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  • 1
    Electronic Resource
    Electronic Resource
    Trapping reactions of sulfenes generated from sulfonic acid derivatives and bases, 1. Cyclopentadiene, methylcyclopentadiene and 1,2,3,4-tetraphenylcyclopentadiene used as sulfene scavengers. [4 + 2] cycloaddition reactions and sulfonylations (1995)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1995 (1995), S. 2137-2149 
    Details
    ISSN: 0947-3440
    Keywords: Sulfenes ; [4 + 2] Cycloaddition ; Cyclopentadiene ; (+)-10-Camphorsulfonyl chloride ; Sulfonyl cyclopentadienides ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The bulky sulfenes generated in situ from (+)-10-camphor-, 10-camphane-, and 2-methyl-2-phenylpropanesulfonyl chloride (1a-c) and Et3N can be trapped by cyclopentadiene to give the [4 + 2] cycloadducts 6a-c. The mixture of endo-6a and exo-6a (no other diastereomers) is formed by complete asymmetric induction. In MeCN solution additionally the 1,3-di- and 1,2,4-trisulfonylated cyclopentadienides 4a-c and 5a (X-ray analysis) + 5c were obtained. On acidification, 4a and 5a were transformed into the pentafulvenoid derivatives 8a, 9a, 10a. The reaction of (+)-10-camphorsulfonyl chloride (1a)/Et3N with 1,2,3,4-tetraphenylcyclopentadiene afforded the sulfonylated product 11a, with 2-methylcyclopentadiene 50% endo-12a (X-ray analysis) and 10% exo-12a. From cyclopentadiene and the more electrophilic cyanosulfene (2e) and mesylsulfene (2f, X = Me), generated in situ from cyanomethanesulfonyl chloride (1e)/Et3N and from mesyl chloride/Et3N, the [4 + 2] cycloadducts 6e and 6g were obtained. Similarly, methanedisulfonyl dichloride (1f, X = Cl)/Et3N afforded stereospecifically by two subsequent [4 + 2] cycloadditions the spirodisulfone 16 (X-ray analysis).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.1995199512300
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  • 2
    Electronic Resource
    Electronic Resource
    Trapping reactions of sulfenes generated from sulfonic acid derivatives and bases, 2. [4 + 2] cycloadditions of 1,2,3,4,5-pentamethylcyclopentadiene and 1,3-diphenylbenzo[c]furan with sulfenes (1995)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1995 (1995), S. 2151-2163 
    Details
    ISSN: 0947-3440
    Keywords: 1,2,3,4,5-Pentamethylcyclopentadiene ; 1,3-Diphenylbenzo[c]furan ; Sulfenes ; [4 + 2] Cycloaddition ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sulfenes 2a-o, generated in situ from sulfonyl chlorides and Et3N, are trapped by 1,2,3,4,5-pentamethylcyclopentadiene (6) to give [4 + 2] cycloadducts 8a-o containing the 7-methyl group in anti position. With mesylsulfene (7), formed in situ from mesyl chloride/Et3N in MeCN solution, the [4 + 2] cycloaddition to endo/exo- 9 (X-ray analyses) is accompanied by a [2 + 2] cycloaddition to 10 (X-ray analysis). (+)-10-Camphorsulfonyl chloride/Et3N afforded only two (and no more) diastereomeric [4 + 2] cycloadducts (endo/exo-8d). Et3N can be replaced by Me3N, N,N,N′,N′-tetramethylnaphthalene- 1,8-diamine or NaH, the sulfonyl chlorides to a limited extent by sulfonyl fluorides, sulfonic acid anhydrides or aryl esters. Formation of 8p from 6 and dichloromethanesulfonyl chloride requires NaH or AgNO3 or tertiary amine/AgNO3. N-(2-Methyl-1-propenyl)pyrrolidine is more reactive than 6 in trapping sulfene 2a. 6, however, is a more efficient sulfene scavenger than 1,3-diphenylbenzo[c]furan (19), which reacts with sulfene 2d by [4 + 2] cycloaddition and SO2 extrusion to give ketone 21d in only 18% yield.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.1995199512301
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  • 3
    Electronic Resource
    Electronic Resource
    Intramolecular Long-Range Exchange Coupling in Dinuclear Copper(II) Complexes with Cu…Cu Separations Greater than 10Å (1995)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 1 (1995), S. 583-593 
    Details
    ISSN: 0947-6539
