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  • 1
    Electronic Resource
    Electronic Resource
    The Interaction between Amminehalocobalt(III) Cations and Polythionate Anions: Hydrogen-Bonding Patterns and S-S Bond Cleavage Reactions (2000)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 2000 (2000), S. 189-193 
    Details
    ISSN: 1434-1948
    Keywords: Cobalt(III) ; Dithionate ; Trithionate ; Sulfato ligand ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Crystal structures of amminehalocobalt(III) compounds with di- or trithionate anions have been determined in order to know whether they interact to adopt specific molecular packing patterns and whether di- and trithionate anions undergo the S-S bond cleavage reactions as has been found for the S4O62- ion. In the structures of p-[Co(tren)(NH3)Cl]S2O6·H2O (1) and t-[Co(tren)(NH3)Cl]S2O6 (2), the configurational differences in the cations dictate the hydrogen-bonding pattern with the dithionate anion to lead to racemic structures. cis-[Co(en)2(NH3)Br]S3O6 (3) also crystallizes in a racemic space group P21/c in which the ions form a macrocyclic hydrogen-bonded network. Aqueous solutions of S3O62- and p-[Co(tren)(NH3)Cl]2+ produce p-[Co(tren)(NH3)(OSO3)]ClO4 (4) which is believed to be derived from the hydrolytic cleavage of S-S bond in the trithionate anion. These results reinforce our previous observation of the S-S cleavage reactions for the tetrathionate anion.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Syntheses of Metal Carbonyls, XVI1). Metal-Metal Multiple Bonds: Synthesis, Crystal and Molecular Structure of Tri-μ-carbonyl-bis[(η5-pentamethylcyclopentadienyl)manganese](Mn ≡ Mn) - The First Manganese-Manganese Triple Bond (1984)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 117 (1984), S. 434-444 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metallcarbonyl-Synthesen, XVI1). Metall-Metall-Mehrfachbindungen: Synthese, Molekül- und Kristallstruktur von Tri-μ-carbonylbis([η5-pentamethylcyclopentadienyl)mangan](Mn ≡ Mn) - die erste Mangan-Mangan-DreifachbindungPhotolyse des Halbsandwich-Mangan-Komplexes (η5-C5Me5)Mn(CO)3 (1) in Tetrahydrofuran (THF) führt ohne Nebenreaktionen zum Solvenskomplex (η5-C5Me5)Mn(CO)2(THF) (2). Dieser ist im festen Zustand im deutlich unter 0°C liegenden Temperaturbereich haltbar, erleidet aber spontane CO-Eliminierung bei Raumtemperatur; dabei bildet sich der neue Zweikernkomplex (η5-C5Me5)2Mn2(μ-CO)3 (3). Während Elementaranalyse, Infrarot- und Massenspektren sowie die 1H- und 13C-NMR-Spektren dieser Verbindung eine hochsymmetrische dreifach Carbonylverbrückte Struktur zuweisen, stützt eine Einkristall-Röntgenstrukturanalyse das Vorliegen der ersten bisher bekannten Mangan-Mangan-Dreifachbindung (dMn - Mn 217.0(1) pm). Eine verbesserte Darstellung von Tricarbonyl(η5-pentamethylcyclopentadienyl)mangan (1) wird beschrieben.
    Notes: Photolysis of the manganese half-sandwich complex (η5-C5Me5)Mn(CO)3 (1) in tetrahydrofuran (thf) cleanly yields the solvent complex (η5-C5Me5)Mn(CO)2(thf) (2). Compound 2 is stable as solid at temperatures well below 0°C but undergoes spontaneous elimination of carbon monoxide at ambient temperature with concomitant formation of the novel dinuclear complex (η5-C5Me5)2-Mn2(μ-CO)3 (3). While elemental analysis, infrared and mass spectroscopy as well as the 1H NMR and 13C NMR spectra unequivocally demonstrate this compound to adopt a highly symmetrical triply carbonyl-bridged structure, a single-crystal X-ray diffraction study supports the presence of the first triple bond between manganese atoms (dMn - Mn 217.0(1) pm). An improved synthesis of tricarbonyl(η5-pentamethylclopentadienyl)manganese (1) is also described.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19841170203
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  • 3
    Electronic Resource
    Electronic Resource
    Multiple bonds between main group elements and transition metals, III. Synthesis, X-ray crystal and molecular structure of μ-germanium-bis[dicarbonyl(η5-pentamethylcyclopentadienyl)-manganese], μ-Ge-[(η5-C5Me5)Mn(CO)2]2 (1985)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 118 (1985), S. 340-347 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mehrfachbindungen zwischen Hauptgruppenelementen und Übergangsmetallen, III Synthese, Einkristall- und Molekülstruktur von μ-Germanium-bis[dicarbonyl(η5-pentamethylcyclopentadienyl)manganl], μ-Ge-[(η5-C5Me5)Mn(CO)2]2Die Titelverbindung 3 wurde nach der Hydrid-Methode durch Behandlung des Solvens-Komplexes (η5-C5Me5)Mn(CO)2(THF) (THF = Tetrahydrofuran) mit Monogerman, GeH4, in Gegenwart von Schwefelsäure synthetisiert. Eine Röntgenstrukturanalysse weist das Vorliegen zweier konformationsisomerer Moleküle im Kristall nach (C/c, monoklin). Bezüglich des streng linearen Mn—Ge—Mn-Gerüsts stehen zwei Carbonyl-Gruppen annähernd auf Deckung, während die anderen beiden anti-Konformation besitzen. Die äquimolar in der Elementarzelle vorlienanden enantiomeren Konformeren leiten sich geometrisch voneinander durch 180°-Drehung einer (η5-C5Me5)Mn(CO)2-Baugruppe um den Mn, Ge, Mn-Vektor ab. Die Mangan  -  Germanium-Bindungslängen betragen 2.18(2) Å (Mittelwert) und weisen damit erheblichen Mehrfachbindungscharakter auf.
