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  • General Chemistry  (2,877)
  • Inorganic Chemistry  (1,375)
  • Aircraft Design, Testing and Performance
  • 1995-1999  (2,488)
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  • 1945-1949
  • 1915-1919
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  • 1991  (1,874)
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  • 1995-1999  (2,488)
  • 1990-1994  (1,874)
  • 1945-1949
  • 1915-1919
Year
  • 101
    Electronic Resource
    Electronic Resource
    2-Phosphaindolizines (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 475-480 
    Details
    ISSN: 0009-2940
    Keywords: 1,3-Azaphosphole, annulation to pyridine ; 2-Phosphaindolizines ; Pyridinium bromides, 1,2-dialkyl ; Phosphorus(III) chloride, condensation with CH2 groups ; Calculations, MNDO ; Chemistry ; Inorganic 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/cber.19911240309
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  • 102
    Electronic Resource
    Electronic Resource
    Medizinisch interessante Metallchelate, III. 99mTc-Komplexe mit vierzähnigen Dibrenzkatechin-Liganden (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 487-491 
    Details
    ISSN: 0009-2940
    Keywords: Bis[3-(2,3-dihydroxyphenoxy)propyl]amine hydrochloride ; 99mTc uptake ; Technetium, radiopharmaceutical containing ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Chelates of Medical Interest, III. - 99mTc Complexes with Tetradentate Dicatechol LigandsThe dicatechol ligand bis[3-(2,3-dihydroxyphenoxy)propyl]-amine hydrochloride, DIPACE (6), reduces the 99m[TcO4]- ion to lower valent 99mTc and subsequently forms a complex with the reduced 99mTc. The structure of benzylbis[3-(2,2-dimethyl-1,3-benzodioxol-4-yloxy)propyl]amine (4) is determined by X-ray crystallography.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240311
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  • 103
    Electronic Resource
    Electronic Resource
    Preparation and Crystal Structures of 2-Aminoethyl Phosphate Complexes of Magnesium, Calcium, and Zinc (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 509-513 
    Details
    ISSN: 0009-2940
    Keywords: 2-Aminoethyl phosphate complexes ; Magnesium complexes ; Calcium complexes ; Zinc complexes ; Hydrogen bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Crystalline magnesium, calcium, and zinc 2-aminoethyl phosphate complexes containing the monoanions PEAH⊖ have been prepared as the tetrahydrates (Ca, Zn) and the hexahydrate (Mg), and their structures determined by single-crystal X-ray methods. The structures of monoclinic Ca(PEAH)2·4 H2O and Zn(PEAH)2·4 H2O (space group C2/c) both contain polymeric chains with metal ions connected by bridging phosphate groups. The zinc atoms are in a tetrahedral environment of four oxygen atoms, while the calcium atoms are found to be hexacoordinated with two additional oxygen atoms from water molecules in axial positions. The triclinic Mg(PEAH)2·6 H2O (space group \documentclass{article}\pagestyle{empty}\begin{document}$ P\bar 1 $\end{document}) contains discrete complex units with hexacoordinate magnesium atoms octahedrally surrounded by six oxygen atoms, four of which from water molecules in the equatorial plane and two from phosphate groups in axial positions.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240315
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  • 104
    Electronic Resource
    Electronic Resource
    A Versatile Synthesis of 1,4-Dienes: Use of Vinyl Ethers as Vinyl Cation EquivalentsDedicated to Professor Karl Heinz Büchel on the occasion of his 60th birthday. (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2785-2790 
    Details
    ISSN: 0009-2940
    Keywords: Enol ether ; Allylsilane ; Bromo ether ; 1,4-Diene ; Alkoxyalkylation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The α,β-dibromo ethers 2, in situ generated from the vinyl ethers 1 and bromine, react with the allylsilanes 3 in the presence of ZnCl2 to give the β-bromo ethers 4. Treatment of 4 with Na in diethyl ether yields 1,4-dienes 5 in 62-79% overall yield.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911241222
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  • 105
    Electronic Resource
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    Small and Medium Rings, 791) 4-Azatetracyclo[3.3.0.02,8.03,6]octanes: New Hetereocycles by Addition of Sulfonyl Azides to 7-Substituted Norbornadienes - Experimental Verification of σ Interactions in the Norbornane Skeleton (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2879-2895 
    Details
    ISSN: 0009-2940
    Keywords: Cycloadditions, dipolar ; Electron-transmission spectroscopy ; Norbornane systems ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of six 7-substituted norbornadienes with seven sulfonyl azides has been investigated. The products consist of either the novel azatetracyclic system 1 or the stereoisomeric bicycles 2 or of a mixture of them. The chemical behaviour of 1 has been studied. Mechanistically the results may be rationalized within the frame of the Mazzocchi-Houk model. The theoretical predictions of this model, concerning the π*and σ* energies, were confirmed experimentally by using electron-transmission spectroscopy.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911241232
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  • 106
    Electronic Resource
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    Zur Bildung von Vinylcyclopropan- und Cyclopentenderivaten aus alkenylsubstituierten Chromcarben-Komplexen: Konkurrenz von formalen [2 + 1]- und [3 + 2]-Cycloadditionen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 957-965 
    Details
    ISSN: 0009-2940
    Keywords: Chromium complexes ; Carbene ligands ; alkenyl-substituted ; [2 + 1] Cycloaddition ; Vinylcyclopropane→cyclopentene rearrangement ; Cyclopropanes ; donor-acceptor-substituted ; Pyrrole derivatives ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Formation of Vinylcyclopropane and Cyclopentene Derivatives from Alkenyl-Substituted Chromium Carbene Complexes: Competition between Formal [2 + 1] and [3 + 2] Cycloadditions.The alkenyl-substituted chromium carbene complexes 1 - 4 were synthesized following the method of Aumann which starts from the corresponding aldehydes. At 80°C the styryl-substituted complex 1 and electron-deficient olefins smoothly provide vinylcyclopropane derivatives 6,8, 10, and 12 in good yields. On the other hand, methyl acrylate and the anisyl- and furyl-substituted vinylcarbene complexes 2 and 3 give mixtures of the expected vinylcyclopropanes and of cyclopentene derivatives. The pyrrolyl-substituted complex 4 and methyl acrylate exclusively afford the cyclopentenes 24a/b which are the result of a hitherto unprecedented formal [3 + 2] cycloaddition of the vinylcarbene complex to the olefin. However, there are strong arguments suggesting the corresponding vinylcyclopropanes as intermediates. The very smooth vinylcyclopropane→cyclopentene rearrangement probably occurs via zwitterionic intermediates that are wellstabilized by donor and acceptor substituents. Hydrolysis of 24a/b to the cyclopentanone derivatives 25a/b demonstrates that this new route to five-membered carbocycles should have synthetic potential.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240441
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  • 107
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    OrganosubstituierteBicyclen undMonocyclen aus 2,5-Dihydro-1,2,5-oxasilaboratolaten (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1017-1023 
    Details
    ISSN: 0009-2940
    Keywords: Borates, triorgano-oxy, potassium salts ; N-Lewis base - diorgano(silyloxy)boranes ; Bicyclo[2.2.1]heptanes, heteroatom-containing, diastereomeric ; P-Lewis base - triorganoboranes, monocyclic, unsaturated ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: OrganosubstitutedBicyclic and Monocyclic Compounds from 2,5-Dihydro-1,2,5-oxasilaboratolates1a)The potassium salts of the cyclic anions of (A: R, R′ = CH3; B: R = C2H5, R′ = CH3; C: R = C6H5, R′ = CH3 react with [(CH3)2NCH2]Br in THF to yield the bicyclic compounds 1a (X-ray crystal structure analysis), 1b/1b' (endo/exo-C2H5), and 1c/1c' (endo/exo-C6H5). D (R=CH3, R'=C6H5) reacts with [(CH)32NCH2]Br to form a 1:4 mixture of 1d together with the heterocycle (3d) with elimination of (CH3)2N-C3H7. - From A - D and CIP(C6H5)2 the six-membered heterocycles (2a-d) are obtained in yields of ca. 90%.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240507
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  • 108
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    Metal Complexes with Tetrapyrrole Ligands, LVIII. Zirconium(IV) and Hafnium(IV) Bisporphyrinate Double Deckers: Synthesis, Spectra, Redox Potentials, and Structure (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1051-1058 
    Details
    ISSN: 0009-2940
    Keywords: Zirconium porphyrins ; Hafnium porphyrins ; Porphyrin double deckers ; Metal bisporphyrinates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of new zirconium and hafnium bisporphyrinate double deckers M(P)2 (M=Zr, Hf; P=OEP, TPP)2,3) is described. The complexes are characterized by UV/Vis/NIR and 1H-NMR spectroscopy and cyclic voltammetry. As compared with M=Ce, the redox potentials or the energies of the nearinfrared absorption bands of the corresponding radical cations [M(P)2]+ are lower by ≍ 0.2 V or higher by ≍ 2000 cm-1, respectively, Hence, there is a stronger π-π interaction between the porphyrin ligands as compared with the cerium analogues due to the smaller ionic radii of Zr(IV) and Hf(IV). X-ray crystallography of Zr(TPP)2 confirms the sandwich-like structure of the compound and the close proximity of the porphyrin ligands.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240511
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  • 109
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    Metal Bonding by Amino Acids: Preparation and Crystal Structures of Calcium Bis-L-pyroglutamate and Lithium L-Pyroglutamate (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1083-1087 
    Details
    ISSN: 0009-2940
    Keywords: Calcium bis-L-pyroglutamate ; Lithium L-pyroglutamate ; Pyroglutamate coordination and conformation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Calcium bis-L-pyroglutamate and lithium L-pyroglutamate are prepared by reaction of the metal hydroxides with L-pyroglutamic acid in aqueous solution. In the solid state calcium bis-L-pyroglutamate adopts a layer structure, built up by sixteen-membered rings consisting of four L-pyroglutamate ligands bridging four calcium centers by their carboxylate groups. All three oxygen donors of the L-pyroglutamate ligands are attached to metal centers. The calcium atom lies at the center of a slightly distorted octahedron formed by four carboxylate oxygens and two amide oxygen atoms. Lithium L-pyroglutamate also features a layer structure. All three oxygen donors of the L-pyroglutamate ligand have contacts with metal atoms. The coordination sphere of the lithium atom is a slightly distorted tetrahedron consisting of three carboxylate oxygen atoms and one amide oxygen atom. The investigation of aqueous solutions of the compounds by multinuclear NMR (1H, 13C, 17O) indicates extensive electrolytic dissociation in dilute solutions.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240515
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  • 110
    Electronic Resource
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    Metallcarbonyl-Synthesen, XX. Einfache Methode zur Darstellung von Tc(CO)3-Komplexen: Synthese und Struktur der neuartigen Technetium(I)-Clusterverbindung Na[Tc3(CO)9(OCH3)4] mit Cuban-Struktur (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1107-1111 
    Details
    ISSN: 0009-2940
    Keywords: Technetium complexes ; Isocarbonyl ligand ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Carbonyl Syntheses, XX. - Simple Method for the Preparation of Tc(CO)3 Complexes: Synthesis, Structures, and Reactivity of the Novel Cubane-Type Cluster Na[Tc3(CO)9(OCH3)4]Carbonyltechnetium complexes of type LTc(CO)3 are accessible along a simple route from Na[Tc3(CO)9(OCH3)4] (2) which represents a novel alkoxy complex of cubane-type geometry (single-crystal X-ray diffraction study). 2 is an isolable product of the incomplete carbonylation of sodium pertechnetate (1) conducted in methanol. Under carbon monoxide pressure, 2 yields the binary metal carbonyl Tc2(CO)10 (3), pentamethyl-cyclopentadiene gives the halfsandwich complex (η5-C5Me5)Tc(CO)3 (4), and with benzene/hydrochloric acid the ionic complex [(η6-C6H6)Tc(CO)3]Cl (5) is formed.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240519
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  • 111
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    Synthese stabiler Alkantellurenyl-pseudohalogenide und -pseudochalkogenide: (Me3Si)3CTeX (X=-CN, - SCN, - SeCN, - NCO, - N3) und (Me3Si)3CTe-Y-TeC(SiMe3)3 (Y=- NCN-, - NSN-) (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1131-1133 
    Details
    ISSN: 0009-2940
    Keywords: Alkanetellurenyl pseudohalides ; Alkanetellurenyl pseudochalcogenides ; Tellurenyl pseudohalides, pseudochalcogenides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis of Stable Alkanetellurenyl Pseudohalides and Pseudochalcogenides: (Me3Si)3CTeX (X=- CN, - SCN, - SeCN, - NCO, - N3) and (Me3Si)3CTe-Y - TeC(SiMe3)3 (Y=- NCN-, - NSN-)The first stable and isolable alkanetellurenyl pseudohalides and pseudochalcogenides, tris(trimethylsilyl)methanetellurenyl cyanide, thiocyanate, selenocyanate, isocyanate, azide (2-6) as well as bis[tris(trimethylsilyl)methyltelluro]carbodiimide and -sulfur diimide (7, 8) are obtained in high yields by the reaction of tris(trimethylsilyl)methanetellurenyl iodide (1) with the silver or potassium salts of the respective pseudohalides or pseudochalcogenides. 5-8 are also the first alkyltellurium(II) compounds with Te-N bonding. All compounds have been characterized by 1H-, 13C-, 125Te-NMR, mass, and IR spectroscopy.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240523
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  • 112
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    Beiträge zur Chemie des Phosphors, 211. Pentaisopropyltetracycloundecaphosphan, P11iPr5 - Darstellung und kernresonanzspektroskopische Strukturbestimmung (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1153-1157 
    Details
    ISSN: 0009-2940
    Keywords: Tetracyclo[6.2.1.02,6.05,10]undecaphosphane ; 3,4,7,9,11-pentaorganyl ; Undecaphospha-2,8-ethanonoradamantane ; Undecaphosphane(5) ; Phosphanes, polycyclic ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Contributions to the Chemistry of Phosphorus, 211. - Pentaisopropyltetracycloundecaphosphane, P11iPr5 - Preparation and Structure Determination by Nuclear Magnetic ResonancePentaisopropyltetracycloundecaphosphane (1) has been obtained by reaction of iPrPCl2 with P4 and magnesium and subsequent thermolysis of the crude reaction product, and has been isolated in 91% purity. According to NMR-spectroscopic investigations, 1 has a constitution analogous to that of the hydrocarbon 2,8-ethanonoradamantane, thus being 3,4,7,9,11-pentaisopropyltetracyclo[6.2.1.02,6.05,10]undecaphosphane Compound 1 is formed as a mixture of two configurational isomers 1a and 1b, which differ from each other in their spatial arrangements of the isopropyl groups at P3 and P4.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240527
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  • 113
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    Reaktion von KSi mit M(CO)6 (M=Cr, Mo, W) und Cr(CO)5NMe3 - Struktur von [K(DME)2]2[Cr2(CO)10] (DME=1,2-Dimethoxyethan) (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1167-1169 
    Details
    ISSN: 0009-2940
    Keywords: Anion-cation interactions ; Carbonyl metalates ; Chromium complexes ; Molybdenum complexes ; Tungsten complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of KSi with M(CO)6 (M=Cr, Mo, W) and Cr(CO)5NMe3 - Crystal Structure of [K(DME)2]2[Cr2(CO)10] (DME=1.2-Dimethoxyethane)M(CO)6 (M=Cr, Mo, W) and Cr(CO)5NMe3 are reduced by KSi in DME during several days with formation of the anions [M2(CO)10]2⊖. These can be obtained from a DME/toluene solution as pale yellow or orange crystals of [K(DME)2]2[M2(CO)10] [M=Cr (1), Mo (2), W (3)]. A crystal structure determination of the chromium compound shows that strong interactions between the [Cr2(CO)10]2⊖ and the K⊕ ions exist in the solid state, leading to the formation of one-dimensional polymeric chains. 2 and 3 are isomorphous to 1 (powder diffraction, Rietveld method).
