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  • Inorganic Chemistry  (602)
  • 1995-1999  (602)
  • 1950-1954
  • 1996  (602)
  • 101
    Electronic Resource
    Electronic Resource
    Control of Regioselectivity in the Transition-Metal-Catalysed Conjugate Additions of Alkylaluminium Compounds and Methyltitanium Ate Complexes to Androsta-1,4-diene-3,17-dione (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 963-966 
    Details
    ISSN: 0009-2940
    Keywords: Steroids ; Androsta-1,4-diene-3,17-dione ; Conjugate addition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: By a variation of the nature of the reagent system conjugate addition to the cross-conjugated steroidal dienone 1 occurs selectively either at C-1 or at the sterically hindered C-5. With Me3Al or Me4AlLi in the presence of catalytic amounts of Cu1 salts, a high regioselectivity (up to 97:3) in favour of position 1 is achieved. Application of ate complexes of aluminium and titanium in the presence of Ni(acac)2 as catalyst, however, leads to a reversal of the regioselectivity in favour of position 5 (up to 11:89). Aluminium and titanium ate complexes are efficient reagents in the Ni(acac)2-catalysed conjugate addition to sterically hindered enones.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290814
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  • 102
    Electronic Resource
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    Komplexe mit Metall-Phosphor-Dreifachbindungen als mögliche Intermediate der Umsetzungen von Chlorophosphiniden-Komplexen mit Metallaten verschiedener ÜbergangsmetalleHerrn Professor Max Herberhold zum 60. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 973-979 
    Details
    ISSN: 0009-2940
    Keywords: M2P2 tetrahedral complexes ; Phosphido ligand complexes as intermediates ; Ni2P4O distorted prismane framework ; CO incorporation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Complexes with Metal-Phosphorus Triple Bonds as Possible Intermediates in the Reactions between Chlorophosphinidenes and Metalates of Various Transition MetalsThe reaction of [{M′(CO)5}2PCl] (M′ = Cr, W) with various metalates ([Cp′Mo(CO)3]-, [Cp * Ni(CO)]-, [Cr2(CO)10]2-) yields the M2P2 tetrahedral complexes [(MLn)2(μ,η2- P2){M′(CO)5}2] (MLn = Cp*Ni, M′= Cr (1), W (2); MLn = Cp′Mo(CO)2, M′ = Cr (4); Cp* = η5-C5Me5, Cp* = η5C5H3tBu2) and the cyclo-P4 compound [{Cr(CO)4}(η4-P4){Cr(CO)5}4] 6. As side products the distorted prismane [(Cp*Ni)2{μ4,η4-(P2-O-P2)}{W(CO)5}2] 3 and the diphosphino-methanone complex [{Cp′Mo(CO)2}2{μ4η2-PC(O)P}-{Cr(CO)5}2] 5 are formed. The complexes are characterised by NMR, IR, MS, and X-ray structure analysis (1-5). Studying the reaction pathway provided evidence of phosphido intermediates of the type [LnM≡P→M′Ln].
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290816
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  • 103
    Electronic Resource
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    Synthesis, Molecular Structure and Reactions of Stable Square-Planar 16-Electron Ruthenium(0) Complexes: trans-[RuCl(NO)(PR3)2]⋆ (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1007-1013 
    Details
    ISSN: 0009-2940
    Keywords: Ruthenium(0) complexes ; Nitrosyl complexes ; Oxidative addition reactions ; Dioxygenruthenium complexes ; Sulfur dioxide, metal-assisted oxidation of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reduction of [RuCl3(NO)(PPh3)2] (1) with Zn/Cu generates [RuCl(NO)(PPh3)2] that by ligand exchange with PR3 (R3 = iPr3, iPr2Ph) affords the stable 16-electron ruthenium (0) complexes trans-[RuCl(NO)(PR3)2] (2, 3). The X-ray structural analysis of 2 confirmed the square-planar geometry around the metal center. HCl oxidatively adds to 2 and 3 to give the octahedral ruthenium(II) compounds [RuHCl2(NO)(PR3)2] (4, 5). On treatment of 2 and 3 with CO, TCNE, CH2 (generated from CH2N2) and O2, five-coordinate 1:1 adducts [RuCl(NO)(L)(PR3)2] (6-12) are formed. The dioxygen complexes 11 and 12 react with SO2 to afford the sulfatoruthenium(II) derivatives [RuCl(NO){η2(O,O)-O2SO2}(PR3)2] (13, 14). Compound 13 (R3 = PiPr3) has been characterized by X-ray structural analysis.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290906
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  • 104
    Electronic Resource
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    Synthesis and Dynamic Behavior of the Dimeric, Monocyclic Barium Bis[bis(isopropyldimethylsilyl)phosphanide] - Molecular Structures of P(SiMe2Ph)3, of Monomeric (thf)4Ba[P(SiMe2iPr)2]2 and of the Dimer {(thf)2Ba[P(SiMe2iPr]2]2}2 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1035-1040 
    Details
    ISSN: 0009-2940
    Keywords: Phosphanes ; Bis(silyl)phosphanes ; Tris(silyl)phosphanes ; Phosphanides ; Barium bis(phosphanide) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Barium bis[bis(trimethylsily)amide] metalates bis(isopropyldimethylsilyl)phosphane (1) to yield nearly quantitatively the corresponding barium bis[bis(isopropyldimethylsilyl)phosphanide] (3). This compound shows a temperature-dependent monomer-dimer equilibrium in toluene solution. Both the isomers were characterized by X-ray crystal structure analyses. The monomeric derivatives precipitate as a tetrakis(tetrahydrofuran) complex with a P-Ba-P bond angle of 139.9°. The barium atoms of the monocyclic, centrosymmetric dimer are pentacoordinated by two tetrahydrofuran molecules, one terminal and two bridging phosphanide ligands. The endo- and exocyclic Ba-P distances with values of 332 and 316 pm, respectively, lie within the characteristic range.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290910
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  • 105
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    Dithio and Thiono Esters, 62Part 61: K. Hartke, S. Barrmeyer, J. Prakt. Chem., in press.. Reactions of Alkanedithioic Acid Dianions with Iodine, Sulfur, and Tin CompoundsDedicated to Prof. Dr. Kurt Dehnicke on the occasion of his 65th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 663-669 
    Details
    ISSN: 0009-2940