    Keywords: bridging ligands ; coordination ; copper compounds ; exchange coupling ; magnetic properties ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Magnetic long-range exchange coupling between two unpaired electrons of two copper(II) ions in a square-pyramidal ligand environment (dx2-y2)1, which are rigidly separated by 〉 10 Å by an organic spacer ligand (e.g., a μ-dicarboxylato ligand) has been systematically studied. The following complexes have been synthesized: [{LCu(OH2)}2(μ-terephthalato)](ClO4)2 (I), [LCuII(OH2)(benzoato)](CIO4) (2), [{LCuII(NCS)}2(μ-terephthalato)]-2 CH3OH (3), [{LCuII(NCS)}2 (μ-4,4′-oxybisbenzoato)] · 3 CH3OH (4), [{LCuII(OH2)}2 (μ-tetrafluoroterephthalato)](CIO4)2 (5), [{LCuII(OH2)}2{LCuII}2 (μ-tetrafluorobenzoato)3](CIO4)2 · 6 H2O (6), [{LCuII(OH2)}2 (μ-biphenyl-4,4′-dicarboxylato)](CIO4)2 (7), [LCuII(μ-biphenyl-4,4′-dicarboxylato)]n (HZO)2n (8), [{LCuII(NCS)}2 (μ-biphenyl-4.4′-dicarboxylato)] (9), [{LCu(OH2)}2, (μ-trans,trans-2,4-hexadien1,6-dicarboxylato)] (CIO4)2 (10) (L = 1,4,7-trimethyl-1,4,7-triazacyclononane). Complexes 1, 2, 3, 4, and 6 have been characterized by X-ray crystallography; the structure of 1 has been described previously.[15] Temperature-dependent magnetic susceptibility data for all complexes have been measured over the range 2.0-298 K. In complexes 2, 3, 4, 6, 8, and 9 only very weak, if any, intermolecular antiferromagnetic or, in the case of 6, ferromagnetic coupling has been observed (|J|≤2cm-1; H= -2JS1 S2 S1 = S2 = 1/2). In contrast, in complexes 5 (2J=-80cm-1), 7(2J=-62cm-1), and 10 (2J = -100 cm-1) relatively strong intramolecular antiferromagnetic exchange coupling has been detected. The intramolecular Cu…Cu separation is 11.3Å in 5, 15.6 Å in 7, and approximately 12.0Å in 10. These data demonstrate that intramolecular antiferromagnetic exchange coupling of considerable magnitude is possible over distances 〉 15 Å, provided that the effective magnetic orbitals are favorably aligned.
    Additional Material: 16 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chem.19950010904
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  • 4
    Electronic Resource
    Electronic Resource
    Novel inorganic cage structures based on ass ligands and cyclopentadienylruthenium groups (1997)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 3 (1997), S. 57-61 
    Details
    ISSN: 0947-6539
    Keywords: clusters ; ruthenium ; sandwich complexes ; arsenic sulfides ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of [Cp(*)2Ru2-(CO)4] [a: Cp(*) = Cp* (η5-C5Me5); b: Cp(*) = Cpx (η5-C5Me4Et)] with β-realgar in boiling n-decane gives [Cp(*)2Ru2-As4S4] (1a,b). in good yields along with some [Cp(*)2Ru2-As4S2] (2a,b). According to X-ray diffraction analyses of 1b and 2a, their structures belong to two different types of inorganic clusters. Whereas 1b has a cage structure in which the [Cp(*)2Ru2 unit is inserted into the As4S4] cradle, 2a has a sandwich structure in which two coplanar η2-As4S ligands and the Cp* ligands are oriented parallel to one another. Analysis of the As-S connectivity in the core of 1 b reveals a structural relationship to the extremely rare form of arsenic sulfide As4S4(II), and not to the metastable high-temperature form β-As4S4 used in the synthesis. At lower temperatures (60, 115°C) formation of CO-containing products is observed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chem.19970030110
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  • 5
    Electronic Resource
    Electronic Resource
    Die Kristall- und Molekülstruktur von 1,4-Dimethyl-9H-tribenzo-[a.c.e]cyclohepten-9e-ol (1979)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 112 (1979), S. 1316-1319 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of 1,4-Dimethyl-9H-tribenzo[a.c.e]cyclohepten-9e-oIThe conformation of the title compound 1 and the quasi-equatorial position of the hydroxyl group on C-9 were established by X-ray analysis. The seven-membered ring of the crystalline compound 1 has a steep boat form with angles of α = 57° and β = 43° and shows Cs-symmetry. Further structural parameters of 1 are discussed.