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240531
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  • 114
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    Substituenteneffekte auf die C—C-Bindungsstärke, 10. Resonanzstabilisierung von Alkylradikalen durch zwei geminale Cyangruppen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1191-1198 
    Details
    ISSN: 0009-2940
    Keywords: Bond cleavage ; C—C kinetics of ; Radicals, stability of ; Geminal substituents, energetic interaction of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Effects of Substituents on the Strength of C-C Bonds, 10. - Resonance Stabilization of Alkyl Radicals by Two Geminal Cyano GroupsThe activation parameters of the homolytic cleavage of the Cq - Cq bonds of several dialkylated malonodinitriles (2-5) and of 1,1,2,2-tetracyanoethane (7) and the heat of dissociation of 6 in solution have been determined. Together with the ground state strain of the radical precursors (obtained from the heats of combustion or EFF calculations) the steric influence on the dissociation process has been determined. The resonance stabilization energy of α,α'-dicyanoalkyl radicals then calculated was (12.4 ± 0.9) kcal/mol. This result is discussed within the concept of capto-dative stabilization. The destabilizing interaction of two geminal cyano groups is apparently the same in the ground state of 2 - 7 and the radicals generated from them.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19911240535
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  • 115
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    Electron-Transfer in the Light-Promoted 1,6-Cyclodimerization of 1,1-Di-2-thienylethylene. A Thermal and Photochemical Study (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1203-1206 
    Details
    ISSN: 0009-2940
    Keywords: Dithienylethylene ; Cyclodimerization ; Photoinduced electron transfer ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,1-Di-2-thienylethanol (1) undergoes light-induced (Δ 〉 400 nm) dehydration to afford 1,1-di-2-thienylethylene (2). Compound 2 is selectively converted into 1,6-cyclodimers under thermal or photochemical conditions. In these latter case the non-aromatic Diels-Alder adduct 3 can be characterized. An ET mechanism involving a methyldithienylcarbenium ion (9) as electron acceptor and a chain mechanism is proposed to account for the products.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240537
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  • 116
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    Heterocyclen mit einem Azaallyl-System, 4. 5H-Dibenz[c,e]azepine mit Donor-Gruppen in 7-Stellung (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2085-2090 
    Details
    ISSN: 0009-2940
    Keywords: 5H-Dibenz[c,e]azepines ; Imidates ; alkyl ; heterocyclic ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Heterocycles with an Azaallyl System, 4.  -  5H-Dibenz[c,e]azepines with Donor Groups at the 7-Position5H-Dibenz[c,e]azepines substituted with a methoxy (1) or methylthio group (10) at the 7-position have been synthesized from 6,7-dihydro-5H-dibenz[c,e]azepin-5-one (5) by regioselective O- or S-alkylation with methyl trifluoromethansulfonate and subsequent NH-deprotonation. According to the spectroscopic properties the semicyclic 7-membered alkyl imidates exist exclusively in the benzenoid 5H structure.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240934
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  • 117
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    Stereoselective Synthesis of Alcohols, XXXVIII Stereoselective Total Synthesis of the Denticulatins (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2127-2139 
    Details
    ISSN: 0009-2940
    Keywords: Marine natural products ; Hemiketal formation, selective ; Denticulatins ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The total synthesis of the denticulatins 1 is described. Key feature is the efficient generation of the C-1-to-C-9 building block 37 by three consecutive stereoselective carbon - carbon bond-forming steps using chiral allylboronates. The C-10-to-C-17 building block was obtained by kinetic Sharpless resolution of an allylic alcohol followed by an Ireland-Claisen rearrangement.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240940
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  • 118
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    Masthead (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911241001
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  • 119
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    Simple Entry into Tricyclo[3.3.0.03,7]octanes (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2147-2147 
    Details
    ISSN: 0009-2940
    Keywords: Tricyclo[3.3.0.03,7]octanes ; Samarium iodide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,5-Dimethylbicyclo[3.3.0]octan-3,7-dione (2) was converted into 1,5-dihydroxy-3,7-dimethyltricyclo[3.3.0.03,7]octane (3) in the presence of Sml2 in 76% yield.
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    URL: http://dx.doi.org/10.1002/cber.19911240943
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    Thiolatokomplexe des einwertigen Golds. Synthese und Struktur von [(2,4,6-iPr3C6H2S)Au]6 und (NH4)[(2,4,6-iPr3C6H2S)2Au] (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2161-2164 
    Details
    ISSN: 0009-2940
    Keywords: Gold(I) 2,4,6-tri(isopropyl)thiophenolate, hexamer ; Aurate(I), bis[2,4,6-tri(isopropyl)thiophenolato] ammonium ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thiolato Complexes of Monovalent Gold. Synthesis and Structure of [(2,4,6-iPr3C6H2S)Au]6 and (NH4)[(2,4,6-iPr3C6H2S)2Au]Reaction of Au(CO)Cl with 2,4,6-tri(isopropyl)thiophenol affords hexameric gold(I) thiolate [(2,4,6-iPr3C6H2S)Au]6 (1). According to an X-ray analysis 1 forms a centrosymmetrical twelve-membered Au - S ring in the chair conformation with the linearly coordinated Au atoms at the mid-edges and the S atoms at the corners of the heterocycle. When the reaction of 2,4,6-tri(isopropyl)thiophenol is carried out with AuI in liquid ammonia the thiolato complex [(2,4,6-iPr3C6H2S)2Au]- -NH+4 (2) is obtained. It crystallizes as NH4 · 2 · 3 NH3. The gold atom in 2 is linearly coordinated by two thiolato S atoms. The ammonium cation forms hydrogen bonds with three NH3 solvate molecules.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19911241003
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    Metallacyclobutene aus η2-Cyclopropen-Komplexen des Titanocens und Zirkonocens (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2165-2170 
    Details
    ISSN: 0009-2940
    Keywords: Titanocene complexes ; Zirconocene complexes ; Cyclopropene complexes ; Metallacyclobutenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metallacyclobutenes via η2-Cyclopropene Complexes of Titanocene and Zirconocene(η2-Cyclopropene)(trimethylposphane) complexes of titanocene (4, 5) and zirconocene (8) are obtained in good yields by the reaction of 1,2-diphenylcyclopropene (2) or 4,8-dioxaspiro[2.5]oct-1-ene (3) with bis(trimethylphosphane)titanocene (1) and (1-butene)(trimethylphosphane)zirconocene (7), respectively. In solution the new complexes 4 and 8 rearrange smoothly above room temperature to give the metallacyclobutene derivatives 6 and 9. All new compounds were characterized by spectroscopic methods (31P, 1H, 13C NMR), and the crystal structure of 9 was determined by an X-ray analysis.
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  • 122
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    Mono-, Bis- and Tris(cyclopentadienyl) Compounds - Syntheses of New Polydentate Ligands and their Molybdenum and Tungsten Complexes (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2185-2190 
    Details
    ISSN: 0009-2940
    Keywords: Cyclopentadienes, mono-, bis-, tris- ; DNMR ; Molybdenum, η5-complexes ; Tungsten, η5-complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Condensation reactions of cyclopentadienyl-substituted chlorosilanes CpSiMe2Cl (Cp = C5H5, C5HMe4) with a number of phenols [C6H5OH, 1,3-C6H4(OH)2, 1,4-C6H4(OH)2, 1,3,5-C6H3(OH)3] in the presence of excess base led to six novel molecules containing up to three cyclopentadienyl groups {e.g. 1,3,5-C6H3[OSiMe2(C5Me4H)]3). The dynamic behavior of 1,4-C6H4[OSiMe2(C5H5)]2 (2) was investigated by temperature-variable 1H NMR and the reaction rate of the degenerate 1,2-silicon shift determined. C6H5OSiMe2(C5H5) (1) and (2) were treated with NaH, (MeCN)3M(CO)3 (M = Mo, W), and Mel to give the η5-complexes C6H6OSiMe2 - (C5H4)M(CO)3Me (8: M = Mo, 9: M = W) and 1,4-C6H4[OSiMe2-(C5H4)M(CO)3Me]2 (10: M = Mo, 11: M = W) in good yields. The X-ray crystal structure of 11 was determined.
    Additional Material: 1 Ill.
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    Synthesis and Molecular Structure of the Solvent-Free [LiN(SiMe3)(2,6iPr2C6H3)]2 Dimer (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2223-2225 
    Details
    ISSN: 0009-2940
    Keywords: Lithium, two-coordinate ; Lithium-nitrogen heterocycle ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [LiN(SiMe3)Ar]2 (1, Ar = 2,6-iPr2C6H3) is prepared by the reaction of HN(SiMe3)Ar with nBuLi in n-hexane. This compound with an unusual structure contains a four-membered [LiN]2 heterocycle with two solvent-free two-coordinate Li centers. Its molecular structure represents the first solid-state X-ray analysis of an uncomplexed [LiN]2 dimer.
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    URL: http://dx.doi.org/10.1002/cber.19911241013
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    Functionalized Oxovanadium Alkoxides  -  Potential Haptens (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2249-2254 
    Details
    ISSN: 0009-2940
    Keywords: Vanadium alkoxides ; Haptens ; NMR, 51V ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several new oxovanadium alkoxides and alkoxides/chlorides of the composition VOCl3-n(OR)n (n = 1, R = CPh3; n = 2 and 3, R = CPh3, iBu, cyclopentyl, tert-pentyl, octyl; n = 3, R = dodecyl, 3-methylbutyl) and the mixed ester VO(OiBu)- (OCPh3)2 have been prepared. The compounds VO(OiBu)2OR' have been synthesized, where R' is a functionalized long-chain alkyl group [  -  (CH2)8OH,  -  (CH2)6NH(FMOC),  -  (CH2)6NH2,  -  C(O)(CH2)5C(O)OMe, p-C6H4CN, p-C6H4NH2]. The chloride/carboxylate VOCl2{O2C(CH2)5CO2H} has also been obtained. The compounds are characterized, inter alia, by 51V-NMR spectroscopy. Typical 51V shift ranges are observed for specific ligand functionalities (chloride, alkoxide, carboxylate). δ(51V) values also depend on the steric requirement of the groups R and the coordination number. The importance of the functionalized esters as potential triggers for the production of abzymes with phosphatase activity is discussed.
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    URL: http://dx.doi.org/10.1002/cber.19911241017
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    Synthese und flüssigkristalline Eigenschaften von Multiethern des myo- und scyllo-Inosits (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2265-2277 
    Details
    ISSN: 0009-2940
    Keywords: Inositol ethers ; Mesogens ; Liquid crystals, thermotropic ; Hydrogen bonding ; Supramolecular structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Liquid-Crystalline Properties of myo- and scyllo-Inositol Multi EthersSelectively alkylated myo- and scyllo-inositol ethers were obtained by multi-step syntheses starting from commercially available myo-inositol. Necessary conversions of axial hydroxy groups into equatorial ones were achieved using either potassium superoxide (KO2) or potassium nitrite (KNO2) as oxygen nucleophiles for the transformation of myo- into scyllo- inositol derivatives. Polarizing microscopic and thermoanalytical studies of numerous members of three families (6, 13, and 20) of inositol ethers reveal for most of them thermotropic liquid-crystalline behavior. Furthermore, in case of the two long-chain scyllitol tetraethers 13d and e an unusual thermopolymorphism has been found. The number, position, and stereochemical arrangement of alkyl chains attached to the inositol cores strongly influence the mesogenic properties of these biomolecule derivatives, chemically vicinal diols and tetrols. The self-assembly of the studied inositol multi ethers to columnar mesophases of “supramolecular structures” is discussed considering geometrical features of these molecules and their capabilities to aggregate by hydrogen bonding.
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    URL: http://dx.doi.org/10.1002/cber.19911241020
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    Masthead (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290101
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    Triferriothioxophosphoranes: First Structural Characterization of a μ3-P=S ComplexDedicated to Prof. Dr. M. Herberhold on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 11-13 
    Details
    ISSN: 0009-2940
    Keywords: Triferriophosphane sulfide ; Metallothioxophosphorane ; PS complex ; Spiro compounds ; Decarbonylation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The P-H-functional triferriophosphonium salts [{CpFe-(CO)2}3PH]2FeCl4 (1) and [{μ-CO(CpFeCO)2}{CpFe-(CO)2}PH]2FeCl4 (4) are easily deprotonated by DBU to the corresponding unstable triferriophosphanes 2, 5, which subsequently are oxidized by sulfur to the triferriophosphane sulfides {CpFe(CO)2}3P=S (3) and {μ-CO(CpFeCO)2}{CpFe-(CO)2}P=S (6), respectively. The photolysis of 3 results only in its decomposition by elimination of [CpFe(CO)2]2, whereas the photolysis of 6 cleaves off one CO ligand to give the new spiro compound (CpFeCO)(μ-η2-PS){μ-CO(CpFeCO)2} (7), where the P=S unit is η2-bonded to the 15-electron CpFeCO fragment, and the phosphorus atom bridges two 17-electron fragments. Compound 7 shows a new coordination mode of the PS unit where sulfur is also bound to one of the metal atoms. Compounds 6 and 7 can be regarded as first examples of a new class of PS complexes of transition metals. All compounds were characterized by IR, 31P{1H}- and 13C{1H}-NMR spectroscopy as well as mass spectrometry; for 6 the X-ray analytical data are given.