    Notes: The title compound 3 has been synthesized along the hydride route by treatment of the solvent complex (η5-C5Me5)Mn(CO)2(THF) (THF = tetrahydrofuran) with monogermane, GeH4, in the presence of sulfuric acid. A single-crystal X-Ray structural analysis revealed two conformers of 3 being present in the solid state in a 1:1 ratio (C2/c, monoclinic). Pairs of carbonyl groups almost eclipse each other, while the remaining two CO ligands an exhibit an anti-conformation relative to the strictly linear Mn—Ge—Mn framework. Both enantiomeric conformers are geometrically related by a 180°-rotation of a (C5Me5)Mn(CO)2 fragment around the Mn, Ge, Mn vector. The manganese  -  germanium bond lenghts average 2.18(2) Å and thus correspond to considerable multiple bonding between these atoms.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19851180131
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  • 4
    Electronic Resource
    Electronic Resource
    Asymmetrische Katalysen, V. Enantioselektive Aminosäuresynthese durch Hydrierung prochiraler Olefine mit Rh-Komplexen des neuen optisch aktiven chelatbildenden Phosphans Norphos (1981)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 114 (1981), S. 1137-1149 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Asymmetric Catalyses, V. Enantioselective Amino Acid Synthesis by Hydrogenation of Prochiral Olefins with Rh-Complexes of the New Optically Active Chelating Phosphane NorphosRacemic bicyclo[2.2.1]hept-5-en-2,3-diylbis(diphenylphosphane oxide), Norphos, can be resolved with (-)-di-O0-benzoyltartaric acid, (-)-DBW. The X-ray structure analysis of the diastereomer (-)-Norphos/(-)-DBW, which is less soluble in ethanol, exhibits strong hydrogen bonds between the carboxylic groups of DBW and the PO groups. The bonding of the DBW-carboxylic groups to different Norphos units leads to the formation of infinite close-packed chains. From the internal comparison with (-)-DBW the absolute configuration follows as (2R, 3R) for (-)-Norphos. The chelating phosphanes (+)-and (-)-Norphos, obtained by SiHCl3-reduction of (+)-and (-)-Norphos, respectively, afford neutral and cationic Rh-complexes which, with H2 at room temperature and atmospheric pressure within a few hours, give quantitative hydrogenation of α-(acetylamino)cinnamic acid, α-(acetylamino)acrylic acid and Dopa precursors. The optical yields very between 79 and 97%.