    Notes: Die Konformation der Titelverbindung 1 und die quasi-äquatoriale Lage der Hydroxylgruppe an C-9 wurden durch Röntgenstrukturanalyse gesichert. Der Siebenring des kristallisierten Carbinols 1 besitzt eine steile Bootform mit den Winkeln α = 57°C und β = 43°C und zeigt Cs-Symmetrie Weitere Abstands- und Winkelparameter von 1 werden diskutiert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19791120425
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  • 6
    Electronic Resource
    Electronic Resource
    Neue μ-Hydroxo-Übergangsmetallkomplexe, I. Darstellung und Struktur des trans-Diaqua-di-μ-hydroxo-bis[(1,4,7-triazacyclononan)cobalt(III)]-Kations; Kinetik und Mechanismus seiner Bildung (1979)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 112 (1979), S. 2220-2230 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Novel μ-Hydroxo-Transition Metal Complexes, I. Preparation and Crystal Structure of the trans-Diaqua-di-μ-hydroxo-bis[(1,4,7-triazacyclononane)cobalt(III)]Cation; Kinetics and Mechanism of its FormationThe binuclear tri-μ-hydroxo-bis[(1,4,7-triazacyclononane)cobalt(III)] cation (1) is prepared. In acidic solutions 1 forms the trans-diaqua-μ-hydroxo-bis[(1,4,7-triazacyclononane)cobalt(III)] cation (2), the structure of which has been established by single crystal X-ray diffraction. The equilibration kinetics of the first hydroxo-bridge cleavage of the triply-bridged complex 1 have been studied. A mechanism is proposed involving cis-trans isomerization of 2 as the rate determining step. The mechanism is consistent with all (including previously published) experimental data for the OH-bridge cleavage processes of tri-μ-hydroxo-bis[aminecobalt(III)] complexes.
    Notes: Das zweikernige Tri-μ-hydroxo-bis[(1,4,7-triazacyclononan)cobalt(III)]-Kation (1) wird dargestellt. In saurer Lösung entsteht daraus das trans-Diaqua-di-μ-hydroxo-bis[(1,4,7-triazacyclononan)cobalt(III)]-Kation (2), dessen Struktur röntgenographisch bestimmt wurde. Die Kinetik der Gleichgewichtseinstellung der Spaltung der ersten OH-Brücke von 1 wurde gemessen. Es wird ein Mechanismus vorgeschlagen. Bei dem die cis-trans-Isomerisierung von 2 den geschwindigkeitsbestimmenden Schritt darstellt, und der alle(auch frühere) experimentelle Daten der OH-Brückenspaltung sowie die Bildung von Tri-μ-hydroxo-bis[amincobalt(III)]-Komplexen widerspruchsfrei deutet.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19791120629
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  • 7
    Electronic Resource
    Electronic Resource
    Chemie der Übergangsmetall-Heterocyclen-Komplexe, I. Über eine elektrophile Pyrrolyl-Eliminierung aus Azacymantren (1979)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 112 (1979), S. 2423-2435 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemistry of Transition Metal Heterocyclic Complexes, I. Electrophilic Pyrrolyl Elimination from AzacymantreneTricarbonyl(η5-pyrrolyl)manganese (2) reacts with diphenylketene in boiling tetrahydrofuran/water to yield the three-nuclear complex 4 as well as N-(diphenylacetyl)pyrrole (3). The configuration of 4 as a complex of the type fac-(CO)3Mn(L1)2L2 (L1 = 2; L2 = diphenylacetato-O) is deductable from the NMR spectra and has been proved by an X-ray structural determination for the crystalline state. - The novel N-azacymantrene complex (η5-C5H5)Mn(CO)2[(s̰-C4H4N)Mn(CO)3] (6) can be synthesized by ligand exchange on (η5-C5H5)Mn(CO)3 (1). Based on its IR and NMR data, 2 possesses a high s̰-donor/π-acceptor ratio when acting as a monodentate nitrogen ligand.
    Notes: Tricarbonyl(η5-pyrrolyl)mangan (2)ergibt bei der Reaktion mit Diphenylketen in siedendem Tetrahydrofuran/Wasser den Dreikern-Komplex 4 sowie N-(Diphenylacetyl)pyrrol (3). Die Konfiguration von 4 als Komplex vom Typ fac-(CO)3Mn(L1)2L2 (L1 =2; L2 = Diphenylacetato-O) ist aus den NMR-Spektren ableitbar und für den kristallinen Zustand durch Röntgenstrukturanalyse gesichert. - Der neuartige N-Azacymantren-Komplex (η5-C5H5)Mn(CO)2[(s̰-C4H4N)Mn(CO)3] (6) läßt sich durch gezielten Ligandenaustausch an (η5-C5H5)Mn(CO)3 (1) synthetisieren. Aufgrund der IR- und NMR-Daten besitzt 2 in seiner Eigenschaft als einzähniger Stickstoffligand ein hohes s̰-Donor/π-Akzeptor-Verhältnis.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19791120710
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  • 8
    Electronic Resource
    Electronic Resource
    Neue μ-Hydroxo-Übergangsmetallkomplexe, III. Darstellung zweikerniger Komplexe des Rhodiums(III) mit einer μ-Acetato- und μ-Carbonato-Brücke. Die Struktur des trans-Diaqua-di-μ-hydroxo-bis[(1,4,7-triazacyclononan)rhodium(III)]-Kations (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 36-41 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Novel μ-Hydroxo-Transition Metal Complexes, III. Preparation of Binuclear Complexes of Rhodium(III) Containing a μ-Acetato- and μ-Carbonato-Bridge. The Structure of the trans-Diaqua-di-μ-hydroxo-bis[(1,4,7-triazacyclononane)-rhodium(III)] CationThe binuclear tri-μ-hydroxo-bis[(1,4,7-triazacyclononane)rhodium(III)] cation 4 has been prepared. In acidic solutions 4 forms the trans-diaqua-di-μ-hydroxo-bis[(1,4,7-triazacyclononane)-rhodium(III)] cation 3, the structure of which has been established by single crystal X-ray diffraction. 3 reacts with acetic acid to yield the μ-acetato complex 5; whereas in alkaline solutions 6 reacts with carbonate ions forming a μ-carbonato complex 7.