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    The Chemistry of 1,3,5-Triazacyclohexane Complexes, 3Part 2: Ref.. High Yield Synthesis of [Cr{N(SiMe3)2}3] and Accurate Structure Determination by Cocrystallization with Me6Si2 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 25-27 
    Details
    ISSN: 0009-2940
    Keywords: Triazacyclohexanes ; Chromium complexes ; Amides ; Hexamethyldisilane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of N,N′,N′′-trimethyl-1,3,5-triazacyclohexane chromium trichloride ((Me3TAC)CrCl3, 1) with LiN(SiMe3)2 or NaN(SiMe3)2 in petroleum ether yields nearly quantitatively [Cr{N(SiMe3)2}3] (2) with loss of the Me3TAC ligand. Compound 2 could be crystallized from hexamethyldisilane as [Cr{N(SiMe3)2}3] · (Me6Si2)0,5 which allowed the refinement of the X-ray crystal structure in the trigonal space group P-31c (no. 163) (a = 16.012(3) Å, c = 8.4796(12) Å, V = 1882.8(6) Å3, Z = 2) without severe disorder.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290107
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    Synthesis of Novel Tridentate N,O,S and N,N,O Ligands of the Tripod Type in Racemic and Enantiomerically Pure Form (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 59-68 
    Details
    ISSN: 0009-2940
    Keywords: Glyceraldehyde ; Ligands, tridentate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of seven chiral, tripodal N,O,S and N,N,O ligands were prepared in which N stands for a secondary amine or imidazole donor, O for a phenol, and S for a thioether or thiol metal-binding group. Key steps are (1) the construction of ortho-hydroxyacetophenones bearing the phenolic binding group and either a thioether, a protected thiol or an imidazole substituent in the α-position, and (2) subsequent reductive amination with a primary amine. The modular synthesis allows a rapid construction of a variety of structurally related ligands. In three cases, the enantiomers of the racemic products could be separated after condensation with (R)-glyceraldehyde acetonide as chiral auxiliary. The relative configurations of the cyclic N,O- and N,N-acetals thus obtained were established by NOE spectroscopy. X-ray structural analysis of two crystalline N,O- and N,N-acetals allowed the assignment of absolute configurations. Hydrolysis of the dia-stereomerically pure acetals afforded the enantiomerically pure ligands in high yield. By comparison of their CD spectra, absolute configuration could also be assigned to the third pair of enantiomerically pure ligands.
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    Kinetic Investigations of the Hydrogenation of Diolefin Ligands in Catalyst Precursors for the Asymmetric Reduction of Prochiral Olefins, II[1] (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 85-89 
    Details
    ISSN: 0009-2940
    Keywords: Rhodium complexes, chiral ; Hydrogenation ; Bisolefins ; Thermodynamic stability ; Kinetic control ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Asymmetric hydrogenations of prochiral olefines by means of chiral rhodium(I) complexes of the type [Rh(L)(PP*)]A (L = COD, [(Z,Z)-cycloocta-1,5-diene], or NBD (norborna-2;5-diene), PP* = chiral bisphosphane forming seven-membered chelate rings, A = anion like BF4-) are often associated with induction periods caused by partial blocking of the catalyst. NBD complexes are hydrogenated faster than the corresponding COD complexes. Catalytic hydrogenation of COD/NBD mixtures and the determination of the ratio of the Michaelis constants showed that the steady-state concentration of the COD complex under hydrogen is higher than that of the NBD complex. However, under argon the NBD complex predominates owing to its higher thermodynamic stability compared with that of the COD complex as determined by 31P-NMR spectoscopy. This complete reversion of the ther-modynamically determined ratios of COD to NBD complex concentration under hydrogenation conditions was proven by means of UV/Vis spectroscopy.
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    URL: http://dx.doi.org/10.1002/cber.19961290117
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    1-Bromo-3,5-bis(trifluoromethyl)benzene: A Versatile Starting Material for Organometallic Synthesis (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 233-235 
    Details
    ISSN: 0009-2940
    Keywords: Positional selectivity ; Bromination ; Halogen/lithium exchange ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1-Bromo-3,5-bis(trifluoromethyl)benzene (1) can be selectively prepared by treatment of 1,3-bis(fluoromethyl)benzene with N,N'-dibromo-5,5-dimethylhydantoin in strongly acidic media. A number of synthetically useful reactions via 3,5-bis(trifluoromethyl)phenylmagnesium, -lithium, and -copper intermediates were accomplished.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290219
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    Lithiierte Phosphanimine. Synthese und Kristallstrukturen von [LiCH2PMe2NSiMe3]4 und [LiCMe2P(iPr)2NSiMe3]2 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 253-257 
    Details
    ISSN: 0009-2940
    Keywords: Lithiated phosphane imines ; Phosphane imines, lithiated ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Lithiated Phosphane Imines. Synthesis and Crystal Structures of [LiCH2PMe2NSiMe3]4 and [LiCMe2P(iPr)2NSiMe3]2The title compounds were prepared by the reaction of Me3-SiNPMe3 and Me3SiNP(iPr)3, respectively, with n-Butylli-thium at 20°C in n-hexane solution. They form white, moisture- and oxygen-sensitive crystals, which were characterized by IR spectroscopy and by crystal structure determinations. - [LiCH2PMe2NSiMe3]4 (1) forms a Li4 tetrahedron, the faces of which are capped with CH2 groups with average Li-C distances of 233 and 251 pm, while the nitrogen atoms occupy the corners of the Li4 tetrahedron. - [LiCMe2P(iPr)2N-SiMe3]2 (2) forms molecules of symmetry C2 in which the lithium atoms have coordination number three by two carbon atoms and one nitrogen atom with Li-C distances of 215.2 and 237.9 pm and Li-N of 192.8 pm.
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    URL: http://dx.doi.org/10.1002/cber.19961290223
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    Synthesis and Characterization of a Novel Cyclobutadiene-octatetrayne Polymer (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 269-273 
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    ISSN: 0009-2940
    Keywords: Organometallic polymers ; Coupling reactions ; Butadiynyl complexes ; Cobalt compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of 3a starting from compound 1 is described. Copper-catalyzed oxidative coupling of 3b under Hay conditions gives the novel polymer 9 with octatetrayne-cyclobutadiene units.
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    A Study on Electronic Interaction Between two [2.2]Metacyclophane Systems Connected with a C=C Bond: Preparation, Structure and Complexation of (E)- and (Z)-8,8′-(Ethene-1,2-diyl)bis(5-tert-butyl[2.2]metacyclophane) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 289-296 
    Details
    ISSN: 0009-2940
    Keywords: Bis[2.2]metacyclophanes ; Stilbenes ; π-π Interaction ; Tricarbonylchromium complexes ; Charge-transfer ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (E)-8,8′-(Ethene-1,2-diyl)bis(5-tert-butyl[2.2]metacyclo-phane) (2) was obtained from a McMurry reaction of 5-tert-butyl-8-formyl[2.2]metacyclophane (1). Irradiation of 2 with a high-pressure mercury lamp gave the corresponding (Z) isomer 3. X-ray crystallographic analyses of 2 and 3 show a certain degree of twisting of the bond connecting the meta-cyclophane unit and the central π system due to steric crowding. UV spectra of 2 and 3 and of the charge-transfer complexes [2/TCNE] and [3/TCNE] allow for a discussion of π-π interaction between the central stilbene subunit and the outer benzene rings of the metacyclophane units. Bis[2.2]meta-cyclophanes 2 and 3 reacted regioselectively with hexacar-bonylchromium on the outer benzene rings giving 1:1 and 1:2 complexes 9-14 with tricarbonylchromium. No 1:3 and 1:4 complexes formed due to steric restrictions. Analysis of UV spectral data of the complexed [2.2]metacyclophanes was performed for an indication of π-π interactions in the complexes.
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    URL: http://dx.doi.org/10.1002/cber.19961290308
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    Thermally Stable Self-assembling Open-Frameworks: Isostructural Cs+ and (CH3)4N+ Iron Germanium Sulfides (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 283-287 
    Details
    ISSN: 0009-2940
    Keywords: Self-assembling frameworks ; Thermal stability ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Here we report on investigations that have revealed for the first time that the Cs+ ion templates the same metal germanium sulfide open-framework as (CH3)4N+ (TMA+), and that metal complexing agents enhance crystal size by at least two orders of magnitude. The synthesis, structures and thermal properties of Cs2FeGe4S10 ·× H2O and TMA2FeGe4S10 are also described. Both have 3D zinc blende-type open-framework structures. These materials have the same connectivity as TMA2MnGe4S10. The tetrahedral sites in the lattice are alternately substituted by pseudo-tetrahedral Fe2+ and adamantanoid Ge4S104- building blocks, covalently linked together by Fe(μ-S)Ge bridge bonds, to give a tetragonal unit cell. The charge-balance of the anionic framework [Fe-Ge4S10]2- is maintained by either Cs+ or TMA+ ions in the cavity spaces. Synthesis of these materials demonstrates an interesting example of a self-assembly process in which a 3D framework is built from molecular precursors. Water adsorption-desorption cycling from room temperature to 200 °C reveals framework flexibility between larger and smaller tetragonal unit cell 14 isotypes. The compound TMA2FeGe4S10 is stable in nitrogen at 350 °C and under vacuum at 450 °C. The corresponding temperatures for Cs2FeGe4S10 are 530 °C and 630°C; it is stable on cooling to room temperature under vacuum, and after subsequent exposure to air. Six hundred thirty degrees celsius is the highest recorded temperature at which the integrity of a non-oxide framework has been maintained. The framework stability and flexibility of “all-inorganic” Cs2FeGe4S10 provides an encouraging example for researchers interested in developing sulfide-based framework materials with practical applications.
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    Complexes with S-Donor Ligands, 4Part 3: J. Vicente, M. T. Chicote, P. González-Herrero, P. G. Jones, J. Chem. Soc., Chem. Commun. 1995, 745.. Mono- and Di-Homo- and -Hetero-Nuclear Gold(I), Silver(I), and Palladium(II) Complexes with 2-(Methylthio)pyridine, Pyridine-2(1H)-thione, and Benzoxazole-2(3H)-thione. Some Examples of the Use of Complexes as Ligands (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 327-330 
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    ISSN: 0009-2940
    Keywords: Gold complexes ; Silver complexes ; Palladium complexes ; S-Donor ; Thiones ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: AgClO4 reacts with bidentate ligands 2-(methylthio)pyridine (SMepy) or complexes PPN[Au(Spy)2] [PPN = N(PPh3)2, HSpy = pyridine-2(1H)-thione) or PPN[Au(Sbz)2] (HSbz = benzoxazole-2(3H)-thione), themselves acting as ligands, to give dinuclear complexes [Ag2(μ-SMepy)2](ClO4)2 (1), [AgAu(μ-Spy)2] (2), or [AgAu(μ-Sbz)2] (3), respectively. By treating 1 with [AuCl(tht)] (tht = tetrahydrothiophene), [Au(SMepy)(tht)]ClO4 (4) is obtained which, in turn, reacts with SMepy to give [Au(SMepy)2]ClO4 (5). Similarly, [PdCl2(NCPh)2] reacts with SMepy in 1:1 molar ratio to give [Pd2Cl2(μ-Cl)2(SMepy)2] (6) which reacts with SMepy in 1:2 molar ratio to give [PdCl2(SMepy)2] (7). On the other hand, HSpy reacts with Ag2CO3 to give [Ag2(μ-Spy)2] (8), and (SMepyH)ClO4 reacts with [Au(acac)PPh3] (acacH = acetyl-acetone) to give [Au(SMepy)PPh3]ClO4 (9).
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    Zinc Complexes of Amino Acids and Peptides, 6. Zinc Complexes of Oligopeptides Containing Histidine at Both Termini (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 347-353 
    Details
    ISSN: 0009-2940
    Keywords: Histidine peptides ; Zinc complexes ; EXAFS analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: One tripeptide, five tetrapeptides, and one pentapeptide, all containing His-Xn-His sequences and being blocked at the N and C termini with acyl and amide functions, respectively, were synthesized by solid-phase methods. With one exception their reaction with various zinc salts led to the precipitation of 1:1 (zinc/peptide) complexes. Analytically pure compounds were obtained from zinc tetrafluoroborate and His-Gly-His (1), from zinc chloride (resp. bromide) and His-Gly -Gly-His (2), His-Ala-Gly-His (3), His-Leu-Gly-His (4), His-Pro-Gly-His (5), and His-Pro-Asn-His (6) as well as from zinc sulfate and His-Leu-Gly-His (4) and His-Ala-Pro-Gly-His (7). 1H-NMR data, when available, indicate the coordination of both histidine units to zinc in all cases. The low solubility of the complexes points to their polymeric nature. The only 1:2 (zinc/peptide) complex in this series was obtained from zinc perchlorate and His-Gly-Gly-His (2). An EXAFS study revealed that it contains zinc symmetrically coordinated by four histidine imidazole ligands. Based on the available information it is proposed that all complexes are one-dimensional polymers containg [-Zn-His-Xn-His-Zn-]x backbones.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290316
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    Masthead (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290401
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  • 139
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    Silanediols Derived from Silanetriols. X-ray Crystal Structures of (2,4,6-Me3C6H2)N(SiMe3)Si(OSiMe3)(OH)2 and (2,4,6-Me3C6H2)N(SiMe3)Si(OSiMe2R)(OH)2 [R = CH2 (2-NH2-3,5-Me2C6H2)] (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 391-395 
    Details
    ISSN: 0009-2940
    Keywords: Silanediols ; Silanetriols ; Siloxanes ; Hydrogen bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The silanediols RN(SiMe3)Si(OSiMe3)(OH)2 (R = 2,4,6-Me3C6H2 4, 2,6-Me2C6H3 5, and 2,6-iPr2C6H3 6) were prepared by the reactions of the respective silanetriols RN(SiMe3)-Si(OH)3 1 - 3 with SiMe3Cl in THF/hexane. Silanetriol 1 in CH2Cl2/hexane solution converts over a period of 4 weeks into the silanediol (2,4,6-Me3C6H2)N(SiMe3)Si(OSiMe2 R)-(OH)2 [R = CH2(2-NH2-3,5-Me2C6H2)] (7). Compounds 4 - 7 were characterized by means of mass, IR and NMR (1H and 29Si) spectroscopy. Additionally, the molecular structures of 4 and 7 were determined by single-crystal X-ray diffraction studies. Compound 4 forms O — H…O hydrogen-bonded tetramers in the solid state. A nine-membered ring formed by an intermolecular O—H…N hydrogen bond is found in the solid-state structure of 7.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290405
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    Novel trialkylstibane iridium(I) and iridium(III) complexes including the x-ray crystal structure of five-Coordinate [IrCl(C2H4)2(SbiPr3)2]Dedicated to Professor Erwin Weiss on the occasion of his 70th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 411-417 
    Details
    ISSN: 0009-2940
    Keywords: Iridium complexes ; Stibane complexes ; Hydrido complexes ; Ethene complexes ; Ligand displacement reactions ; Alkyne-to-vinylidene rearrangement ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of [IrCl(C8H14)2]2 (2) with SbiPr3 in the presence of H2 yields the dihydridoiridium(III) complex cis,mer-[IrH2Cl(SbiPr3)3] (3) which on treatment with CO and with HC≡CR (R = Ph, CO2Me) affords the octahedral derivatives [IrH2Cl(CO)(SbiPr3)2] (4) and [IrHCl(C≡CR)(SbiPr3)3] (5, 6), respectively. The stibane ligand trans to hydride in 5 and 6 is rather labile and, therefore, 5 and 6 react with pyridine to give [IrHCl(C≡CR)(py)(SbiPr3)2] (7, 8). Five-coordinate bis-(stibane)iridium(I) complexes [IrCl(C2H4)2(SbR3)2] (10-12) were prepared from [IrCl(C2H4)2]2 (9) and four equiv. of SbR3 (R = iPr, Me, Ph). The X-ray crystal structural analysis of 10 reveals a distorted trigonal-bipyramidal geometry around the metal center with one stibane ligand and the two olefinic ligands in the equatorial plane. Compound 10 reacts with NaC5H5 to yield [C5H5Ir(C2H4)(SbiPr3)] (13) and with different alkynes by partial or complete displacement of the ethene ligands to give trans-[IrCl(PhC≡CPh)(SbiPr3)2] (14), [IrHCl(C≡CTol)(C2H4)(SbiPr3)2] (15), and trans-[IrCl-{=C=C(SiMe3)R}(SbiPr3)2] (16, 17), respectively.