    Notes: Racemisches Bicyclo[2.2.1]hept-5-en-2,3-diylbis(diphenylphosphan-oxid), Norphos, kann mit Hilfe von (-)-Di-O-benzoylweinsäure, (-)-DBW, optisch gespalten werden. Die Röntgenstrukturanalyse des in Ethanol schwerlöslichen Diastereomeren (-)-Norphos/(-)-DBW zeigt starke Wasserstoffbrücken zwischen den Carboxylgruppen der DBW und den PO-Gruppierungen. Die Bindung der DBW-Carboxylgruppen an verschiedene Norphos-Einheiten führt zur Ausbildung unendlicher dicht gepackter Ketten. Aus dem internen Vergleich mit (-)-DBW folgt für (-)-Norphos die absolute Konfiguration (2R, 3R). Die durch SiHCl3-Reduktion von (+)-bzw. (-)- Norphos erhaltenen chelatbildenden Phosphane (+)-bzw. (-)-Norphos ergeben in neutralen und kationischen Rh-Komplexen bei der Hydrierung von α-(Acetylamino)zimtsäure, α-(Acetylamino)acrylsäure und Dopa-Vorstufen unter Normalbedingungen in wenigen Stunden quantitativ Aminosäurederivate mit optischen Ausbeuten zwischen 79 und 97%.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19811140331
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  • 5
    Electronic Resource
    Electronic Resource
    Transition metal methylene complexes, VII. Studies on metal-metal bonds, V. Preparation and molecular structure of a carbonylcobalt complex containing a novel carbocyclic μ-methylene ligand (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 1377-1384 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Übergangsmetall-Methylen-Komplexe, VII Studien über Metall-Metall-Bindungen, V. Darstellung und Molekülstruktur eines Carbonylcobalt-Komplexes mit einem neuartigen carbocyclischen μ-Methylen-LigandenDicarbonyl(η5-cyclopentadienyl)cobalt (1) reagiert mit 2-Diazo-1,3-dioxoindan (2) unter thermischen Bedingungen (siedendes Benzol) unter Bildung des zweikernigen Cobalt-Komplexes 3, der das von 2 abgeleitete Carben als Brückenliganden enthält. Eine Röntgenstrukturanalyse wies nach, daß die beiden Cyclopentadienyl-Ringe ebenso wie die beiden Carbonyl-Gruppen trans-Positionen zueinander einnehmen. Trotz seiner vier Bindungspartner weist das Methylen-Kohlenstoffatom eine sehr stark verzerrte tetraedrische Konfiguration auf [∢Co(1)—C(3)—Co(2): 79.0(1)°, ∢C(4)—C(3)—C(11): 104.3(3)°]. Der Cobalt-Cobalt-Abstand beträgt 247.5(1) pm; die Abstände und Winkel der Co—C(C5H5)- sowie Co—C(CO)-Bausteine sind normal. Das μ-1,3-Dioxoindan-2-yliden-Gerüst ist entlang der Verbindungslinie zwischen den beiden Carbonyl-Kohlenstoffatomen des Dion-Systems um 2° abgewinkelt.
    Notes: Dicarbonyl(η5-cyclopentadienyl)cobalt (1) reacts with 2-diazo-1,3-dioxoindane (2) under thermal conditions (boiling benzene) to yield the dinuclear cobalt complex 3 which contains the carbene derived from 2 as a bridging ligand. An x-ray diffraction study proved that both the cyclopenta-dienyl rings are oriented trans to each other, which is also true for the two metal-carbonyl groups. While four-bonded, the methylene carbon is highly distorted from tetrahedral geometry [∢Co(1)—C(3)—Co(2): 79.0(1)°, ∢C(4)—C(3)—C(11): 104.3(3)°]. The cobalt  -  cobalt distance is 247.5(1) pm and the Co—C(C5H5) and Co—C(CO) distances and angles are normal. The μ-1,3-dioxoindane-2-ylidene backbone is bent by 2° along the vector joining the two carbonyl carbon atoms of the dione system.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130416
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  • 6
    Electronic Resource
    Electronic Resource
    Metallcarbonyl-Synthesen, X: Synthese neuer Niob- und Tantal-Halbsandwichkomplexe. Molekülstruktur der Stammverbindung (η5-C5H5)Nb(CO)4 (1981)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 114 (1981), S. 3558-3571 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metalcarbonyl Syntheses, X: Synthesis of New Niobium and Tantalum Halfsandwich Complexes. Molecular Structure of the Parent Compound (η5-C5H5)Nb(CO)4The halfsandwich complexes (η5-C5H4CH3)Nb(CO)4 (3a), [η5-C5(CH3)5]Nb(CO)4 (3b), (η5-C5H4CH3)Ta(CO)4 (3c), and [η5-C5(CH3)5]Ta(CO)4 (3d) are accessible by reductive high-pressure carbonylation of the corresponding NbV- and TaV precursors (η5-C5R4R′)MCl4 (2a-d). Successive introduction of methyl groups in the cyclopentadienyl ring facilitates the reduction of the halogeno complexes 2a-d; moreover, the niobium complexes are more susceptible to reduction than their tantalum counterparts. Upon photolysis of the carbonyl complexes 3a-d in tetrahydrofuran, the solvens complexes of type (η5-C5R4R′)M(CO)3(THF) (4a-d) are generated. The parent compound (η5-C5H5)Nb(CO)4 (1) has a regular square-pyramidal structure as shown by X-ray analysis.