    Keywords: Alkanedithioic acid ; Dithiocarboxylic acid ; 1,2-Dithiine ; 1,2,4-Trithiolane ; 1,2,3,4-Tetrathiane ; 1,3,2-Dithiastannetane ; Thioacyltin sulfide ; Bis(thioacyl)tin sulfide ; 1,2,3,4,5,6-Hexathiepane ; 1,2,3,5,6,7-Hexathiocane ; 1,2,3,5,6-Pentathiepane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The monoanion of the alkanedithioic acid 1a is oxidized with hypervalent iodine compounds to form the 1,2-dithiine 6, the monoanion of 1b yields the 1,2,4-trithiolane 7 and the dianions 2b, c furnish the 1,2,4,5-tetrathianes 3b, c. With diphenyltin or dimethyltin dichlorides 8 the monoanions of 1b, c afford the monothioacyl or bisthioacyl organotin sulfides 10a-c or 11a, b respectively. When treated with lithium hexamethyldisilazane, 10b undergoes an intramolecular cyclization to the 1,3,2-dithiastannetane 9b; 10a is deprotonated by triethylamine to the 1,3,5-trithia-2-stanninane 13. The dianion 2c reacts with diphenyltin dichloride 8 to yield the 1,3,2-dithiastannetane 9d, with dimethyltin dichloride the 1,2,4-trithiolane 16 is formed. 9d is cleaved by thionyl chloride, sulfur dichloride, and disulfur dichloride to give a complex mixture of the 1,2,4,5-tetrathiane 3c and the cyclic polysulfides 1,2,3,4,5,6-hexathiepane 18, 1,2,3,5,6,7-hexathiocane 19 and the 1,2,3,5,6-pentathiepane 20 in varying amounts. Reaction of the dianion 2b with thionyl chloride leads to the formation of the 1,2,4,5-tetrathiane 3b as main product; byproducts are cyclic polysulfides, the 1,2,3,5,6-pentathiepane 21 and the 1,2,3,4,5,6-hexathiepane 22.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290612
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  • 106
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    Zweikernige Tripod-Cobalt-Komplexe mit verbrückenden 1,4,5,8-Tetraoxonaphthalin und 1,4,9,10-Tetraoxoanthracen-Liganden: Strukturen, spektroskopische, magnetische und elektrochemische EigenschaftenHerrn Prof. Dr. R. Gleiter zum 60. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1115-1122 
    Details
    ISSN: 0009-2940
    Keywords: Tripod ligands ; Dinuclear cobalt complexes ; Dihydroxynaphthoquinones ; Dihydroxyanthraquinones ; Magnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Dinuclear Tripod Cobalt Complexes with Bridging 1,4,5,8-Tetraoxonaphthalene and 1,4,9,10-Tetraoxoanthracene Ligands: Structures, Spectroscopic, Magnetic, and Electrochemical PropertiesThe syntheses, structures, optical, magnetic, and redox properties of dinuclear tripodcobalt(II) complexes [tripod = CH3C(CH2PPh2)3] with briding 1,4,5,8-tetraoxonaphthalene 12- and 1,4,9,10-tetraoxoanthracene 22- are described. UV/Vis/NIR spectroscopy indicates interaction between the ligand and the metal orbitals. The magnetic interactions involving the two cobalt(II) centers and the bridging ligand are characterized by EPR spectroscopy and magnetic measurements and are analyzed in terms of qualitative Molecular Orbital calculations. The redox chemistry of these complexes is investigated by cyclic voltammetry and interpreted as metal-based oxidations and ligand-based reductions.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290922
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  • 107
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    The Thermally Induced Solid-State Polymerization Reaction in HalogenoacetatesDedicated to Prof. Günther Klar on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1123-1129 
    Details
    ISSN: 0009-2940
    Keywords: Halogenoacetates ; Solid-state reactions ; Polyglycolide ; Thermal analysis ; Polymerization ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Nine salts of halogenoacetic acids MOOC-CH2—X were prepared and characterized by their thermochemical reactivity. It was found that in seven cases elimination of MX led to polymerization of the organic part of the molecule. The resulting polyester, polyglycolide, could be isolated easily by washing the reaction product with water. It has a distinct porous morphology. The reaction takes place at moderate temperatures (100—200°C).
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290923
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  • 108
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    Hydride Fluxionality in Transiton Metal Complexes: An Approach to the Understanding of Mechanistic Features and Structural Diversities (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1143-1155 
    Details
    ISSN: 0009-2940
    Keywords: Fluxionality, hydride ; Hydride fluxionality ; Transition metal complexes ; Dynamics, intramolecular ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mechanisms of intramolecular dynamics in transition metal hydride complexes are surveyed in this review. The NMR data for a number of fluxional hydrides are interpreted in terms of principal and secondary topological changes of the coordinated ligands. The principal ligand motions can be further categorized as being of migratory (M) and replacement (R) type. Discussion of these ligand motions is followed by analysis of more complex rearrangements of hydride systems, in which both types are operative in multiple exchange processes. The attempted systematic approach appears to be a useful general mechanistic concept for the understanding of the fluxional behavior of hydride complexes.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961291002
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  • 109
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    Silver(I) Sandwich Complexes of Oxa-Crowned Derivatives of Dithiomaleonitrile (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 807-814 
    Details
    ISSN: 0009-2940
    Keywords: Silver(I) sandwich complexes ; Crown dithioethers, unsaturated ; Bis(methylthio)maleonitrile ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The coordination chemistry of the four oxa-crowned derivatives of dithiomaleonitrile mn-12S2O2, mn-15S2O3, mn-18S2O4, and mn-21S2O5 as well as of the acyclic bis(methylthio)maleonitrile mn-S2 with AgI was investigated by X ray structural and spectroscopic methods. The 2:1 complexes (ligand/AgI) [Ag(mn-12S2O2)2]PF6, [1]PF6, [Ag(mn-15S2O3)2]PF6, [2]PF6, and [Ag(mn-S2)2]PF6, [6]PF6, and the 1:1 complexes [Ag(mn-15S2O3)]ClO4, [3]ClO4, [Ag(mn-18S2O4)]PF6, [4]PF6, and [Ag(mn-21S2O5)]PF6 [5]PF6, were obtained with AgPF6 or AgClO4 in MeOH. The stoichiometry of the macrocyclic AgI complexes and the coordination mode of mn-S2On+1 coronands (n = 1-4) is determined by the length of the macrocyclic oligoethylene chain. - The mn-crown dithioethers mn-12S2O2 and mn-15S2O3 form with AgPF6 the new sandwich complexes [Ag(mn-12S2O2)2]PF6, [1]PF6, and [Ag(mn-15S2O3)2]PF6, [2]PF6. [1]PF6 crystallises in the triclinic space group P1. In the centrosymmetric cation [1]+ each mn-12S2O2 ligand is coordinated to the AgI centre in an endo manner via both S atoms and one O atom. The distance of the second O atom of mn-12S2O2 to AgI is somewhat longer than a normal Ag-Oether bond. The overall environment around AgI in [1]+ is that of a distorted cubic S4O4 set of donors. [2]PF6 crystallises in the monoclinic space group C2/c. In the centrosymmetric cation [2]+ silver(I) is planar-coordinated by the four S atoms of both mn-15S2O3 molecules. The six O atoms of both mn-15S2O3 ligands show only long-range interactions to the AgI ion. They surround AgI almost vertically to the planar S4 set of donors in a crown-like manner. - The crystal structures of the 1:1 complexes [Ag(mn-18S2O4)]PF6, [4]PF6, and [Ag(mn-21S2O5)]PF6, [5]PF6, consist of linear chain polymers. [5]PF6 forms an N-bridged chain polymer of endocyclic [Ag(mn-21S2O5)]+ units with S1O4NNitrile coordination at the AgI centre. In the 2:1 complex [Ag(mn-S2)2]PF6, [6]PF6, each mn-S2 acts as a monodentate NNitrile donor. - 13C-NMR studies in nitromethane solution confirm that the AgI ions in the complexes of the mn-crown dithioethers remain coordinated. However, the AgI ion in complex of mn-S2 is decoordinated.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290711