    Additional Material: 1 Ill.
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  • 141
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    Azolylborane adducts. Structural and conformational analysis by x-ray diffraction and NMR. Protic-hydric (C=Hδ+-δ-H=B) and Protic-Fluoride (C=Hδ+-δ-F=B) interactions (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 441-449 
    Details
    ISSN: 0009-2940
    Keywords: Azolylborane adducts ; Boron-imidazole adducts ; Boron-pyridine adducts ; Protic-hydric interactions ; Protic-fluoride interactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation, NMR and X-ray diffraction studies of a series of azolylboron hydrides derived from pyrrole, indole, and carbazole coordinated with tetrahydrofuran, pyridine, and imidazole are reported. The azolyl substituents are very electroattractive leading to an acidic boron atom which strongly coordinates with the Lewis bases. The stabilization of the =BH2=groups against disproportionation could be explained in terms of the interactions found between the acidic hydrogen atoms of the heterocycles (C=Hδ+ acceptor) and the hydrides (B=Hδ- donors).
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290413
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    Masthead (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290501
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    The Synthesis of Stabilized Dimetallated Thioimidate Complexes by the Insertion of Ethoxycarbonylisothiocyanate into a Rhenium-Rhenium Bond (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 485-487 
    Details
    ISSN: 0009-2940
    Keywords: Dimetallations ; Insertions ; Rhenium ; Isothiocyanates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Molecules containing dimetallated hydrocarbyl groupings are of great chemical interest[1-3]. These groupings often represent intermediates in important catalytic processes[4]. Recently, we have shown that substituted dimetallated olefins can be formed by alkyne insertion into the metal-metal bonds of certain dinuclear complexes[2,5]. Complexes having dimetallated hydrocarbyl groups combined with heteroatoms are quite rare[6]. Herein is described the formation of a dimetallathioimidate grouping by the insertion of an organic isothiocyanates into an unsupported metal-metal bond. Organic isothiocyanates are useful reagents in organic synthesis[7], but the organometallic chemistry of these molecules is not yet well developed[8].
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290503
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    Supermolecules Containing a Tetrahedral Core: A New Class of Liquid-Crystalline Siloxanes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 521-525 
    Details
    ISSN: 0009-2940
    Keywords: Liquid crystals ; Siloxanes ; Phase behaviors ; Defined topology ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It is shown that supermolecules with a tetrahedral symmetry and appropriate side-chains exhibit liquid-crystalline phase behaviour. The use of an optimised hydrosylation reaction allows for the synthesis of materials that have four mesogenic groups attached to a siloxane core, where the conformation and the configuration are unambiguous. The materials show low glass transition temperatures and, depending on the spacer length, complex liquid-crystalline morphologies.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290508
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    Transition Metal Complexes with Sulfur Ligands, Part 119Part 118: D. Sellmann, H.-J. Kremitzl, F. Knoch, M. Moll, J. Biol. Anorg. Chem., in press.. Synthesis of Water Soluble Fe and Ru Complexes with Novel Multidentate Thioether Thiolate Ligands Containing Carboxylate Substituents (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 509-519 
    Details
    ISSN: 0009-2940
    Keywords: Iron and ruthenium complexes ; Water soluble complexes ; Sulfur ligands ; X-ray structure analyses ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In search of water soluble transition metal complexes with sulfur dominated coordination spheres that model key reactions of nitrogenases, the benzenedithiol derivatives ‘CO2HS2’-H2 (1) and ‘CO2Me-S2’-H2 (2) were synthesized as precursors for multidentate sulfur ligands. The template alkylation of 2 by C2H4Br2 at [Fe(CO)2] fragments yielded a mixture of two diastereomeric C2 symmetrical [Fe(CO)2(‘CO2Me-S4’)] complexes (4a and 4b), which were separated by crystallization. The hydrolysis of the mixture of the diastereomers 4a and 4b led to the isomerically pure tetradentate thioether thiol ligand ‘CO2Me-S4’-H2 (5) proving the regioselectivity of the template alkylation of the asymmetrical dithiol 2. The C1 symmetrical [Fe(‘CO2Me-S2’)2]2- anion is an intermediate of the template alkylation and was isolated as (AsPh4)2 [Fe(‘CO2Me-S2’2] (11), 4a, 5 and 11 were characterized by X-ray structural analysis. Saponification of the methyl ester groups of 5 yielded ‘CO2H-S4’-H2 (7). Treatment of 7 with FeCl2 · 4 H2O in the presence of CO and LiOMe gave a mixture of two C2 symmetrical and water soluble diastereomers of Li2[Fe(CO)2(‘CO2-S4’)] (8). Upon treatment with [RuCl2 (PPh3)3] 7 yielded isomerically pure [Ru(PPh3)2-(‘CO2H-S4’)] (9). 9 also exhibits C2 symmetry and could be reversibly deprotonated to form the water soluble complex K2[Ru(PPh3)2 (‘CO2-S4’)] (10). Treatment of (NBu4)2 (‘CO2MeS2’) with “Ru(NO)Cl3” led to isomerically pure (NBu4)[Ru(NO)(‘CO2Me-S2’)2] (12).
    Additional Material: 6 Ill.
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    Syntheses and Photochemistry of Fluorinated and Chlorinated Titanium Porphyrinates: Crystal Structure of Oxotitanium meso-Tetrakis(2,3,4,5,6-pentafluorophenyl)porphyrinate (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 833-836 
    Details
    ISSN: 0009-2940
    Keywords: Oxotitanium(IV) porphyrinate ; Peroxotitanium(IV) porphyrinate ; Photochemistry ; Singlet oxygen ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The syntheses of oxotitanium(IV) meso-tetrakis(2,3,4,5,6-pentafluorophenyl)porphyrinate O=Ti(TPPF20) (1), oxotitanium(IV) meso-tetrakis(2,6-difluorophenyl)porphyrinate O=Ti-(TPPF8) (3), and oxotitanium(IV) meso-tetrakis(2,6-dichlorophenyl)porphyrinate O=Ti(TPPCl8) (5) from titanium tetrachloride and the corresponding porphine are described. The structure of 1 was determined by single-crystal X-ray diffraction. The reaction of oxotitanium porphyrinates with aqueous hydrogen peroxide leads to the corresponding light-sensitive peroxotitanium(IV) complexes: Ti(O2)(TPPF20) (2), Ti(O2)-(TPPF8) (4), Ti(O2)(TPPCl8) (6). All complexes are efficient and stable photosensitizers for the generation of singlet oxygen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290715
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    Syntheses of Hetero-sila-closo-boranes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 837-839 
    Details
    ISSN: 0009-2940
    Keywords: Boron compounds ; Silaboranes ; Dihetero-closo-borane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Addition of 3 equivalents of KH · BEt3 to [Me3NH][Me-SiB10H12] followed by addition of one equivalent of SnCl2 or SbI3 affords the stanna-sila-closo-borate(1-) 3 and stiba-sila-closo-borane 4, respectively. [MePh3P] · 3 crystallizes in the orthorhombic space group P212121.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290716
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    Intramolekular stabilisierte Übergangsmetallamide: 2-(Dimethylaminomethyl)pyrrolyl-Komplexe des Titan(III), Vanadium(III), Chrom(III), Cobalt(II) und Nickel(II) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 853-857 
    Details
    ISSN: 0009-2940
    Keywords: Amides ; Pyrrolyl complexes ; Chelate complexes ; Transition-metal complexes ; Metallacycles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Intramolecularly Stabilized Metal Amides: 2-(Dimethylaminomethyl)pyrrolyl Complexes of Titanium(III), Vanadium(III), Chromium(III), Cobalt(II) and Nickel(II)By the metallation of 2-(dimethylaminomethyl)pyrrol (HL) with butyllithium the lithium pyrrolide LiL (1) was obtained. The reactions of 1 with TiBr3 · 3 THF, VBr3 · 3 THF, CrBr3 · 3 THF, CoBr2 · 2 THF, and NiBr2 · 1.67 THF result in the formation of the 2-(dimethylaminomethyl)pyrrolyl complexes of type ML3 (2-4), and ML2 (5, 6), respectively. The structures of these new compounds are discussed on the basis of magnetic and visible absorption measurements. An X-ray crystal structure determination of 4 reveals a strongly distorted octahedral environment of the chromium atom with facial arrangement of the ligands.
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    URL: http://dx.doi.org/10.1002/cber.19961290719
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    Stepwise Insertion of Alkylisocyanides into the Metal-Alkyne Bond of Half-Sandwich Type Rhodium Complexes: Synthesis and Structural Characterization of Metallacyclobutenes and MetallacyclopentenesDedicated to Professor Gerhard E. Herberich on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 903-910 
    Details
    ISSN: 0009-2940
    Keywords: Rhodium complexes ; Alkyne complexes ; Insertion reactions ; Alkyl isocyanides ; Metallacycles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The cyclopentadienyl complexes [C5H5Rh(RC≡CR′)(SbiPr3)] (5-8), which were prepared from trans-[RhCl-(RC≡CR′)(SbiPr3)2] (1-4) and NaC5H5 and which contain a labile Rh-SbiPr3 bond, reacted with CO and CNR″ (R″ = Me, tBu) to give the carbonyl and isocyanide derivatives [C5H5Rh(RC≡CR′)(CO)] (9-11) and [C5H5Rh(RC≡CR′)-(CNR″)] (12-16), respectively. On treatment of 12 (R = R′ = Ph; R″ = Me) with SbiPr3, the metallacyclobutene complex [C5H5Rh{κ2(C,C}-C( = NMe)CPh=CPh}(SbiPr3)] (17) was formed; it reacts with excess CNMe or CNtBu to yield the metallacyclopentenes [C5H5Rh{κ2(C,C)-C(=NMe)CPh=CPhC-(=NR)}(CNR)] (18, 19). Similar compounds 20-23 containing a five-membered RhC4 metallacycle were prepared either from [C5H5Rh(RC≡CR′)(SbiPr3)] (7, 8) or [C5H5Rh-(PhC≡CPh)(CNtBu)] (14) and excess isocyanide. The crystal and molecular structures of 17 and 18 (R = Me) have been determined.
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    Isolation and Spectroscopic Characterization of Heteroleptic, Anionic and Neutral (Phthalocyaninato)(tetra-4-pyridylporphyrinato)lanthanide(III) Double-DeckersDedicated to Professor Shang-Wai Tam on the occasion of his retirement from The Chinese University of Hong Kong. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 933-936 
    Details
    ISSN: 0009-2940
    Keywords: Phthalocyanines ; Porphyrins ; Lanthanide(III) compounds ; Macrocyclic ligands ; Double-decker complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of 5,10,15,20-tetra-4-pyridylporphyrin [(TPyP)H2] with europium(III) or gadolinium(III) acetylacetonate [Ln(acac)3 · nH2O] (Ln = Eu, Gd) in 1,2,4-trichlorobenzene produced Ln(acac)(TPyP), which reacted with dilithium phthalocyaninate [Li2(Pc)] to give Li[Ln(Pc)(TPyP)] in moderate yields. Upon exposure to air, solutions of these compounds converted slowly to the corresponding neutral complexes Ln(Pc)(TPyP). The new compounds were spectroscopically characterized.
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    Synthesis, Spectroscopic Characterization, and Crystal Structure Determination of Cationic [(Cyclopentadienyl)dicarbonyliron](alkynyl)-aminocarbene Complexes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 937-944 
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    ISSN: 0009-2940
    Keywords: Iron acyl complexes ; (Alkynyl)carbene ligand ; Cationic aminocarbene complexes ; Iron (2-methoxyvinyl)aminocarbene complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (Alkynoyl)iron complexes 1, Cp(CO)2Fe(O=CC≡CR) (R = CH3, Ph, SiMe3), were synthesized by applying a mixed anhydride procedure and transformed into the cationic methoxycarbene complexes 2, [Cp(CO)2 Fe(C(OMe)C≡CR)+]-[PF6-]. Primary amines H2NR′ react with the methoxycarbene complexes to furnish exclusively cationic aminocarbene complexes 3, [Cp(CO)2 Fe(C(NHR′)C≡CR)+][PF6-], or (2-methoxyvinyl)aminocarbene complexes 5. The spectroscopic properties of the new complexes are discussed. The (alkynyl)-aminocarbene complexes 3e and 3f were characterized by X-ray crystal structure analysis.
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    URL: http://dx.doi.org/10.1002/cber.19961290810
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    Synthesis and Characterization of Novel Phthalocyanines with Four 16-Membered Diazadithia Macrocycles (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 967-971 
    Details
    ISSN: 0009-2940
    Keywords: Phthalocyanines, sulphonated ; Diazadithiamacrocycles ; Pentanuclear complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal phthalocyanines (M = Cu, Ni, Co) 3-5 bearing four 16-membered diazadithia macrocycles at the peripheral positions were prepared. Detosylation with concentrated sulfuric acid afforded products containing both sulfonated groups on the aromatic rings of the macrocyclic substituents which are excellently soluble in water and donor sites for binding four CuII ions to give a pentanuclear complex.
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    A Search for Thionitrosyl Chloride (Cl-N=S) in the Gas Phase (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1379-1381 
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    ISSN: 0009-2940
    Keywords: Thionitrosyl chloride ; Thiazyl chloride ; Neutralization-reionization mass spectrometry ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ab initio MO calculations at the QCISD(T)/6-311++G(3df,2p) + ZPE level show that the thionitrosyl chloride ion, ClNS+•, is 36 kJ/mol more stable than the thiazyl chloride ion, NSCl+•, whereas neutral NSCl is 77 kJ/mol more stable than ClNS [IEa (ClNS) = 9.2 ± 0.3 eV, IEa (NSCl) = 10.5 ± 0.3 eV]. Mild flash-vacuum pyrolysis of the thiazyl chloride trimer (NSCl)3 followed by electron impact ionization resulted in the formation of [N,S,Cl]+• ions (m/z 81). The fragments observed in the CA spectrum of these ions indicate the formation of both NSCl+• and ClNS+• ions. A very weak recovery signal is observed in a neutralizationreionization experiment. This signal is tentatively assigned to the neutral thionitrosyl chloride.