    Notes: Die Halbsandwich-Komplexe (η-5C5H4CH3)Nb(CO)4 (3a), [η5-C5(CH3)5]Nb(CO)4 (3b), (η5-C5H4CH3)Ta(CO)4 (3c) und [η5-C5(CH3)5]Ta(CO)4 (3d) sind durch reduzierende Hochdruckcarbonylierung der entsprechenden NbV-bzw. TaV-vorstufen (η5-C5R4R′)MCl4 (2a-d) synthetisierbar. Die Reduzierbarkeit der Halogeno-Komplexe, 2a-d, wird durch sukzessive Einführung von Methyl-Substituenten in den Cyclopentadienyl-Ring erleichtert und ist bei den Niob-Verbindungen mit milderen Reduktionsmitteln als bei den analogen Tantal-Komplexen möglich. Bei der Photolyse von 3a-d in Tetrahydrofuran entstehen die Solvens-Komplexe (η5-C5R4R′)M(CO)3(THF) (4a-d). Die Stammsubstanz (η5-C5H5)Nb(CO)4 (1) wurde röntgenstrukturanalytisch untersucht und besitzt eine unverzerrt tetragonal-pyramidale Molekülstruktur.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19811141109
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  • 7
    Electronic Resource
    Electronic Resource
    Struktur und absolute Konfiguration eines optisch aktiven quadratisch-pyramidalen Molybdän-KomplexesHerrn Professor Helmut Behrens zum 60. Geburtstag gewidmet (1975)
    Weinheim : Wiley-Blackwell
    Zeitschrift für die chemische Industrie 87 (1975), S. 379-379 
    Details
    ISSN: 0044-8249
    Keywords: Chemistry ; General 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/ange.19750871004
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  • 8
    Electronic Resource
    Electronic Resource
    Crystal Structures of Oxalato and Oxamido Polyaminecobalt(III) Complexes Produced by Hydrolysis of Monooxamide (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 723-728 
    Details
    ISSN: 1434-1948
    Keywords: Monooxamide ; Amide hydrolysis ; Cobalt(III) ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions of sodium monooxamide (H2NCOCO2Na) with trans-[Co(en)2Cl2]Cl, trans-[Co(3,2,3-tet)Cl2]Cl (3,2,3-tet = 1,5,8,12-tetraazadodecane), cis-α-[Co(trien)Cl2]Cl and [Co(tren)Cl2]Cl result in the formation of [Co(en)2(ox)]Cl · 4H2O (1), cis-β-[Co(3,2,3-tet)(ox)]Cl· 4 H2O (2), cis-α-[Co(trien)(ox)]Cl · 2 H2O (3), and [Co(tren)(ox)](ClO4) · 0.5 H2O (4) respectively, implying a hydrolytic cleavage of the amide bond. [Co(tren)(O,O′-oxam)]Cl2 · 2 H2O (5) (oxam = H2NCOCO2-) and p-[Co(tren)(NH3)(O-oxam)]Cl2 (6) have also been prepared in order to give mechanistic information for the hydrolysis of monooxamide. Crystal structures of the products are reported and possible pathways for the hydrolysis reactions are discussed.
    Additional Material: 5 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    Syntheses of K[Co(tren)(NH3)(SO4)](S4O6)·2(H2O) and of [cis-α-Co(trien)(NH3)Cl](S5O6) - Compounds Produced by Hydrolytic Cleavage of Sulfur-Sulfur Bonds of the Tetrathionate Anion (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 717-722 
    Details
    ISSN: 1434-1948
    Keywords: Tetrathionates ; Pentathionates ; Sulfato ligands ; Cobalt(III) complexes ; Thiobacillus ferrooxidans ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: K[Co(tren)(NH3)(SO4)](S4O6)·2(H2O) (1) and [cis-α-Co-(trien)(NH3)Cl](S5O6) (2) have been prepared unexpectedly while attempting to obtain crystals suitable for X-ray diffraction of [Co(tren)(NH3)Cl](S4O6) (3) and of [cis-Co(trien)(NH3)Cl](S4O6) (4), respectively. 1 is derived from 3 by hydrolysis of the tetrathionate anion resulting in a sulfato moiety which displaces the chloro ligand from the coordination sphere of the metal center. 2 is derived from 4 by hydrolysis of the tetrathionate anion followed by reformation into pentathionate anion and H2S, as described in previous chromatographic work by Steudel. Compounds 1 and 2 have been characterized by elemental analyses and by single-crystal X-ray diffraction studies.
    Additional Material: 5 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Röntgen-Strukturanalyse von N,N′-Dimethyl-3,6-epitetrathio-2,5-piperazindion1. Mitteilung zur Kristallstruktur von 2,5-Piperazindionen mit Schwefelbrücken zwischen C-3 und C-6.  -  Ein Teil der Arbeit (B. R. D. und I. B.) wurde von der U. S. Atomic Energy Commission unterstützt.  -  Wir danken Mr. John Smith für technische Mitarbeit und Dr. H. Poisel für die Herstellung der Kristalle. (1972)
    Weinheim : Wiley-Blackwell
    Zeitschrift für die chemische Industrie 84 (1972), S. 640-641 
    Details
    ISSN: 0044-8249
    Keywords: Chemistry ; General 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/ange.19720841308
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