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  • 110
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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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290715
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  • 111
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    Contributions to the Chemistry of Boron, 233Part 232: Ref.[1].. Reactions of a 1,2,3,4-Diphosphadiboretane with Some Carbonylmetal CompoundsDedicated to Professor Kurt Dehnicke on the occasion of his 65th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1233-1241 
    Details
    ISSN: 0009-2940
    Keywords: 1,2,3,4-Diphosphadiboretane-tetracarbonyliron complexes ; 1,3,2,4-Diphosphadiboretane-tetracarbonylchromium complexes ; 1,2,3,4-Diphosphadiboretane, isomerisation of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,2-Di-tert-butyl-3-(diisopropylamino)-4-(dimethylamino)- 1,2,3,4-diphosphadiboretane (1) reacts with Fe2(CO)9 to give two isomeric tetracarbonyliron complexes 2, 3 with P-Fe bonds and a bis(tetracarbonyliron) complex 4. In contrast, 1 displaces the olefinic ligand from tetracarbonyl(η4-norbornadiene)metal (metal = Cr, Mo) to form the tetracarbonylmetal complexes 5 and 6 with a rearranged ligand molecule, i.e. a 1,3,2,4-diphosphadiboretane. This process is accompanied by a change of the tert-butyl groups from an anti orientation in 1 to a syn orientation in 5 as shown by X-ray crystallography.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961291015
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  • 112
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    Reactive E=C [p-p]π Systems, 45[Part 44: See ref.[1].]. 1-Aza-3,4-diphospholenes by [3 + 2] Cycloaddition of 2-(Diisopropylamino)phosphaethyne to Diazo Derivatives R1R2C=N2Dedicated to Professor Max Herberhold on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1271-1274 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkyne ; [3 + 2] Cycloaddition ; 1-Aza-3,4-diphospholenes ; Diphosphiranes ; 1-Aza-3,4-diphospholes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of the (diisopropylamino)phosphaethyne (1) with diazo compounds of the type R1R2C=N2 (2a-2c) unexpectedly leads in high yields (60-90%) to the 1-aza-3,4-diphospholene derivatives 3a-3c, a new class of heterocycles. NMR investigations of the analogous reaction of 1 with diazocyclopentadiene 2d show that the multi-step formation of 3a-3c proceeds via the 1-aza-3,4-diphospholes 6a-6d as intermediates.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961291020
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  • 113
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    Crystal Structure of a Representative Mixed Adduct of Trimethylaluminium and a Lithium Amide and a Theoretical MO Study on Model Systems (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1293-1300 
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    ISSN: 0009-2940
    Keywords: Calculations, ab initio ; Aluminium compounds ; Heterometallic compounds ; Lithium compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of the simple alane adduct [Me3Al · HN(CH2Ph)2] (2) with the lithium amide [(PhCH2)2NLi] leads to the formation of the mixed adduct [Me3Al · (PhCH2)2NLi · HN(CH2Ph)2] (1). The crystal structures of 1 and 2 are reported. Exhibiting a four-membered, mixed-metal, mixedanion ring-core, the structure of 1 is unusual in containing a monomeric lithium dibenzylamide fragment. Such fragments generally convert to aza-allyl derivatives, so its existence here can be attributed to the stabilising effect of the attached Me3Al ligand. Crystalline 2 adopts the classical, distorted-tetrahedral arrangement of simple monomeric alane adducts. Ab initio MO calculations on model systems show that mixed adduct formation from Me3Al and Me2NLi is exothermic, while further reaction to give Me2AlNMe2 and MeLi (i.e., complete transmetallation) is endothermic.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961291024
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  • 114
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    Cyclobutadiene Complexes, XII. Alkynyl-Substituted Tricarbonyl(cyclobutadiene)iron Complexes: Stille Coupling of Iodocyclobutadiene Complexes with Stannylalkynes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1311-1311 
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    ISSN: 0009-2940
    Keywords: Alkynylation ; Palladium catalyzed coupling reactions ; Cyclobutadiene complexes ; Iron complexes ; Cobalt complexes ; Modular chemistry ; 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.19961291027
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  • 115
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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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  • 116
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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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    The Synthesis, Structural Analysis and Magnetic Properties of a New Mixed Metal Ferrite Ba3Fe24Ti7O53 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1441-1445 
    Details
    ISSN: 0009-2940
    Keywords: Ferrite ; Iron oxide ; Titanate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new mixed metal titanate Ba3Fe24Ti7O53, 1 was obtained by heating stoichiometRic mixtures of BaCO3, Fe3O4 and TiO2 to 1375°C for 48 h. Compound 1 was characterized by single crystal x-ray diffraction analysis. Two of the barium ions lie in a network of channels in the bc crystallographic plane. The iron and titanium atoms were refined in a random distribution in 16 independent MO6 octahedral sites and 2 MO4 tetrahedral sites. Magnetization measurements reveal a strong magnetic ordering up to 600 K. M vs. H loop measurements show no hysteresis effects.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291207
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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.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291210