    Additional Material: 4 Ill.
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    Synthesis and Reactivity of Some Nitroaryl Complexes of HgII and AuIII  -  Synthesis of a Substituted Biphenyl by C-C Coupling - Crystal Structure of [Hg(C6H4NO2-3, OnBu-6)2] (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1395-1399 
    Details
    ISSN: 0009-2940
    Keywords: Gold ; Mercury ; Nitroaryl ; Transmetallation ; Biaryl ; C-C Coupling ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 4-Butoxynitrobenzene reacts with [Hg(O2CCF3)2] and LiCl to give [Hg(R)Cl] [R = C6H3NO2-3, OnBu-6 (1)] which is symmetrized by Me4NCl to give [HgR2] (2), the crystal structure of which has been determined. The reaction of 2 with Me4N[AuCl4] affords Me4N[Au(R)Cl3] (3) by a facile transmetallation process. Complex 3 reacts with PPh3 (1:1) to give cis-[Au(R)(PPh3)Cl2] (4). The diaryl complex [-Ph-2)(R)Cl] (5) is obtained by reaction of 3 with [Hg-(C6H4N=NPh-2)2] through a second transmetallation reaction. Complex 5 and PPh3 (1:1) give [AuClPPh3] and the C-C coupling biphenyl RC6H4N=NPh-2 (6).
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    URL: http://dx.doi.org/10.1002/cber.19961291114
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    Sulfenato, Thiosulfinato, and Thiosulfonato Transition Metal ComplexesDedicated to Professor M. Herberhold on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1409-1419 
    Details
    ISSN: 0009-2940
    Keywords: Sulfenic acid anions ; Thiosulfinic acid anions ; Thiosulfonic acid anions ; Transition metal complexes ; Stereochemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis and coordination chemistry of sulfenic, thiosulfinic, and thiosulfonic acid anions are reviewed. Different approaches, which yield the platinum(II) and ruthenium(II) complexes containing the anionic sulfur(0), sulfur(II), and sulfur(IV) oxid ligands, are described. The oxidative addition of thiosulfinates or N-sulfinyl phthalimides to platinum(0) complexes L2Pt(C2H4) [L = PPh3, 1/2 PPh2CH2CH2PPh2, 1/2 (R,R)-(-)-DIOP, 1/2 (C5H4PPh2)Fe(C5H4PPh2) leads to sulfenato complexes; those of N-thiosulfinyl phthalimidies or trisulfid 1-oxides afford the thiosulfinato complexes. Moreover, the reactions of CpRu(PPh3)(L)(SH) (L = CO, PPh3) with N-sulfinyl phthalimides forming the thiosulfinato moiety, are reported. The spectroscopic, structural and chemical properties of these complexes are discussed.
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    Cationic Iron Aminocarbene Complexes as Dienophiles in Diels-Alder Reaction with Cyclopentadiene (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1057-1059 
    Details
    ISSN: 0009-2940
    Keywords: (Alkynyl)carbene ligands ; Iron acyl complexes ; Cationic iron aminocarbene complexes ; Diels-Alder reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The cationic iron (alkynyl)aminocarbene complexes [Cp(CO)2Fe(C(NHR)C≡CSiMe3][PF6], (R = C6H5, p-CH3C6H4) 1 derived from aromatic amines smoothly react with cyclopentadiene in dichloromethane to yield the cycloadducts 2. No reaction was observed for complexes derived from sterically demanding aliphatic amines, like L-alanine tert-butyl ester. For comparison, the alkynyl-substituted acyl iron compounds Cp(CO)2Fe(C=O)C≡C̊ (R = SiMe3, C6H5) 3 were investigated, requiring TiCl4 catalysis to undergo the cycloaddition reaction. The structures of the cycloadducts 4 were determined by X-ray crystallography.
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    URL: http://dx.doi.org/10.1002/cber.19961290913
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    Synthesis, Structure and Reactions of the Homoleptic Alkyne Nickel(0) Complex (Alkyne)4Ni3 (Alkyne: 2-methyl-4-trimethylsilyl-3-butyn-2-ol)Dedicated to Professor Walter Siebert on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1457-1461 
    Details
    ISSN: 0009-2940
    Keywords: Nickel(0) ; Alkyne complexes ; Hydrogen bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of (cdt)Ni (cdt: cyclododeca-1,5,9-triene) with 2 equivalents of 2-methyl-4-trimethylsilyl-3-butyn-2-ol leads to the selective formation of the homoleptic complex (alkyne)4Ni3 (compound 3), which can be isolated in excellent yields. The solid-state structure of 3 exhibits three Ni centers, forming a bent Ni3 chain connected by two bridging alkynes. The other two alkynes are terminally coordinated. Additionally, the trimeric units are stabilized by three intramolecular hydrogen bonds. Two intermolecular hydrogen bonds connect the trimeric units to form a polymer rope. According to the 13C- and 1H-NMR spectra in THF the structure of the complex 3 in solution is very similar to that in the solid state. The reaction of 3 with some alkynediols and with 2,5,5-trimethylhex-3-yn-2-ol affords compounds of the type (alkyne)2Ni. Cot (cot: 1,3,5,7-cyclooctatetraene) converts 3 into [(cot)Ni]2, which in turn reacts with 2,5-dimethylhex-3-yne-2,5-diol to form the dimeric complex (alkyne)2Ni2(cot) 6. X-ray analysis of 6 reveals a very symmetrical structure in which cot connects both Ni(0) centers at opposite sides of the ring system.
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    Control of the SO2 Coordination Mode at the (Monochelate)rhodium Complex ClRh(P∼O) with the Hemilabile Ligand Cy2PCH2CH2OCH3Dedicated to Professor Michael Hanack on the occasion of his 65th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1103-1105 
    Details
    ISSN: 0009-2940
    Keywords: Sulfur dioxide ; Rhodium complexes ; Ether-phosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The SO2 coordination mode at the rhodium complex [ClRh(P∼O)()] (1) [ = η2(O,P)-chelated Cy2PCH2CH2OCH3 ligand; P∼O = =1(P)-coordinated] is controlled by the hemilabile ligand Cy2PCH2CH2OCH3 and shows a dependence on the polarity of the solvent. In polar organic solvents (e.g. acetone) the addition of sulfur dioxide results in the formation of a trigonal-pyramidal oriented SO2 group in [ClRh(η1-SO2)(P∼O)()] (2a). However, in nonpolar media (e.g. n-hexane) a trigonal-coplanar geometry of the SO2 unit in [ClRh(η1-SO2)(P∼O)2] (2b) is favored.
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    Masthead (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961291001
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    1,3-Heterobinuclear Cyclobutenylidene Complexes with an Exocyclic C=C bond  -  Synthesis, Structure, and Spectroscopic Properties (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1475-1482 
    Details
    ISSN: 0009-2940
    Keywords: Allenylidene complexes ; Alkynyl complexes ; Cyclobutenylidene complexes ; Cycloadditions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pentacarbonyl(allenylidene)chromium and -tungsten, [(CO)5—M=C=C=CR2] (M=Cr, R=C6H4CH3-p(1a), C6H4OCH3 (1b); M=W, R=C6H4CH3-p (1c), react with the alkynyl complexes [Cp(CO)2Fe—C≡CR′] (R′ = nBu (2), Ph (4)), [Cp*(CO)2Fe—C≡CnBu] (6), [Cp(CO){P(OMe)3}-Fe—C≡CnBu] (8) and [Cp(PPh3)Ni—C≡CnBu] (10) by cycloaddition of the C≡C bond of the alkynyl complexes to the Cα=Cβ bond of the allenylidene ligand to give 3a-c), (5), (7), and respectively. The cycloaddition is highly selective. The spectroscopic data of these 1,3-heterobinuclear complexes indicate a delocalized π-system (M=Cr, W; Y=[Fe(CO)2Cp], [Fe(CO)(P{OMe}3)Cp], [Fe(CO)2Cp*], [Ni(PPh3)-Cp]). X-ray structural analyses of the compounds 3a, 9a, and 11c reveal a “butterfly” conformation of the four-membered ring. Its puckering angle is 142° (3a), 152° (9a), and 151° (11c). All Complexes exhibit a moderate to strong negative solvatochromic behavior. The extent of the solvatochromic effect depends on [(CO)5M] and Y and considerably decreases when C=CR2 is replaced by e.g. CMe2.
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    The Phosphonate-Phosphate- and Phosphate-Phosphonate Rearrangement and Their Applications, 4Part 3: Ref.[1].. Deprotonation of Secondary Benzylic Phosphates  -  Configurationally Stabile Benzylic Carbanions with a Diethoxyphosphoryloxy Substituent and Their Rearrangement to Optically Active Tertiary α-Hydroxyphosphonates (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1503-1508 
    Details
    ISSN: 0009-2940
    Keywords: Phosphate - Phosphonate rearrangement ; Carbanions, benzylic, configurational stability of ; α-Hydroxyphosphonates, tertiary, chiral, non-racemic ; t-Butyl(phenyl)phosphinothioic acid, homochiral ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Optically active alcohols (ee ≥ 98%) such as 1-phenylpropanol, 1-(2-naphthyl)ethanol, 1-tetralol, and 1-indanol were transformed into diethyl phosphates 7a-d. sBuLi/TMEDA  -  induced phosphate - phosphonate rearrangement in diethyl ether furnished tertiary α-hydroxyphosphonates 8a-d of high enantiomeric purity (ee 94-98%) in yields of 43-83% with retention of configuration. The enantiomeric excesses were determined by using homochiral t-butyl(phenyl)phosphinothioic acid as chiral solvating agent.
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    Hydride Addition to Coordinated S2CPR3 Ligands in Mononuclear Mn and Re Complexes: Phosphane-dithioformate Adducts as Five-electron Bridging Ligands (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1535-1540 
    Details
    ISSN: 0009-2940
    Keywords: 1,1-Dithiolate ; Manganese complexes ; Rhenium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The cationic tetracarbonyl complex cis-[Mn(CO)4-(S2CPCy3)]+ undergoes addition of hydride ion to the central carbon of the S2CPR3 ligand to afford, after spontaneous dimerization with loss of CO, the dimer [Mn2(CO)6{μ-S2C(H)PCy3}2] (5a), which was characterized by analytical and spectroscopic methods as well as by X-ray diffraction. In the molecule of 5a each S2C(H)PCy3- ligand is coordinated to one manganese in an η2-S,S′ chelate fashion, and one sulfur of each ligand serves as a bridge to bind the other manganese atom, thus forming a distorted Mn2S2 square. This appears to be a very stable arrangement. Compound 5a can be more easily prepared by treating the perchlorato complex [Mn(CO)3(S2CPCy3)(OClO3)] (2a) with NaBH4. This procedure is general and can be used for the preparation of several derivatives containing either manganese or rhenium [M2(CO)6{μ-S2C(H)PR3}2] 5a-d. The reaction of cationic tricarbonyl complexes [M(CO)3(S2CPR3)(PPh3)]PF6 (M = Mn, Re) with NaBH4 produced the same dimers 5a or 5c by displacement of the PPh3 ligand. Treatment of the dimer 5a with excess PEt3 or P(OMe)3 leads to the cleavage of the bridges and loss of one CO and the PR3 group from the S2C(H)PR3 unit to afford ultimately the dithioformate complexes [Mn(CO)2(S2CH)(L)2] [L = PEt3, P(OMe)3].
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    URL: http://dx.doi.org/10.1002/cber.19961291221
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    Zinkorganische Phosphaniminato-Komplexe mit Heterocuban-StrukturHerrn Prof. Dr. Armin Berndt zum 60. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1621-1625 
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    ISSN: 0009-2940
    Keywords: Organo-zinc compounds ; Phosphaneiminato complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organo-Zinc Phosphaneiminato Complexes with Heterocubane StructureThe organo-zinc heterocubanes [ZnR(NPMe3)]4 with R = CH3 (1) and n-C4H9 (2) were prepared by the reaction of [ZnBr(NPMe3)]4 with MeLi and nBuLi, respectively, in hexane solution. In a similar reaction of nBuLi with [ZnI(NPMe3]4 the phosphaneiminato complex [Zn4I(nBu)4(NPMe3)3] (3) is formed. 1-3 were characterized by IR, NMR and MS spectroscopy, and by crystal-structure determinations. 1 and 2 possess heterocubane structures in which the zinc atoms are linked via μ3-N bridges of the phosphaneiminato groups, and all bond angles in the Zn4N4 core are close to 90°. A distorted heterocubane structure is observed for 3 with one of the NPMe3 moieties replaced by an iodine atom.
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    On the Synthesis of Sulfoxonium Ylides: New Aspects of the Chemistry of 1,3-Dithietane 1,1,3,3-Tetraoxide and 1,3,5-Trithiane 1,1,3,3,5,5-Hexaoxide (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 161-167 
    Details
    ISSN: 0009-2940
    Keywords: Sulfoxonium ylides ; 1,3-Dithietane 1,1,3,3-tetraoxide, silylated ; 1,3,5-Trithiane 1,1,3,3,5,5-hexaoxide, silylated ; Disulfenes, unsaturated ; Disulfenes, dianions of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sulfoxonium ylides 3a-h were synthesized by silylation of the cyclic methylene disulfones 1,3-dithietane 1,1,3,3-tetraoxide (1) and 1,3,5-trithiane 1,1,3,3,5,5-hexaoxide (4) with the silylating agents silyl nonafluorobutanesulfonates. The structure and constitution of the ylides were established with 1H-NMR, 13C-NMR, 29Si-NMR spectroscopy, mass spectrometry, and elemental analysis. On the route to the sulfoxonium ylides a new class of unsaturated disulfenes 7, 8, 12, 13 of 1 and 4 were synthesized via Knoevenagel and substitution reactions. Dianions of newly formed alkyl disulfenes 16a, b, e, f, and the trianion 17 were prepared and characterized by 1H-NMR and 13C-NMR spectroscopy and compared with the results of the ylides.
