihnen muß für die Tetrafluorodiazadiphosphetidine, [RPF2—NC6H4X]2, auf einen intramolekularen Positionswechsel der Fluoratome am Phosphor geschlossen werden. Der Einfluß der Substituenten R und X auf die NMR-Parameter wird anhand einfacher Modelle der Molekülstruktur diskutiert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19875440124
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