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    The Interlocking of Salicylic Aldehydes and Ketones with a 2h-1,2,4,3-Triazaphosphole (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1493-1495 
    Details
    ISSN: 0009-2940
    Keywords: Phosphorus heterocycles ; ortho-Hydroxybenzaldehydes ; Phosphonic amide ; Michaelis-Arbuzov rearrangement ; Hydrogen bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Salicylic aldehyde (2a) adds to 2-methyl-5-phenyl-2H-1,2,4,3-triazaphosphole (1) to yield the bicyclic phosphonic amide 3a. The OH group adds to the P=N bond, the carbon atom the carbonyl group is inserted into the other P - N bond, and the phosphorus atom is oxidized. In the crystal the compound forms dimers by a double hydrogen bond between two HN-PO units. Substituted salicylic aldehydes as well as ortho-hydroxyacetophenone and benzophenone react in the same way.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291215
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    Mixed Bent Sandwich Titanium Complexes with the [2-(Diisopropylamino)ethyl]cyclopentadienyl Ligand  -  Catalysts for the Polymerization of Ethylene and the Dehydrocoupling of Phenylsilane (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1509-1515 
    Details
    ISSN: 0009-2940
    Keywords: Substituted metallocene complexes ; N-Functionalized cyclopentadienyl ligands ; Ethylene polymerization ; Dehydrocoupling of phenylsilane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mixed bent sandwich titanium (IV) complexes containing the donor-substituted [2-(diisopropylamino)ethyl]cyclopentadienyl (C5H4CH2CH2NiPr2 ≡ CpN) ligand are described. The highly moisture-sensitive metallocene dichloride (C5H4CH2CH2NNiPr2)(C5H4SiMe3)TiCl2 (1) was synthesized by reaction of CpNLi with CpSTiCl3 (CpS ≡ C5H4SiMe3). Complex 1 reacts with one equivalent of HCl with protonation of the amino group to give the air- and water-stable metallocene dichloride-hydrochloride [(C5H4CH2CH2-N(H)iPr2)(C5H4SiMe3)TiCl2]+Cl- (2). The structure of 2 was determined by a single-crystal X-ray diffraction study. Compounds 1 and 2 are precursors for ethylene polymerization catalysts. The reaction of 2 with one equivalent of Na+B[3,5-(CF3)2C6H3]4- afforded the borate [(C5H4CH2CH2N(H)iPr2)-(C5H4SiMe3)TiCl2]+B[3,5-(CF3)2C6H3]4- (3). The dimethyl compounds (C5H4CH2CH2NiPr2)(C5H4SiMe3)Time2 (4) was obtained by reaction of 1 with two equivalents of methyllithium. The diphenoxy complex (C5H4CH2CH2-NiPr2)(C5H4SiMe3)Ti(OPh)2 (5) was prepared analogously with a stoichiometric amount of lithium phenoxide. Compounds 4 and 5 show remarkable activity in the catalytic dehydrocoupling of phenylsilane.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291218
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    Reactions of (CF3)2BNMe2 with ω-Halonitriles  -  Crystal and Molecular Structure of [cyclo-C3H4(CN)](CF3)2B·NHMe2Dedicated to Professor Peter Sartori on the occasion of his 65th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1541-1545 
    Details
    ISSN: 0009-2940
    Keywords: Dimethylaminobis(trifluoromethyl)borane ; Nitriles ; Cyclopropanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Dimethylaminobis(trifluoromethyl)borane, (CF3)2BNMe2 (A), reacts with Cl(CH2)3CN to yield [Cl(CH2)2CH(CN)](CF3)2B·NHMe2 (1) whereas Br(CH2)3CN and A combine in a 1:2 ratio to form [cyclo-C3H4(CN)](CF3)2B·NHMe2 (2) and Br(CF3)2B·NHMe2. Br(CH2)nCN and A yield [Br(CH2)n-1 CH-(CN)](CF3)2B·NHMe2, n=4 (3), n=5 (4) and n=6 (5). Compound 2 and (NCCH2)CF3)2B·NHMe2 can be alkylated at nitrogen with CH3I/KOH in ether to yield [cyclo-C3H4(CN)]-(CF3)2B·NMe3 (6) and (NCCH2)(CF3)2B·NMe3 (7), respectively. treatment of 1 and 3 with hydroxide in ether gives the respective five- and six-membered heterocycles (CF3)2 (8) and (9). Reduction of the nitrile group with (iBu)2Alh in CH2Cl2 at -50°C followed by hydrolysis furnishes the corresponding aldehydes (OCHCH2) (CF3)2B·NMe3 (10), [cyclo-C3H4(CHO)](CF3)2B·NMe3 (11) and (12). The structure of 2 was determined by an X-ray investigation.
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    URL: http://dx.doi.org/10.1002/cber.19961291222
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    Synthesis, Structure and Conformation of cis- and trans-(μ-1,6-Dimethylheptalene)bis(tricarbonyliron) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1569-1572 
    Details
    ISSN: 0009-2940
    Keywords: Heptalenes ; Carbonyliron complexes ; cis and trans complexation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of 1,6-dimethylheptalene (2) with Fe2(CO)9 affords two binuclear iron complexes 4a and 4b, each bearing two tricarbonyliron moieties, in trans and cis orientation, respectively. The reaction leads additionally to the formation of the monocomplexed compound 3. NMR studies indicate that the heptalene moiety of the new compounds is a π-bond isomer of 2, and this is clearly attributable to steric factors. Single-crystal X-ray structure analyses of the metal complexes 4a and 4b confirm that the Fe(CO)3 fragments adopt trans and cis geometries, respectively, with respect to the plane of the carbocycle. The ring systems of the two isomers adopt different conformations in the solid state. In the case of 4a, a hitherto unknown chair-like conformation is determined, whereas in complex 4b the ring system shows a twisted double boat conformation.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291226
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    Metallkomplexe mit biologisch wichtigen Liganden, LXXXIXPart LXXXVIII: Ref.[1].. Oxidative Addition von elektrophilen α-Aminosäurederivaten an Platin(II)- und Cobalt(I)-Komplexe: α-Übergangsmetallierte AminosäurenHerrn Professor Dr. Hans Georg von Schnering zum 65. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1617-1620 
    Details
    ISSN: 0009-2940
    Keywords: α-Amino acid, α- and β-C-metallated ; Platinum(IV) complexes ; Cobaloxime complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Complexes of Biologically Important Ligands, LXXXIXPart LXXXVIII: Ref.[1]. .  -  Oxidative Addition of Electrophilic Derivatives of α-Amino Acids to Platinum(II) and Cobalt(I) Complexes: α-Transition-Metallated Amino Acids Herrn Professor Dr. Hans Georg von Schnering zum 65. Geburtstag gewidmet.The addition of methyl α-bromohippurate to PtMe2(bipy) gives the α-metallated amino acid derivative (bipy)-Me2(Br)PtC(H)(NHCOPh)(CO2Me) as a mixture of isomers 1a, b of which the trans adduct 1a was characterized by X-ray diffraction. Methyl α-bromohippurate and N-Boc-O-tosylserine methyl ester are added to [Co(py)(DH)]- (DH = dimethylglyoxime, diphenylglyoxime) to give cobalt(III) complexes 2-5 with a cobalt-carbon bond.