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    Addition von CS2 und anderen Heteroallenen an die 16-Elektronen-Osmium(0)-Komplexe trans-[OsCl(NO)(PiPr2R)2] (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 405-410 
    Details
    ISSN: 0009-2940
    Keywords: Osmium(0) complexes ; Nitrosyl complexes ; CS2, COS, SCNPh, and Ph2C=C=O as bidentate ligands ; Protonation and methylation reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Addition of CS2 and Other Heteroallenes to the 16-Electron Osmium(0) Complexes trans-[OsCl(NO)(PiPr2R)2]The coordinatively unsaturated 16-electron compounds trans-[OsCl(NO)(PiPr2R)2] (1: R = iPr; 2: R = Ph) react with CS2 and COS to form the 1:1 adducts [OsCl(NO){κ2(C,S)-S=C=S}(PiPr2R)2)] (3, 4) and [OsCl(NO){κ2(C,S)-S=C=O}-(PiPr2R)2] (6, 7), respectively. While compounds 3, 4 are inert toward PMe3, the Os(COS) complexes 6, 7 react with tri-methylphosphane by abstraction of sulfur to give (OsCl(NO)-(CO)(PiPr2R)2] (8, 9). From 1 or 2 and phenylisothiocyanate the corresponding 1:1 adducts (OsCl(NO){κ2(C,S)-S=C=NPh}(PiPr2R)2] (10, 11) are obtained. Protonation and methylation reactions of 10 (R = iPr) with HBF4 or CF3SO3Me lead, by addition of the electrophile to the C=N nitrogen atom, to the formation of [OsCl(NO){κ2(C,S)-S=CNHPh}-(PiPr3)2]BF4 (12) and [OsCl(NO){κ2(C,S)-S=CN(Me)Ph}-(PiPr3)2]CF3SO3 (13). Treatment of 1 with diphenylketene yields [OsCl(NO){κ2(C,O)-O=C=CPh2}(PiPr3)2] (14). The X-ray structure analyses of 10 and 14 confirm the coordination of phenylisothiocyanate via S and C and of diphenylketene via O and C, respectively.
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    8-quinolylcyclopentadienyl, a ligand with a tailored fit for chelate complexes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 459-463 
    Details
    ISSN: 0009-2940
    Keywords: Cyclopentadienes ; Half-sandwich complexes ; Intramolecular nitrogen donors ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 8-Lithioquinoline reacts with 2,3,4,5-tetramethylcyclopentenone to give 8-quinolylcyclopentadiene (1/2) after acidic workup and treatment with ammonia. Two of the possible three isomers are formed; the acidic protons on the Cp rings show unusual downfield shifts in the 1H-NMR spectra. Treatment with strong bases led to the intensely coloured anionic 4 which was converted into the trimethylsilyl derivative 5. This is a suitable starting compound for the trihalotitanium and -zirconium compounds 6 and 7. The two complexes were investigated by crystal structure analyses. In both cases the quinolyl nitrogen atom is coordinated to the metal.
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    Über das Silaethen tBu2Si=C(SiMe3)2 und die Struktur sowie Reaktivität seines [4 + 2]-Cycloaddukts mit Ph2C=OFrau Prof. Marianne Baudler zum 75. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 471-478 
    Details
    ISSN: 0009-2940
    Keywords: Silaethenes ; [4 + 2] Cycloadditions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: On the Silaethene tBu2Si=C(SiMe3)2, and the Structure and Reactivity of Its [4 + 2] Cycloadduct with Ph2C=OFrom tBu2SiF—CLi(SiMe3)2 by LiF elimination only Me2Si= C(SiMe3)(SiMetBu2) (1b) instead of tBu2Si=C(SiMe3)2 (1a) is isolated. With benzophenone, silaethene 1b (from its THF adduct 1b · THF) forms at -78 °C a yellow [4 + 2] cycloadduct (5) and a colorless [2 + 2] cycloadduct (6). With increasing temperature 5 transforms into 6, and 6 transforms -more slowly - into the yellow [4 + 2] cycloadduct (7) of 1a and Ph2CO. It follows from this that the migration equilibrium 1a ⇄ 1b really exists. The structure of 7 shows a planar —O—CPh=C6H5-framework with the cycloadded atoms Si and C from -tBu2Si—C(SiMe3)2- located above the plane. The =C6H5—C bond (1.62 Å) is exceptionally long. 7 is a source for 1a which is trapped by acetone (formation of an ene product) and by benzaldehyde [formation of a [2 + 2] cycloadduct, unstable against cycloreversion into PhHC=C(SiMe3)2 and tBu2SiO-containing substances]. Reaction of 7 with trimethylsilyl azide, less reactive than acetone or benzaldehyde, leads - by way of 1a which transforms into 1b - to a trapping product of 1b (formation of a [3 + 2] cycloadduct, unstable against transformation into (RMe2Si)(Me3Si)CN2 with R = (Me3Si)2N, or cycloreversion into (tBu2MeSi)(Me3Si)CN2 and Me2SiNSiMe3-containing substances). Reaction of 1b or 1b · THF with acetone leads only to an ene reaction product of 1b. This means, that only undetectable amounts of 1a or 1a · THF are in equilibrium with 1b or 1b · THF. A minor substance which is shown by NMR at low temperatures besides 1b or 1b · THF is interpreted as a rotamer of 1b or 1b · THF.
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    Organophosphorus Compounds, 112Part 111: Ref.[1].. Lewis Acid Mediated Spirocyclotrimerization of Kinetically Stabilized Phosphaalkynes - Key Step for the Selective Generation and Trapping of Triphospha Dewar BenzenesDedicated to Professor H. W. Roesky on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 489-494 
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    ISSN: 0009-2940
    Keywords: Phosphaalkynes ; Phosphaalkenes ; Spirocyclotrimerization ; Triphospha Dewar benzenes ; Phosphaalkyne cyclooligomers ; Cage compounds, phosphorus-carbon ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In the presence of Lewis acidic derivatives of group 13 elements, phosphaalkynes 7 undergo spirocyclotrimerization with incorporation of the corresponding Lewis acids to form 10a-f. Scope and limitations of this novel cyclooligomerization process are examined. Starting from the spirocyclotrimer 10a reaction with the Lewis base dimethyl sulfoxide, we have in hand for the first time a method for the selective generation of two isomeric triphospha Dewar benzene derivatives (18, 19). Both can be trapped efficiently by further reaction with the phosphaalkyne to furnish the two novel phosphaalkyne cyclotetramers 20 and 21, both still possessing a phosphorus-carbon double bond. In the case of 21, further functionalization of the phosphaalkene unit is possible by [3 + 2] cycloaddition with a nitrile oxide (→ 23).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290504
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    Self-Assembly of Substituted 6-Hydroxy-trans-3-hexenoic Acids - Formation of Extended Ribbon-Like Structures by Hydrogen Bonds (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1029-1034 
    Details
    ISSN: 0009-2940
    Keywords: Hydrogen bonding ; Hydroxy carboxylic acids, self-assembly of ; Crystal engineering ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The substituted 6-hydroxy-trans-3-hexenoic acids 2a and 2b are prepared by an organometallic template reaction involving a sequence of CC coupling reactions between a CO2 equivalent, butadiene, and 3-cyclopenten-1-one or 3,4-diphenyl-3-cyclopenten-1-one, respectively. In the crystal 2a assembles to form an infinite ribbon-type structure, exhibiting an alternating array of 12 and 18 atom-containing loops. The former are each constructed by an alternating CO2H/OH/CO2H/OH sequence, originating from four different monomeric units, that are linked together by means of hydrogen bonds. Two complementary ribbons of 2a are connected by van der Waals interactions to form staples that constitute the microscopic building blocks of the true (2a)n structure in the crystal. Stacks of cyclopentene π bonds are oriented inside the columnar structure of 2a. Acid 2b also forms a related ribbon-like assembly in the solid state. Here the bulky 3,4-diphenylcyclopentadienylidene moieties are oriented laterally at the ribbons, and van-der-Waals interactions with adjacent ribbons construct a three-dimensional hydroxyhexenoic acid network.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290909
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    Preparation and Structure of Dithioxo- and Diselenoxophosphoranes Stabilized by Intramolecular Coordination with a Dialkylamino GroupDedicated to Prof. Dr. Marianne Baudler on the occasion of her 75th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1049-1055 
    Details
    ISSN: 0009-2940
    Keywords: Dithioxophosphoranes ; Diselenoxophosphoranes ; Internal coordination ; Steric protection ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Some dithioxophosphoranes 3 stabilized by intramolecular coordination with a dialkylamino group were prepared, and their structures were analyzed by X-ray crystallography involving [2,4-di-tert-butyl-6-(isopropylmethylamino)phenyl]- (3c), {2,4-di-tert-butyl-6-[(dimethylamino)methyl]phenyl}- (3f), and {2,4-di-tert-butyl-6-[2-(dimethylamino)-1,1-dimethylethyl]phenyl}dithioxophosphorane (3h). The bond between the phosphorus atom and the aromatic ring is flexible and the angle narrows with decreasing ring size of the intramolecular coordination. The 31P-NMR signals are shifted to higher field with increasing ring size of the intramolecular coordination or strength of coordination. Similarly, the corresponding diselenoxophosphoranes 4 were prepared. Both their 31P- and 77Se-NMR signals are shifted to higher field with increasing contribution of intramolecular coordination.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290912
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    Structural Studies on Indium and Tin Thiobenzoates (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1093-1098 
    Details
    ISSN: 0009-2940
    Keywords: Indium tris(thiobenzoate) ; Triethylammonium tetrakis(thiobenzoato)indate ; Tin, butyl-, tris(thiobenzoate) ; Tin, dichloro-, bis(thiobenzoate) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Indium(III) and tin(IV) thiocarboxylates were prepared and characterized on the basis of their IR, 13C- and 19Sn-NMR data. Indium tris(thiobenzoate) (1) decomposes into a sulfido complex In (S)[S(O)CPh] (2a). The corresponding tris(thioacetate) In[S(O)CMe]3 is thermally too unstable to be isolated. The anionic tetrakis complex [Et3NH]{In[S(O)CPh]4} (3) was characterized by X-ray crystallography which revealed a distorted tetrahedral coordination at the In atom. X-ray diffraction analysis of the complexes BuSn[S(O)CPh]3 (4) and Cl2Sn[S(O)CPh]2 (7) showed distorted tetrahedral and cis-octahedral structures, respectively.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290918
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    Reaktionen des Tripod-Co-Templats CH3C(CH2PPh2)3Co(II) mit funktionalisierten HydrazinenMax Herberhold zum 60. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1107-1113 
    Details
    ISSN: 0009-2940
    Keywords: Tripod ligands ; Hydrazines, substituted ; Diazenes ; Cobalt(III), fivefold coordination of ; Cobalt(II), fivefold coordination of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The coordination behaviour of ligands having the same basic constitution RN=NC(=X)R′ (X = O, NR″, S) in their tripod cobalt derivatives has been analyzed. The ligands themselves may be considered as neutral heterodiene compounds and are in this respect vinylogues to diazenes RN=NRy′. Two- electron reduction of these neutral species results in dianionic heterosubstituted heteroolefins RN- -N=C(X-)R′. Due to their redox ambiguity the oxidation state of the metal M in chelate complexes is not a priori evident. Compounds tripod [5: X, R′ = O, Ph; 6; (X, R′) = (py); 7: X, R′ = S, NH2] are best described as containing low-spin Co(III) and dianionic ligands. Co(II) species are obtained with diethyl azodicarboxylate EtOOCN=NCOOEt as the ligand. In the mononuclear compound, with only one nitrogen and one carbonyl oxygen of the ligand acting as donor groups, the neutral ligand is coordinated to give the high-spin cobalt(II) species tripod (8). In the dinuclear compound 9 with both of the nitrogen atoms and carbonyl groups involved in coordination the dianionic ligand bridges two high-spin cobalt(II) centers to give tripod (9) as a derivative with two fused five-membered chelate rings. In addition to the conventional analytical techniques X-ray structure analyses, cyclovoltametric measurements, magnetic susceptibility and ESR data are used to characterize the compounds.