    Notes: Das zweikernige Tri-μ-hydroxo-bis[(1,4,7-triazacyclononan)rhodium(III)]-Kation 4 wird dargestellt. In saurer Lösung entsteht daraus das trans-Diaqua-di-μ-hydroxo-bis[(1,4,7-triazacyclononan)rhodium(III)]-Kation 3, dessen Struktur röntgenographisch bestimmt wurde. Mit Essigsäure reagiert 3 zum μ-Acetato-Komplex 5; wohingegen in alkalischer Lösung aus 6 mit Carbonat-Ionen der μ-Carbonato-Komplex 7 entsteht.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130107
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  • 9
    Electronic Resource
    Electronic Resource
    Reaktionen von Hydroxylamin mit Molybdän(VI): Synthese von (Hydroxylamido-O,N)nitrosylmolybdän-Komplexen. Die Struktur des [(Hydroxylamido-O,N)nitrosylbis(1,10-phenanthrolin)molybdän]-Kations (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 629-638 
    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 Molybdenum(VI) with Hydroxylamine: Synthesis of Some (Hydroxylamido-O,N)-nitrosylmolybdenum Complexes: The Structure of the [(Hydroxylamido-O,N)nitrosylbis(1,10-phenanthroline)molybdenum] CationMolybdenum(VI) oxoanions react with hydroxylamine in alkaline or acidic media without formation of N2, N2O, or NH3 to yield yellow solutions. Upon addition of bidentate or tridentate ligands yellow nitrosylmolybdenum complexes of the type {Mo — N = O}4 have been isolated, 1 - 4, 6. These complexes contain one or two O,N-coordinated hydroxylamido ligands (H2NO-). The molybdenum centers have the coordination number seven (pentagonal bipyramidal). The structure of (phen)[(phen)2Mo(NO)(H2NO)]I2 · H2O (7 · I2 · H2O · phen) has been determined by single crystal X-ray diffraction.
    Notes: Molybdän(VI)-Oxoanionen reagieren im sauren oder alkalischen wäßrigen Medium mit Hydroxylamin ohne Bildung von N2, N2O oder NH3 zu gelben Lösungen, aus denen durch Zugabe von zweizähnigen oder dreizähnigen Liganden gelbe Nitrosylkomplexe 1 - 4, 6 des Typs {Mo — N = O}4isoliert wurden. Alle dargestellten Verbindungen enthalten zusätzlich ein oder zwei O,N-koordinierte Hydroxylamido-Liganden (H2NO-). Die Koordinationszahl des Molybdäns ist immer sieben (pentagonal-bipyramidal). Die Struktur von (phen)[(phen)2Mo(NO)(H2NO)] I2 · H2O (7 · I2 · H2O · phen) wurde röntgenographisch bestimmt.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130221
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  • 10
    Electronic Resource
    Electronic Resource
    The Structure of an Isomeric Pair of a (Tetraamine)copper(II) Compound in the solid state and in solutionDedicated to Professor Achim Müller on the occasion of his 60th birthday (1997)
    New York, NY : Wiley-Blackwell
    Helvetica Chimica Acta 80 (1997), S. 1831-1842 
    Details
    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The template condensation of [Cu(3, 2, 3-tet)]2+ (3, 2, 3-tet = N, N″)-(ethane-1, 2-diyl)propane-1, 3-diamine with CH2O and en (en = ethane-1, 2-diamine) affords the copper(II) compounds of two isomeric tricyclic ligands in high yield. The strikingly different UV/VIS and EPR spectroscopic behavior of these two compounds, [Cu(‘syn’-L)](CIO4)2 and [Cu(‘anti’-L)](ClO4)2 · 1/2 H2O (L = 1, 4, 8, 10, 13, 15-hexaazatricyclo [13.3.1.14, 8]icosane), is analyzed by angular overlap model (AOM) calculations based on the experimentally determined solid-state structures (powder spectra) and a combination of molecular mechanics and AOM calculations (MM-AOM) for the solution-structure behavior.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/hlca.19970800607
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