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    The First Triisopropylstibane Ruthenium(II) and Ruthenium(0) Complexes Including the X-ray Crystal Structure of [Ru(η3-C3H5)2(SbiPr3)2]Dedicated to Professor Markus Wieber on the occasion of his 60th birthday (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1191-1194 
    Details
    ISSN: 0009-2940
    Keywords: Ruthenium complexes ; Stibane complexes ; Dihydrogen complexes ; Butadiene complex ; π-Allyl complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The hydridoruthenium(II) complexes [RuHCl(H2)(SbiPr3)3] (2) and [RuH2(H2(SbiPr3)3] (3), containing dihydrogen as ligand, were prepared from [RuCl2(C8H12)]n (1) as the starting material. Compound 3 reacts with CO by displacement of H2 to yield [RuH2(CO)(SbiPr3)3] (4) and with C2H4 to give both [RuH2(C2H4)2(SbiPr3)2] (5) and [RuH2(C2H4)(SbiPr3)3] (6), the latter as the more stable and isolable product. Treatment of 3 with propene leads to the formation of [Ru(η3-C3H5)2] (7) while the reaction of 3 with butadiene affords the pentacoordinated ruthenium(0) compound [Ru(η4-C4H6)2(SbiPr3)] (8). The molecular structure of the bis-(allyl) complex 7 was determined by X-ray crystallography.
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    URL: http://dx.doi.org/10.1002/cber.19961291008
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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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    URL: http://dx.doi.org/10.1002/cber.19961291217
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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].
    Additional Material: 1 Ill.
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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 
    Details
    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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    Ethene Polymerization Activity and Coordination Gap Aperture in non-ansa Alkyl-substituted Cyclopentadienyl- and Phospholyl-zirconium/MAO CatalystsDedicated to Prof. Dr. Karl-Heinz Reichert on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1517-1529 
    Details
    ISSN: 0009-2940
    Keywords: Zirconocenes ; Metallocene-methylalumoxane catalysts ; Ethene polymerization ; Structure - reactivity correlation ; Coordination gap aperture ; Cone angles ; 91Zr NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The ethene polymerization activities of a series of Cp'(C5H5)ZrCl2 and Cp'2ZrCl2 pre-catalysts (Cp' = C5HMe4, C4Me4P, C5Me5, C5H4tBu, C5H3-1,3-tBu2, C5H2-1,2,4-tBu3) together with (C5H5)2ZrCl2 have been correlated with the coordination gap aperture. In the case of the mixed substituted C5R5-nR'n ligands, the coordination gap aperture has been determined with the help of the cyclopentadienyl cone angle and the bending angle at zirconium. A hindered rotatability of the tert-butyl substituted systems has been evaluated by molecular modeling calculations and was included in the gap aperture estimation. Deviations from the activity - gap aperture correlation in the case of the phospholyl (C4Me4P) systems could be accounted for in terms of adduct formation between aluminum species and the phosphorus donors. These Lewis acid/base adducts form in an equilibrium reaction at high Al/Zr ratios, as shown by 31P NMR. Ab initio calculations on model L2TiMe+ complexes (L = C5H5, C5H4N and C5H4P) for the insertion of ethene in the Ti—Me bond suggest a high electronic similarity for phospholyl and cyclopentadienyl. The 91Zr-NMR data (chemical shift and line width) for the above zirconocene series are reported. The 91Zr chemical shift values increase with a good linear correlation to the number of methyl or tert-butyl groups, which is traced to the additive electron donating effect of the alkyl groups. The hyperconjugative donor effect of a tert-butyl group is found here to be 1.25 times that of a methyl group. The X-ray structure of (C5H3-1,3-tBu2)(C5H5)ZrCl2 has been determined (monoclinic, P21/n, a = 6.631(3), b = 18.843(9), c = 15.265(5) Å, β = 91.3°, Z = 4).
    Additional Material: 12 Ill.
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    P/O Ligand Systems: Synthesis, Reactivity, and Structure of Tertiary o-Phosphanylphenol Derivatives (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1547-1560 
    Details
    ISSN: 0009-2940
    Keywords: o-Phosphanylphenols ; P,O hybrid ligands ; P asymmetry ; C,O-dilithium reagents ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of C,O-dilithium reagents 1 (M = M′ = Li) or C,O-lithium-sodium reagents 1 (M = Li, M′ = Na) with chlorophosphanes afford C,O-disubstitution products 2 or phosphanylphenolates 3 which are treated subsequently with ClSiMe3 to give 4-methyl- and bulky 4,6-di-tert-butyl substituted o-phosphanylphenol silyl ethers 4. These were applied for the preparation of the corresponding o-phosphanylphenols 5, mainly P-asymmetric derivatives. Limitations and side reactions by use of 1 in the above synthesis are discussed. Acid-base properties, pH-dependent solubility in water/hexane, and substitution reactions at oxygen and phosphorus of selected representatives of 5 are reported. An example for the separation of enantiomers by esterification with (1S)-(—)-camphanic acid chloride is given. IR studies revealed intramolecular P-H—O bonds and 2J(PC) the preferred trans arrangement of the phenoxy group in solution. In the solid state, inter- and intramolecular P-H—O bonds were detected by X-ray structure analysis. The trans arrangement of the phenoxy group is preserved. Because of steric hindrance, the O substituents are tilted towards the phosphorus atom and thus induce large through-space coupling constants. The P-Sn distance of 336.9 pm in the bulky substituted O—SnMe3 moiety 8h is however too large for the formation of genuine intramolecular coordination. The versatility of o-hydroxyarylphosphanes and objectives of further studies are shown by preliminary results on complex formation and applications of these phosphanes in catalysis.
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    URL: http://dx.doi.org/10.1002/cber.19961291223
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    Compounds of Germanium and Tin, 20Part 19: Ref.[1].. Stannylene Complexes of Iron and Nickel without Donor StabilizationDedicated to Professor Alois Haas on the occasion of his 65th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1565-1567 
    Details
    ISSN: 0009-2940
    Keywords: Tin compounds ; Iron complexes ; Nickel complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of [Fe2(CO)9], [Fe3(CO)12] or [Ni(CO)4] with the alkylarylstannylene RR′Sn: [R= 2,4,6-tBu3C6H2, R′ = CH2C(CH3)2-3,5-tBu2C6H3] furnishes the stannylene complexes [(OC)4Fe=SnRR′] (5) and [(OC)3Ni=SnRR′]. The X-ray structure analysis of 5 reveals a trigonal-bipyramidal environment of the iron atom with the tricoordinated tin atom occupying an axial site, thus indicating that RR′Sn: is a strong σ-donor but weak π-acceptor.