    Additional Material: 3 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19961290921
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    Übergangsmetall-Stannyl Komplexe, 10[1]. Molybdocen- und Wolframocen-Derivate mit zwei unterschiedlichen Liganden der 4. Hauptgruppe (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1131-1142 
    Details
    ISSN: 0009-2940
    Keywords: Stannyl complexes ; Plumbyl complexes ; Tungsten complexes ; Molybdenum complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transition-Metal Stannyl Complexes, 10 - Molybdocen and Wolframocen Derivatives with Two Different Main-Group-4 LigandsReactions of Li[Cp2MSnPh3] (M = Mo, W) with CH3I, BuBr, PhCH2Br, PhC(O)Cl or Br(CH2)nBr (n = 4,5) yield Cp2M(R)SnPh3 [R = CH3, Bu, CH2Ph, C(O)Ph, (CH2)nBr], while tBuBr or CH3C(O)Cl give the hydrido complexes Cp2M(H)SnPh3. A silyl stannyl complex is only obtained from Li[Cp2WSnPh3] and Me3SiOSO2CF3, but not with Me3SiCl or from the anionic Mo complex. In contrast, the reactions of chlorostannanes provide the bis(stannyl) complexes Cp2M(SnR′3)SnPh3 or Cp2M(SnR′2Cl)SnPh3. R/Cl exchange at the tin atom is observed when an excess of the chlorostannane is used. Upon reaction of Li[Cp2MSnPh3] with Ph3PbCl only Cp2M(PbPh3)SnPh3 is formed, while a mixture of Cp2M(PbMe3)SnPh3 and Cp2M(PbMe2Cl)SnPh3 is obtained with Me3PbCl due to redistribution reactions. The structures of Cp2W(SnPh3)C(O)Ph, Cp2W(SnPh3)SntBu2Cl and Cp2W(SnPh3)PbMe2Cl were determined by X-ray structure analyses.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19961290924
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    Thietane and Selenetane Complexes by Thermal Cycloaddition of Vinyl Ethers to Transition-Metal-Coordinated Thio- and Selenoaldehydes - Crystal Structure of Pentacarbonyl(7-phenyl-2-oxa-8-thiabicyclo[4.2.0]octane-S)tungsten(0)Dedicated to Professor Max Herberhold on the occasion of his 60th birthday (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1169-1175 
    Details
    ISSN: 0009-2940
    Keywords: Thioaldehyde complexes ; Selenoaldehyde complexes ; Thietane complexes ; Selenetane complexes ; Rearrangements ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pentacarbonyl(thiobenzaldehyde)tungsten und pentacarbonyl(selenobenzaldehyde)tungsten (1a and 1b) undergo a thermal [2 + 2] cycloaddition with several vinyl ethers to give highly substituted transition metal-coordinated thietanes and selenetanes. The addition is highly regio- and stereospecific. The products undergo acid-catalyzed rearrangements, which lead to thermodynamically more stable diastereomers of the thietanes and selenetanes. The stereochemistry of both addition and rearrangement was established by reaction of deuterium-labeled vinyl ethers and by reaction of the cis and trans isomers of ethyl propenyl ether. The crystal structure of the bicyclic addition product of 1a and 3,4-dihydro-2H-pyran is reported.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291005
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    Zinc Complexes of Amino Acids and Peptides, 9[Part 8: Ref.[1].]. Coordination of Cysteine and Histidine Derivatives to the Pyrazolylborate-Zinc Unit (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1251-1257 
    Details
    ISSN: 0009-2940
    Keywords: Zinc complexes ; Cysteine ligands ; Histidine ligands ; Imidazole ligands ; Pyrazolylborate ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Highly substituted pyrazolylborate ligands TpR,Me were used to limit the coordination number of zinc towards cysteine- and histidine-derived coligands. Monodentate thiolate attachment (→ 1a-f) was achieved with N- and C-protected cysteine, monodentate carboxylate attachment (→ 3) with N-protected histidine. C-protected cysteine was found to form a five-membered N,S-chelate ring (2). While imidazole coordination with N- and C-protected histidine could not be achieved, cationic pyrazolylborate-zinc-coligand complexes [TpZn-L]+ (4a, b) were obtained for L = 2-methylimidazole. The new complexes were characterized by their spectra and three structure determinations.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291017
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    Organmetallic Selenolates, IVPart III: Ref.[1].. Reactions of MSeW(CO)3cp (M=Li, Na) with Organodi- and -tetrahalides - X-ray Crystal Structures of C6H5CH2W(CO)3(η5-C5H 5), μ-[m-C6H4{CH2SeW(CO)3(η5-C5H5)}2], μ-[p-C6H4{CH2SeW(CO)3- (η5-C5H5)}2], and C6H5CH[SeW(CO)3(η5-C5H5)]2 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1275-1279 
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    ISSN: 0009-2940
    Keywords: Organotungsten selenolates ; 77Se NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organotungsten-selenolato complexes were prepared in moderate yields by insertion of selenium into the alkali metaltungsten bonds of MSeW(CO)3cp (M = Li, Na) and subsequent reactions with the organohalides o-, m-, and p- C6H4(CH2Br)2, C6H5CHBr2, m-C6H4(CHBr2)2 and C6H5CCl3. The 77Se-NMR data of the new complexes are discussed and compared with those of related complexes derived from organomonohalides. Moreover, the X-ray crystal structures of C6H5CH2W(CO)3cp (1), μ-[m-C6H4{CH2SeW(CO)3cp}2] (3), μ-[p-C6H4{CH2SeW(CO)3cp}2] (4), and C6H5CH[SeW-(CO)3cp]2 (5) were determined. In complex (1), the W-CH2 bond length is 2.374 Å; the W-Se bond lengths in the complexes 3, 4 and 5 are all in the range 2.625-2.655 Å, corresponding to W-Se single bonds.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291021
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    Masthead (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961291101
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    Suzuki-Coupling of Cp*Ru(para-C6H4Br2) with Phenyl Boronic Acid: A Model Reaction for the Synthesis of Organometallic PolymersDedicated to Professor Günter Szeimies with gratitude on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1323-1325 
    Details
    ISSN: 0009-2940
    Keywords: Suzuki coupling ; π Complexes, organometallic ; π Complexes, dihaloarene ; Ruthenium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of a terphenyl derivative complexed by the cationic moiety Cp*Ru+ by Suzuki coupling of [Cp*Ru(BrC6H4Br)]OTf with phenyl boronic acid under catalysis of Pd(PPh3)4 in a DME-water mixture at 85°C in quantitative yield is reported. The stable coupling product 3 was characterized by X-ray crystal structure analysis.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291103
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    Molecular Gymnastics of Alkynes Orchestrated by Ruthenium Complexes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1313-1322 
    Details
    ISSN: 0009-2940
    Keywords: Vinylidene complexes ; Allenylidene complexes ; Ene type reactions ; Atom economial reactions ; Reconstitutive additions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ruthenium complexes catalyze a variety of addition or isomerization reactions that are highly atom economical. Terminal alkynes react with allyl alcohols to form β,γ-unsaturated ketones that can be readily isomerized to α,β-unsaturated ketones via transient vinylidene complexes. A cyclization via a transient allenylidene complex concomitant with this addition represents a novel way to build heterocycles. Ancillary studies with these catalysts revealed an internal oxidation reduction whereby allyl alcohols are isomerized to saturated ketones and propargyl alcohols are isomerized to α,β-unsaturated carbonyl compounds. Consideration of the reaction mechanism led to a general Alder ene type reaction wherein alkynes serve as the enophile and alkenes serve as the ene component. These discoveries have led to a number of efficient total syntheses of biologically interesting targets. Mechanistic investigations into the activation of a ruthenium complex led to the discovery of a novel bis-homo-Diels-Alder reaction of 1,4-cyclooctadiene.
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    URL: http://dx.doi.org/10.1002/cber.19961291102
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    A Theoretical Study of Thionitrosyl Azide (N3—N=S), Thiazyl Azide (N3—S≡N) and Nitrosyl Azide (N3—N=O) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1373-1377 
    Details
    ISSN: 0009-2940
    Keywords: Thionitrosyl azide ; Thiazyl azide ; Nitrosyl azide ; Tetranitrogen sulfide ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Stimulated by the recent detection of nitrosyl azide (N3—N=O), we investigated the stability of the sulfur analogues thionitriosyl azide (N3—N=S) and thiazyl azide (N3—S≡N) by using ab initio MO calculations up to the QCISD(T)/6-311+G(d)//QCISD/6-311G(d) + ZPE level. Both azides have a similar energy content. While thionitrosyl azide is not stable with respect to N2 elimination, thiazyl azide resists to this process by an energy barrier of about 110 kJ/mol. The NS and N3 fragments resulting from homolytic cleavage lie about 100 kJ/mol above the azides. The five-membered ring is thermodynamically much more stable than both azides but kinetically unstable with respect to cheletropic decomposition yielding N2S + N2. Overall, trans-thiazyl azide is the most likely candidate for experimental observation of, for example, the reaction of NS+ salts with the azide anion. IR wavenumbers of the azides were also predicted.
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    URL: http://dx.doi.org/10.1002/cber.19961291110
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    Synthese, Eigenschaften und Kristallstrukturen der Titan(III)-Amido-Komplexe Ti[N(SiMe3)2]3, [TiCl2{N(SiMe3)2}(THF)2] und [Na(12-Krone-4)2][TiCl2{N(SiMe3)2}2] (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1401-1405 
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    ISSN: 0009-2940
    Keywords: Amido complexes ; Titanium(III) compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Syntheses, Properties, and Crystal Structures of the Titanium(III) Amido Complexes Ti[N(SiMe3)2]3, [TiCl2{N(SiMe3)2}(THF)2], and [Na(12-Crown-4)2][TiCl2{N(SiMe3)2}2]TiCl3(THF)3 reacts with NaN(SiMe3)2 to furnish [TiCl2{N(SiMe3)2}(THF)2] (1), whereas in the presence of 12-crown-4 the ionic amido complex [Na(12-crown-4)2][TiCl2{N(SiMe3)2}2] (5) is obtained besides [Na(12-crown-4)2][TiCl4(THF)] (4). On the other hand, the titanium(III) amido complex Ti[N(SiMe3)2]3 (2), the crystal structure of which was solved, reacts with NaN(SiMe3)2 in the presence of 12-crown-4 with deprotonation of one of the methyl groups to give the carbometalated complex [Na(12-crown-4)2][Ti{N(SiMe3)2}2{N(SiMe 3CH2)}] (3).
    Additional Material: 4 Ill.
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    Masthead (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240101
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    Addition von Alkenen an 5-(Trifluormethyl)-1,3,2,4,6-dithiatriazin (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 39-45 
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    ISSN: 0009-2940
    Keywords: 1,3,2,4,6-Dithiatriazines ; CNS Polycycles, structure determination ; Calculations, MNDO ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Addition of Alkenes to 5-(Trifluoromethyl)-1,3,2,4,6-dithiatriazinesDechlorination of 1,3-dichloro-5-(trifluoromethyl)-1,3,2,4,6-dithiatriazine (1) with Ph3Sb gives (CF3CN3S2)n (2) in quantitative yield. By 1,3-addition of alkenes (dicyclopentadiene, cyclopentene, cis- and trans-2-butene, propene, and ethene) to 2 the corresponding penta- (4a), tri-(5a), and bicyclic ring systems 6a, 6b, 7, 8a, 8b, and 9 are prepared in 65-85% yields. The molecular structures of 6a and 7 were determined by single-crystal X-ray analysis; the other structures were derived from NMR data. The NMR analyses are in accordance with MNDO calculations. For 4a and 5a only the thermodynamically favoured anti-isomers are found, as expected from these calculations; for 6 and 8 they show satisfactory agreement for anti/syn-proportions as determined by NMR spectroscopy. The product distribution corresponds to a symmetry-allowed alkene addition to a singlet dithiatriazine.
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    URL: http://dx.doi.org/10.1002/cber.19911240107
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    Synthese und Eigenschaften von 1,2,4,3-Thiadiazaboretidinen. Kristallstruktur des 2,4-Di-tert-butyl-3-phenyl-1,2,4,3-thiadiazaboretidins (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 47-50 
    Details
    ISSN: 0009-2940
    Keywords: Sulfur diimides ; 1,3-Cycloaddition, reductive ; 1,2,4,3-Thiadiazaboretidines ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Properties of 1,2,4,3-Thiadiazaboretidines. Crystal Structure of 2,4-Di-tert-butyl-3-phenyl-1,2,4,3-thiadiazaboretidineReaction of sulfur diimides with alkyl(aryl)bis(methylthio)boranes leads to reductive 1,3-cycloaddition of the NSN sequence with formation of the 1,2,4,3-thiadiazaboretidines 2a-g. NMR (1H, 11B, 13C, 15N, 29Si), mass spectra and the results of the X-ray analysis of 21 are reported and discussed. The 11B chemical shifts have been calculated for 3-phenyl-1,2,4,3-thiadiazaboretidine and some related model compounds by the IGLO method and correlate acceptably with the experimental values.
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    URL: http://dx.doi.org/10.1002/cber.19911240108
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    Metallatome in der Synthese von Metallclustern, II1) Reaktionen von substituierten Cyclopentadienen und Nickelocen mit Nickel- und Eisenatomen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 301-308 
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    ISSN: 0009-2940
    Keywords: Metal atom synthesis ; Clusters ; Electrochemistry ; Cyclic voltammetry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Atoms in the Synthesis of Metal Clusters, II1). - Reactions of Substituted Cyclopentadienes and Nickelocene with Nickel and Iron AtomsBy vaporizing nickel atoms into solutions of tert-butyl-substituted cyclopentadienes in methylcyclohexane mononuclear sandwich compounds (1, 4, and 6 as main products) as well as tri- and tetranuclear clusters are prepared. With mono- and di-tert-butyl-substituted cyclopentadienes as ligands the new clusters 2 and 5 are obtained. In the reaction with 1,2,4-tri-tert-butylcyclopentadiene 6 is the only observed product. Hindered rotation around the metal-ligand bond vector is observed for 4 even at room temperature. When treating 1 with nickel atoms cluster 2 is formed, indicating some importance of 1 during the formation of 2 in the above reaction. Clusters 2 and 5 contain hydrido ligands, which could be identified in the case of tris(1,3-di-tert-butyl-η5-cyclopentadienyl)trinickel dihydride (5) by a single crystal structure determination as μ3-H bridges. A tetrahedral structure is found for the cluster 2 by X-ray crystallography. With the aid of MS, IR, magnetic measurements, and cyclovoltammetric investigations 2 is identified as a mixture of 2a and 2b bearing one or three bridging hydrogens, respectively. In general 2a, 2b, and 5 show a rich redox chemistry with reversible redox couples between -2 and +2. Reaction of iron atoms, nickelocene, and mesitylene in methylcyclohexane at -120°C leads unexpectedly to cluster 3, tetrakis(η5-cyclopentadienyl)tetranickel trihydride and a not yet identified (η5-cyclopentadienyl)mesityleneiron complex. Possible formation routes for 1-6 are discussed.
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    1,8-Bis(diphenylphosphino)anthracene and Metal Complexes1) (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 333-336 
    Details
    ISSN: 0009-2940
    Keywords: Phosphine ligand ; Anthracene ; Nickel(II) complexes ; Palladium(II) complexes ; Cyclometallated chelate complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The title compound 4 was synthesized from dipotassium 1,8-anthracenedisulfonate (9) and potassium diphenylphosphide (Ph2PK). On reaction of 4 with nickel(II) chloride and bis-(benzonitrile)palladium(II) chloride, cyclometallation of the C - H bond in anthracene 9-position led to the square-planar chelate complexes 11 and 13, respectively. In the case of the palladium complex 13, the cyclometallated structure was proved by X-ray structure analysis. Treatment with aqueous potassium cyanide did not remove nickel from 11, but converted 11 into 12 by substitution of chloride with cyanide, demonstrating the high stability of these cyclometallated chelate complexes.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19911240214
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  • 187
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    Untersuchungen zum Reaktionsverhalten von Benzocyclopropen unter Yb(fod)3-Katalyse (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 353-356 
    Details
    ISSN: 0009-2940
    Keywords: Benzocyclopropene ; 1,3-Dihydroisobenzofurans ; Yb(fod)3 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Experiments Concerning the Reactions of Benzocyclopropene under Yb(fod)3 Catalysis1,3-Dihydroisobenzofuran derivatives 3a - e and 5a - c are obtained by reactions of α,β-unsaturated carbonyl compounds with benzocyclopropene (1). The yields increase by addition of Yb(fod)3. Aromatic aldehydes react in the same way. Yb(fod)3 has no influence on the reactions of α,β-unsaturated hydrazones with 1.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240217
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  • 188
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    Synthese heterocyclischer Dialkine und deren Umsetzung mit CpCo(CO)2 (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 357-363 
    Details
    ISSN: 0009-2940
    Keywords: Heterodiynes, medium-sized ; [2.2](2,5)-Thiophenophanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis of Heterocyclic Diynes and their Reaction with CpCo(CO)2The preparation of the heterocyclic diynes 1,6-dithia-3,8-cyclodecadiyne (1b), thia-3,8-cyclodecadiyne (11), 1-thia-6-selana-3,8-cyclodecadiyne (12), oxa-3,8-cyclodecadiyne (13), 1,6-dioxa-3,8-cyclodecadiyne (14), 1-oxa-6-thia-3,8-cyclodecadiyne (15), 1,6-diselena-3,8-cyclodecadiyne (26), thia-3,9-cyclounde-cadiyne (22a), thia-3,13-cyclopentadecadiyne (22b) and its selena analogues 23a, 23b is described. The thia and monoselena compounds are obtained by a thia- or selenacyclization of the corresponding dibromides. Compound 26 has been obtained by a Misumi coupling reaction. The thiacycloalkadiynes of medium-sized rings (10, 11) react with CpCo(CO)2 to yield [2,2](2,5)thiophenophane derivatives. Acyclic thiadialkynes or thiacycloalkadiynes of larger ring size (22b) with CpCo(CO)2 by [2 + 2 + 2] cycloaddition.
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    URL: http://dx.doi.org/10.1002/cber.19911240218
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  • 189
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    A New Route to Alkoxy Radicals  -  Photochemical Reactions with (Alkylperoxy)cobaloximes (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 387-390 
    Details
    ISSN: 0009-2940
    Keywords: Peroxy compounds ; Cobaloximes ; Oxygen insertion ; Radicals, alkoxy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Alkoxy radicals have been generated by photochemical reactions of (alkylperoxy)cobaloximes 1. The occurrence of alkoxy radicals has been proved by characteristic cyclization and β-scission reactions of the reactive intermediates.