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    URL: http://dx.doi.org/10.1002/cber.19961291225
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    Conformation of tripod Metal Templates in CH3C(CH2PPh2)3MLn (n = 2, 3): Neural Networks in Conformational AnalysisDedicated to E. Weiss on the occasion of his 70th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 745-757 
    Details
    ISSN: 0009-2940
    Keywords: Conformational analysis ; Triphos ligands ; Neural networks ; Factor analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The conformational space spanned by tripod metal templates CH3C(CH2Ph2)3M is analysed on the basis of the solid-state structures of 82 tripodCo templates in compounds tripodCoL2 and tripodCoL3. Systematic analysis, including the techniques of conformational space group scatter graphs, principal-component analysis, and partial least squares, reveals a series of basic regularities: The torsion of the phenyl groups is strongly linked to the torsional skew of the bicyclooctane-type framework of the chelate cage. For one sense of this skew there are two classes of low-energy conformation that differ by the helicity of the phenyl arrangement and by the degree of torsional skew in the chelate backbone. From the scatter graphs it is evident that a change in helicity may occur by one- or by two-ring flip mechanisms. The basic regularities found by the above methods are also evident from the analysis of the same data by a neural network approach. The fact that these regularities are found for tripodCoL2 and tripodCoL3, irrespective of the widely different coligands L and crystal environments, means that the conformation of the tripod metal templates is governed by the forces acting within them and not so much by the forces imposed on them by their individual chemical or crystal environment. It is shown that the classifications, although derived from a data basis only containing Co compounds, are characteristic for tripod metal templates irrespective of the specific metal involved.
    Additional Material: 11 Ill.
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    Structural and Electrochemical Comparison of NiII in an N2S2 Plane with Two, One and No Axial Ligands: Isolation and Characterization of a Five-Coordinate Nickel(II) Complex (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 779-784 
    Details
    ISSN: 0009-2940
    Keywords: Thioether, benzyl ; Mercapto amines ; Nickel complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Addition of two equivalents of benzyl bromide to [N,N′-bis(2-mercaptoethyl)-1,5-diazacyclooctane]nickel(II) (Ni-1) produced the green dibenzyl dithioether complex [Ni-1-Bzl2Br2] structurally characterized by X-ray crystallography as a six-coordinate octahedral complex in a monoclinic crystal system and the P21/c space group. Benzylation of the methyl thioether/thiolate [(Ni-1-Me)+I- yielded the mixed benzyl/methyl dithioether [(Ni-1-BzlMe)Br]I, structurally characterized by X-ray crystallography as a five-coordinate square pyramidal nickel(II) complex with a Ni-Br distance of 2.451 Å. The complex crystallizes in the orthorhombic Cmca space group. The latter is the first nickel(II) pentacoordinate complex isolated for the N,N′-bis(2-mercaptoethyl)-1,5-diazacyclooctane (daco) ligand. Structural comparison of these two complexes with the square-planar dimethyl compound [Ni-1-Me2]I2 found an expansion of the N2S2 plane upon addition of axial ligands. The five-coordinate nickel complex showed a displacement of the Ni ion from the N2S2 plane by 0.43 Å toward the axial bromide ligand, a common observation of pentacoordinate complexes of this ligand with metals such as Zn and Fe. Electrochemical studies as well as the X-ray crystal structures for complex [Ni-1-Bzl2Br2] and [(Ni-1-BzlMe)Br]I are presented and discussed in detail.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290708
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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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    Synthesis and Structure of Bis(2,4-di-tert-butyl-1,3-cyclopentadien-1-yl)-disulfane, S2(tBu2C5H3)2, and Bis[2,4-di-tert-butyl-5-(trimethylsilyl)-1,3-cyclopentadien-1-yl]disulfane, S2 [tBu2(Me3Si)C5H2]2 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 69-71 
    Details
    ISSN: 0009-2940
    Keywords: Disulfanes ; Cyclopentadienyl ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of 1,3-di-tert-butylcyclopentadienyllithium and 1,3-di-tert-butyl-4-(trimethylsilyl)cyclopentadienyllithium with S2Cl2 gives bis(2,4-di-tert-butyl-1,3-cyclopentadien-1-yl)di-sulfane (1) and bis[2,4-di-tert-butyl-5-(trimethylsilyl)-1,3-cyclopentadien-1-yl) disulfane (2), respectively. The structure of 2 was determined by single-crystal X-ray diffraction. Compounds 1 and 2 are the first biscyclopentadienylchalcogens with the chalcogen in vinylic position.
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    URL: http://dx.doi.org/10.1002/cber.19961290114
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    Chirale Tripodliganden mit Phosphor- und Schwefeldonoren. Synthese und Komplexchemie (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 97-108 
    Details
    ISSN: 0009-2940
    Keywords: Tripod ligands ; Chiral ; Oligodentate P,S-ligands ; Nickel-sulfur Compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chiral Tripod Ligands with Phosphorus and Sulfur Donors. Synthesis and Complex ChemistryNeopentane based tripod ligands CH3C(CH2X)(CH2Y)-(CH2Z) with mixed donor groups X,Y,Z (PR2, SR, SH) are accessible via two different strategies. The functionalized thietane CH3(CH2X)ČH2SCH2 allows stepwise introduction of P or S donors by substitution of the mesylate function and subsequent nucleophilic cleavage of the thietane ring. Tripod ligands 5 [CH3C(CH2X)(CH2Y)(CH2Z)] with up to three different donor groups (X = SH; Y = PPh2; Z = P(4-Tol)2, SCH2Ph, PPh2) are thus available. As an alternative the neopentane derivatives 8 [CH3C(CH2X)(CH2Y)(CH2Cl)] which are easily assessible from CH3C(CH2OSO2Me)(CH2Br)-(CH2Cl) (7) by stepwise substitution with phosphides LiPAr2 (Ar = aryl) may be transformed to 9 [CH3C(CH2X)(CH2Y)(CH2SBzl)]. Under controlled conditions the S - benzyl bond of 9 is cleaved reductively without concomitant cleavage of P - Ar bonds. Ligand 5a [CH3C(CH2PPh2)2(CH2SH)] reacts with Ni(BF4)2 · 6 H2O to yield the dinuclear species [(CH3C(CH2PPh2)2-(CH2S)Ni)2]2+ (10). The two ligands are bonded in an equivalent way with each of the two nickel centers interacting with one of the two phosphane functions of the ligand; the thiolate functions form μ2-SR bridges between the two nickel atoms. The SCH2 group at the four-membered S2Ni2 ring are in mutual cis position with the four-membered ring bent along the sulfur-sulfur axis by 70°. The internal strain in 10 is analyzed by comparing its structure with the ones of [(CH3C(CH2-PPh2)3NiSPh)2]2+ (11) and [(CH3C(CH2OH)(CH2PPh2)2-NiOH)2]2+ (12).
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290119
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    The First Selective Cage Redistribution Reaction of P4O6Dedicated to Professor Rolf Appel on the occasion of his 75th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 121-124 
    Details
    ISSN: 0009-2940
    Keywords: N-Organyl tetraphosphorus hexaoxide ; Cage redistribution ; Nitrene insertion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of tetraphosphorus hexaoxide with organic azides leads selectively to the cage redistribution products 1 P4O6NPh, 2 P4O6NC2H4Ph, 3 P4O6NSO2CH3, 4 P4O6NC6H13, and 5 P4O6NCO2C2H5 by nitrene insertion. The molecular structure consists of an adamantane-like P4O5N cage with a terminally bound oxygen atom. The P4O5N cagelike structure is confirmed by 31P NMR spectroscopy and X-ray structure analysis. The P4O5N cages of the P4O6NR molecules possess a significant geometrical distortion.
    Additional Material: 4 Ill.
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    Phosphorus Analogs of Bipyridines: Their Synthesis and Coordination ChemistryMost of the work described in this review was done in the laboratory of the authors. The help of many dedicated coworkers and colleagues, whose names are cited in the references, is acknowledged. The unpublished X-ray crystal structure analyses were performed by our colleague Dr. Louis Ricard. Over the years, this program has been supported by CNRS, SNPE and Ecole Polytechnique. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 263-268 
    Details
    ISSN: 0009-2940
    Keywords: 2-(2-Pyridyl)phosphinines ; 2,2′-Biphosphinines ; Transition metals ; Biphosphinine chelates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis and coordination chemistry of 2-(2-pyridyl)-phosphinines and 2,2′-biphosphinines are reviewed. A noteworthy series of homoleptic complexes of 4,4′,5,5′-tetramethyl-2,2′-biphosphinine (tmbp) with Cr(0), Mo(0), Wo(0) and Ni(0) are described. A [Cu(bpy)(tmbp)]+ cationic polymer has been characterized by X-ray analysis. Ruthenium, manganese and rhenium chelates were also obtained. With Mn2(CO)10, a (tmbp)-Mn2(CO)6 complex is formed where tmbp acts as an eight electron donor.
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    Organometallic Group-13 Metal Complexes of d-Block Elements, XIVPart XIII: See ref.[10].. Intramolecularly Base-adduct-stabilized Transition-metal-substituted Indanes: Synthesis and Spectroscopic Characterization, Structure of (η5-C5H5)(CO)Ni—InBr2(NC7H13) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 297-303 
    Details
    ISSN: 0009-2940
    Keywords: Transition-metal indium complexes ; Nickel-indium bonds ; Intramolecular Lewis base adducts ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of InBr/InBr3 or InBr/BrIn[(CH2)3NMe2]2 with the transition metal dimers [L(CO)nM]2 {L = CO, Cp, C5H4[(CH2)2NMe2]; M = Fe, Co, Ni; n = 1-3} in THF or dioxane gives in almost quantitative yield the transition metal indium complexes L(CO)nM—InBr2(Do) (Do = THF, NC7H13) and L(CO)nM—In[(CH2)3NMe2](Br) respectively. The new compounds were characterized by elemental analysis, infrared v(CO) spectroscopy, NMR, and mass spectrometry. An X-ray single crystal structure determination of (η5-C5H5)(CO)-Ni-InBr2(NC7H13) (1a) revealed a short Ni-In bond of 246.3(1) pm.
    Additional Material: 3 Ill.
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    Improved Access to {[ω-(Phosphanyl)alkyl]cyclopentadienyl}cobalt(I) Complexes: Decomplexation of the Phosphane Arm; Alkyne Complexes; Synthesis of Mononuclear Vinylidenecobalt(I) Complexes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 319-325 
    Details
    ISSN: 0009-2940
    Keywords: {[ω-(Phosphanyl)alkyl]cyclopentadienyl}cobalt(I) ; Cobalt complexes ; Bidentate ligand ; Alkynes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An improved synthesis of [(2-phosphanylethyl)cyclopenta-dienyl]cobalt(I) chelate complexes is presented, in which the paramagnetic chloride 3 is a precursor of the ethene complex 4. The latter readily undergoes ligand exchange reactions which in the case of bidendate reagents (1,5-cyclooctadiene, 1,2-bis(diisopropylphosphanyl)ethane, 2,2′-bipyridine, nor-bornadiene) cause a decomplexation of the phosphane arm at room temperature with formation of 7, 5, 6, 8. The ethene ligand in 4 can be replaced by alkynes under equally mild reaction conditions (formation of 9, 11 - 16). The reaction with ethyne results in the formation of vinylidene complex 10. The yields of the reactions with nonaromatic alkynes could be improved by treating 3 with the alkyne in the presence of sodium amalgam. The unsubstituted vinylidene complex 10 and its tert-butyl derivative 17 were obtained by this route in 38 and 40% yield, respectively.
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    Cäsium-Fluor-Vierringe als Strukturmotiv in Cäsium-Triorganofluorometallaten der Gruppe 13Herrn Prof. Dr. Ekkehard Fluck zum 65. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 355-359 
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    ISSN: 0009-2940
    Keywords: Aluminium compounds ; Gallium compounds ; Indium compounds ; Trimethylfluoro metalates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cesium-Fluorine Four-Membered Rings as Structural Motive in Cesium Triorganofluoro Metalates of Group 13The reactions of AlMe3, GaMe3, and InMe3 with CsF in acetonitrile furnish the corresponding trimethylfluoro metalates Cs[Me3MF] (1: M = Al, 2: M = Ga, 3: M = In). The salt-like compounds 1 - 3 were characterized by NMR, IR, and MS techniques as well as by X-ray structure analysis. Cs2F2 four-membered rings are the structure-dominating units in all three compounds. Compound 1 consists of puckered layers of weakly associated Cs2F2 rings parallel to (100), while the four-membered rings in 2 form infinite ladder-type chains. The Cs-F rings in 3 build up a heterocubane with a Cs4F4 core by ring stacking.
    Additional Material: 5 Ill.