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    URL: http://dx.doi.org/10.1002/cber.19911240223
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  • 190
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    On the Electronic Structure of Phosphabutatriene and Related Phosphacumulenes. A Theoretical Study (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 271-274 
    Details
    ISSN: 0009-2940
    Keywords: Phosphacumulenes ; Cumulenes ; Calculations, MNDO, SCF ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The title compound phosphabutatriene possesses two energetically closely spaced frontier orbitals, as in methylenephosphane and in phosphaallene. They are built up from the π system or the s̰ orbital of phosphorus by interaction with neighboring π bonds. The extension of these frontier orbitals over all (heavy) atoms makes self-dimerization to different cyclobutane derivatives feasible. Substituent effects on the ordering of s̰ and π are analyzed. Vibrational analyses indicate P=C vibrations of low intensity which decrease with increasing length of the heterocumulene chain. The analysis is extended to the two next higher homologs, which are hitherto experimentally unknown.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19911240205
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  • 191
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    Dioxirane Epoxidation of α,β-Unsaturated Ketones (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 227-232 
    Details
    ISSN: 0009-2940
    Keywords: Epoxidation ; Dioxiranes ; Ketones, α,β-unsaturated ; (E)-Chalcones ; (E)-2′-Hydroxychalcones ; 2-Cycloen-1-ones ; Caroate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of epoxides 3a - r is achieved in excellent yields by reaction of the α,β-unsaturated ketones 1a-c, 4,4′-disubstituted (E)-chalcones 1d-o, and 2′-hydroxy-4-substituted (E)-chalcones 1p - r with isolated dimethyldioxirane (2a) (as acetone solution) and/or in situ generated ethyl(methyl)dioxirane (2b). This method constitutes a useful alternative to the Weitz-Scheffer epoxidation (alkaline H2O2) of such electronpoor substrates.
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    URL: http://dx.doi.org/10.1002/cber.19911240134
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  • 192
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    Umlagerungen von 5,5,6,6-Tetraalkyl-2-norbornyl-Kationen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 241-245 
    Details
    ISSN: 0009-2940
    Keywords: 2-Norbornyl cations, 5,5,6,6-tetramethyl- ; Tetracyclo[4.2.2.12,5.01,6]undec-3-yl cations ; Wagner-Meerwein rearrangements ; Alkyl-bridged ions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Rearrangements of 5,5,6,6-Tetraalkyl-2-norbornyl CationsWhen the 6,6-dimethyl-2-norbornyl cation (9) is generated from the tosylhydrazone 5 by way of the diazonium ion 8, a 2H label is distributed equally between positions 1 and 2 of the exo-alcohol 10. The degeneracy of 9, previously derived from solvolytic studies, is thus confirmed for the deaminative route. 5,5,6,6-Tetramethyl-2-norbornanone (25) and tetracyclo[4.2.2.12,5.01,6]undecan-3-one (31) are prepared by using Diels-Alder methodology. The corresponding tosylhydrazones 26 and 32 are employed as precursors for the 5,5,6,6-tetramethyl-2-norbornyl and tetracyclo[4.2.2.12,5.01,6]undec-3-yl cations (11 and 12). Again, the distributions of 2H labels are close to 1 : 1. The angular distortions expected from repulsive interactions of the methyl groups in 11 and from cyclobutane annulation in 12 do not affect the relative energies of the bridged ions.
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    URL: http://dx.doi.org/10.1002/cber.19911240137
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  • 193
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    Verschiedenartige Koordinationen bei η2-Alken)-(η5-cyclopentadienyl)organylnickel(II)-Komplexen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 441-452 
    Details
    ISSN: 0009-2940
    Keywords: (η2-Alkene)(η5-cyclopentadienyl)organylnickel(II) complexes, stability and reactivity of ; Cyclopentadienyl ligands, substituted ; Chelating alkenylcyclopentadienyl ; Nickel complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Various Coordinations in (η2-Alkene)(η5-cyclopentadienyl)organylnickel(II) ComplexesA series of (η2-alkene)(η5-cyclopentadienyl)organylnickel(II) complexes with substituted cyclopentadienyl ligands is synthesized in order to compare the structures, the thermal stabilities, and chemical reactivities. In (allyl)(η5-Cp')Ni compounds the allyl moiety is η3-coordinated when Cp'=C5H5, C5Me5 (1), C5Ph5 (2), indenyl (3), [Hydridotri(pyrazolyl)borato] (4) (as an equivalent of the cyclopentadienyl ligand), and [C5H4((CH2)3CH=CH2)] (22). It is found that the [(η2-alkene)alkyl(η5-Cp')nickel] compounds [Cp'=C5Me5; alkene=C2H4, alkyl=Me (10), Et (9) or alkene=(1 - 2-η2)-1,3-butadiene, alkyl=Me (11); Cp'=C5Ph5; alkene=C2H4, alkyl=Me (12)] are thermally more stable and less reactive than their η5;- C5H5 analogues; the largest increase in thermal stability is observed when the η5-Cp' and the η2-alkene functions are connected by substitution of the cyclopentadienyl ligand with an alkenyl group of suitable chain length. In the case of compounds of the general type [(η5-C5R4((CH2)nCH=CH2))-(ligand)Ni(II)] with Ph3P as the ligand these complexes are cationic [R=H, n=3 (14+) or R=Me, n=2 (17+)]. On the other hand, the compounds with anionic ligands are neutral complexes (R=H, n=3, ligand=methyl (19), ethyl (20), isopropyl (21) or R=Me, n=3 and ligand=iodide (24), bromide (25), methyl (26), ethyl (27)]. In 14+, 17+, 19 - 21 and 24 - 27 the C=C bond of the alkenyl group is η2-coordinated to the nickel atom. X-ray structures have been determined for 4 and 25.
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    Medizinisch interessante Metallchelate, I. 99mTc-Komplexe mit sechszähnigen Tribrenzkatechin-Liganden (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 481-486 
    Details
    ISSN: 0009-2940
    Keywords: Tris[3-(2,3-dihydroxyphenoxy)propyl]amine hydrochloride containing ; 99mTc uptake ; Technetium, radiopharmaceutical ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Chelates of Medical Interest, I. - 99mTc Complexes with Hexadentate Tricatechol LigandsThe tricatechol ligand tris[3-(2,3-dihydroxyphenoxy)propyl]-amine hydrochloride, TRIPACE (9), is prepared from tris(3-chlorpropyl)amine (5) and the potassium salt of 2,2-dimethyl-1,3-benzodioxol-4-ol (7). This ligand is capable of reducing the 99m[TcO4]- ion to lower valent 99mTc and subsequent complexation of the reduced 99mTc ion. The structures of 5 and of tris[3-(2,2-dimethyl-1,3-benzodioxol-4-yloxy)propyl]amine (8) are determined by X-ray diffraction.
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    Steuerung der Aggregation von Mangankomplexen durch unterschiedliche Basen an den Beispielen [Mn(O2CCF3)2(py)4] und [Mn3(O2CCF3)6(benz)6] (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 515-517 
    Details
    ISSN: 0009-2940
    Keywords: Manganese complexes ; Aggregation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Influencing the Aggregation of Manganese Complexes by Different Bases: Formation of [Mn(O2CCF3)2(py)4] and [Mn3(O2CCF3)6(benz)6]Manganese powder reacts quantitatively with trifluoroacetic acid to yield Mn(O2CCF3)2 (1). The aggregation of 1 is directed by different N-containing bases. Pyridine (py) forms the mono-nuclear complex [Mn(O2CCF3)2(py)4] (2), while benzonitrile (benz) yields the trinuclear complex [Mn3(O2CCF3)6(benz)6] (3). The X-ray structures of 2 and 3 are described.
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    URL: http://dx.doi.org/10.1002/cber.19911240316
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    Darstellung von [Dimethylamino(thiocarbonyl)thioamido]titan(IV)-dihalogeniden - Verbindungen mit kurzen Ti - N-Bindungen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 523-526 
    Details
    ISSN: 0009-2940
    Keywords: Titanium complexes ; Short bonds, Ti - N ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Preparation of [Dimethylamino(thiocarbonyl)thioamido]titanium(IV) Dihalides - Compounds with Short Ti - N BondsReaction of Me2NC(S)SN(SiMe3)2 (1) with TiCl4 and TiBr4 yields (2) and (3). Treatment of 2 and 3 with pyridine (py) leads to the solvates · 3 py [2a (X=Cl), 3a (X=Br)]. These adducts have been characterized by X-ray structure determination.
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  • 197
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    The Conformational Behaviour of 10-Substituted Spiro[4.5]decanes (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 551-561 
    Details
    ISSN: 0009-2940
    Keywords: Conformational analysis ; Spiro[4.5]decanes ; Allylboration, transition state models ; Ketals, chiral, cleavage by Lewis acids ; Calculations, MNDO and SYBYL ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The conformational behaviour of 10-X-substituted 1,4-dioxa-and 1,4,6-trioxaspiro[4.5]decanes 1 - 4 has been studied by 13C-, 19F- and 1H-NMR spectroscopy. Two X-ray analyses (of 2a,e) are presented, and their implications to cleavage reactions of chiral acetals are discussed. Participation of twist boat forms in the conformeric equilibrium of at least 1c has been made plausible by observing 13C,19F-NMR coupling constants. The ratios of axial to equatorial conformer in 1 - 4 have been calculated by molecular mechanics.
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    URL: http://dx.doi.org/10.1002/cber.19911240322
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    Darstellung von dreikernigen Carbonylmanganaten sowie deren Reaktionsprodukten mit InCl3; Röntgenstrukturanalysen von K3[Mn3(μ-CO)2(CO)10], [(C6H5)4As]2[(μ-H)Mn3(μ-CO)10], [{(C6H5)3P}2N]2[μ-H)Mn3(CO)12], [(C6H5)4As]2[{μ-H)Mn3(CO)12}2(μ4-In)] und [(C6H5)4As]2[{(μ-H)Mn3(CO)12}(μ3-In){Mn(CO)5}Cl] (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 453-463 
    Details
    ISSN: 0009-2940
    Keywords: Manganates, carbonyl, trinuclear ; Indium-manganese clusters ; Spiro cluster ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis of Trinuclear Carbonylmanganates and Their Reaction Products with InCl3; X-ray Structure Determinations of K3[Mn3(μ-CO)2(CO)10], [(C6H5)4As]2[(μ-H)Mn3(μ-CO)10], [{(C6H5)3P}2N]2[μ-H)Mn3(CO)12], [(C6H5)4As]2[{μ-H)Mn3(CO)12}2(μ4-In)] und [(C6H5)4As]2[{(μ-H)Mn3(CO)12}(μ3-In){Mn(CO)5}Cl]Mn2(CO)10 reacts with KOH in aqueous solution to give the potassium carbonylmanganate K3[Mn3(μ-CO)2(CO)10] (1). The trianion 1 is isoelectronic with Fe3(CO)12 and is protonated with methanol to form the μ-hydrido cluster [(μ-H)Mn3;-(CO)12]3⊖, which is precipitated with [{(C6H5)3P}2N]Cl as [{(C6H5)3P}2N]2[(μ-H)Mn3(CO)12] (2), whereas the carbonyl-bridged μ-hydrido species [(μ-H)Mn3(μ-CO)2(CO)10]2⊖ seems to be trapped as the [(C6H5)4As]⊕ salt 3. The reaction of 3 with InCl3 yields the Mn-In clusters [(C6H5)4As]2[{(μ-H)Mn3(CO)12}2;-(μ4-In) (4) and [(C6H5)4As]2[{(μ-H)Mn3(CO)12}(μ3-In){Mn(CO)5}Cl] (5). X-ray structure analyses have been carried out for the compounds 1 - 5.
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    Neue σ2λ3-P=C - O-Systeme: Stabile nichtkonjugierte Phosphaalkenether - Synthese und Reaktionen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 493-496 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkene ethers ; 1,3-Oxaphospholes, dihydro- ; 1,3-Oxaphosphorines, tetrahydro- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New σ2λ3-P=C - O Systems: Stable Non-Conjugated Phosphaalkene Ethers - Synthesis and ReactivityNon-conjugated cyclic phosphaalkene ethers (2, 4, 6) are obtained by cyclocondensation of (2- or 3-hydroxyalkyl)phosphanes 1, 3 with N-arylpivalimidoyl chlorides. Hydrolysis of 2, 4 with H2O (→7, 8), addition of hydrogen compounds (HCl, HSPh, MePhPH) (→ 9-12), and oxidation with air (→ 14) are studied. The reactivity of the title compounds and of benzoxaphospholes are compared.
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    URL: http://dx.doi.org/10.1002/cber.19911240312
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    Verhalten von cis;-2-Boryl-1-stannylalkenen gegenüber (Dimethylamino)trimethylstannan, Methoxytrimethylstannan und Methanol - Aufbau neuer Zinn - Element-Bindungen, Beispiele für Lösungsmittel-gesteuerte Reaktionen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 503-508 
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    ISSN: 0009-2940
    Keywords: cis;-2-Boryl-1-stannylalkenes ; Addition reactions ; Exchange reactions ; Solvent-controlled reactions ; Tin - Element bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Behaviour of cis;-2-Boryl-1-stannylalkenes Against (Dimethylamino)trimethylstannane, Methoxytrimethylstannane, and Methanol - Formation of New Tin - Element Bonds, Examples of Solvent-Controlled ReactionsWhen alkene derivatives1 [Me3Sn(R1)C=C(R)BR2], with the trimethylstannyl- and the dialkylboryl group in cis position at the C=C double bond, are treated with (dimethylamino)-trimethylstannane (4), methoxytrimethylstannane (5), or methanol, the product distribution depends remarkably on the solvent [hexane or tetrahydrofuran (THF)]. In hexane, 1a, b (R1=H, R=Et, Pr) react with 4 to give the B-dimethylamino compounds 6a, b in high yields as a result of addition and rearrangement. Other derivatives 1 do not react with 4 in hexane. Under the same conditions in hexane some alkenes 1 react with 5 to yield the B-methoxy derivatives 8, which are analogous to 6. A complex mixture of various products is obtained from the reaction of 1 with methanol in hexane. If the same reactions are carried out in THF, many compounds 1 react with 4 and 5 to eliminate tetramethyltin and give dihydro- 1,2,5-azonia- (7) or dihydro-1,2,5-oxoniastannaboratoles (9), respectively. The reaction with methanol in THF also leads to the oxonia-stannaboratoles 9, this time by elimination of methane. Pure samples of compound 9g are obtained as the crystalline THF adduct 9g-THF. A mechanism is proposed involving adduct formation at the boryl group, followed by intramolecular reactions depending on the donor quality of the respective solvent.
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    URL: http://dx.doi.org/10.1002/cber.19911240314
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