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    (tert-Butoxy)aluminium and -gallium HydridesDedicated to Prof. H. W. Roesky on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 381-384 
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    ISSN: 0009-2940
    Keywords: Alanes, tert-butoxy- and bis(tert-butoxy)- ; Gallanes, tert-butoxy- and bis(tert-butoxy)- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The crystal structures obtained by X-ray methods of (tert- butoxy)alane and -gallane (tBuOMH2) are isotypic and are composed of discrete centrosymmetric dimers. The dimers arise from almost symmetrical Al—O—Al [1.810(3), 1.815(3) Å] and Ga—O—Ga [1.902(9), 1.908(9) Å] bridges forming a central rhombohedral four membered M2O2 cycle [O—Al—O 81.0(2)°, O—Ga—O 78.6(5)°] with the metallic atoms in a distorted tetrahedral environment. When one of the hydride ligands on the metals is further substituted by tert-butoxy, the formation of (tBuO)2AlH and (tBuO)2 GaH is observed. These two compounds crystallize in different lattices and space groups, but they are nevertheless very similar in their structure: the centrosymmetric M2O2 cycle is maintained [Al—O 1.817(3), 1.817(3) Å; Ga—O 1.904(4), 1.907(4) Å] As expected, the terminal Al-O [1.675(3) Å] and Ga—O [1.783(4) Å] distances are considerably shorter than the bridging ones.
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    Compounds of Germanium and Tin, 18Part 17: Ref.[1].. Cleavage Reactions of Hexa-tert-butylcyclotrigermane: Racemate versus Conglomerate CrystallizationDedicated to Professor Marianne Baudler on the occasion of her 75th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 401-404 
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    ISSN: 0009-2940
    Keywords: Germanium ; Trigermanes ; Germylene ; Trapping reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of hexa-tert-butylcyclotrigermane (3) with CCl4, Br2, and I2 furnishes the correspondingly substituted 1,3-dichloro- (4), 1,3-dibromo- (5), and 1,3-diiodotrigermanes (6). The symmetries of the molecules of 5 and 6 are very similar (point group C1) revealing gauche-anti conformations and different Ge—Ge bond lengths. However, while 5 crystallizes as a racemate, 6 forms a conglomerate of enantiomerically pure crystals. The X-ray structure analysis of the 1,3-dimethyltrigermane (7) derivative, derived from 6 by a sequence of metalation and methylation reactions, reveals more symmetrical molecules of the point group C2 which also crystallize as a racemate. Irradiation of 3 leads to tetra-tert-butyldigermene (8) and di-tert-butylgermylene (9) which could be trapped by addition and cycloaddition reactions with selenium, tellurium, and 3,5-di-tert-butyl-1,2-benzoquinone.
    Additional Material: 2 Ill.
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    The chemistry of metallacyclic alkenylcarbene complexes, 3Part 2: Ref.[2].. C=C bond formation with carbon nucleophiles. stereoselective dienylation of lithium enolates and cuprates and a novel cascade synthesis of highly substituted cyclopentenones from lithium acetylides (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 427-433 
    Details
    ISSN: 0009-2940
    Keywords: Carbene complexes ; Metallacycles ; Claisen rearrangement ; Cascade reaction ; Cyclopentenones ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The cationic ferracyclic carbene complexes 1 react with carbon nucleophiles like lithium enolates and organocuprates to give the corresponding 4-substituted 1, (3E)-diene tricarbonyl-iron complexes 6 and 9. The reaction is thought to proceed by initial attack on the allyl terminus and subsequent ferra Claisen-Ireland rearrangement of the intermediate (η2 alkene)carbene complex 4. This rationale is supported by the isolation and characterisation of analogous aminooxocarbene derivatives 8. With sterically demanding enolates products 6 are formed in diastereomeric ratios of up to 90:10, thus demonstrating the inductive power of the chiral metallacycle in 1. Lithium acetylides as carbon nucleophiles react with 1 according to a novel cascade to give regio- and stereospecifically 2,5,5-trisubstituted-cyclopentenones 10 suggesting a concerted formation of four C=C bonds together with a CO insertion and a formal carbene transfer step.
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    Zinc complexes of the N,N,S ligand (mercaptophenyl)(picolyl)amine (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 435-440 
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    ISSN: 0009-2940
    Keywords: Zinc complexes ; Sulfur and nitrogen ligands ; Structure and bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The zinc complex chemistry of the tridentate thiol ligand N- (2-mercaptophenyl)(2-picolyl)amine (MPPAH) differs considerably from that of the aliphatic analogue N-(2-mercaptoethyl)(2-picolyl)amine reported previously. This is due to the lower basicity and hence bridging tendency of its aromatic thiolate function. With zinc salts of oxo anions the 1:1 complexes (MPPA)ZnX (1a-c: X = ONO2, OAc, OBz) are formed which according to spectroscopic data are monomeric while the halide (MPPA)ZnBr (2) seems to be polymeric. In the absence of coordinating anions the monomeric 2:1 complex (MPPA)2Zn (3) results which according to a crystal structure determination contains tetrahedral zinc coordinated by one MPPA ligand in a tridentate fashion while the other is only monodentate and sulfur-bound. A similar N2S2 coordination can be deduced for the 1:1:1 complex (MPPA)Zn(STrt) (4) resulting from ZnEt2, MPPAH and triphenylmethanethiol.
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    Reactions of diaminophosphenium and 1,3,2-diazaphospholenium triflates with silver saltsDedicated to Professor Dr. Marianne Baudler on the occasion of her 75th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 465-469 
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    ISSN: 0009-2940
    Keywords: Phosphenium cations ; Silver complexes ; 31P, 109Ag NMR shift correlation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of bis(diisopropylamino)phosphenium triflate (1[CF3SO3]) with silver salts AgY [Y- = CF3CO2- (2a), CF3-SO3- (2b), CH3CO2- (2c)] affords neutral complexes [{(iPr2N)2(Y)P} Ag(OSO2CF3)] (3a-c). While 3a, c are stable up to ambient temperature, 3b is only stable at low temperature and in equilibrium with the cation 1. The constitution of 3a-c was derived from multinuclear (1H, 13C, 31P, 109Ag) NMR spectra. Compound 3a was further studied by X-ray single-crystal diff ractommetry which showed the presence of dimeric units with μ2-bridging triflate ligands and three-coordinate silver atoms with a planar T-shaped coordination geometry. Reaction of 4-chloro-1,3-bis(2,6-dimethylphenyl)-1,3,2-diazaphospholenium triflate (4[CF3SO3]) with 2a, c affords equilibrium mixtures whose 31P- and 109Ag-NMR spectra suggested the presence of silver complexes 5a, c with constitutions similar to those of 3a, c besides unreacted cation 4. No reaction was observed between 4[CF3SO3] and 2b. A common mechanism accounting for the different outcome of the individual reactions will be discussed.
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    Alkali Metal Polyphosphides in Low Dimensions: Synthesis and Structure of [(CH3)4N]2RbP7(NH3) and [(C2H5)4N]Cs2P11 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 155-159 
    Details
    ISSN: 0009-2940
    Keywords: Polyphosphides ; Heptaphosphanortricyclane ; Undecaphosphatrishomocubane ; Ufosane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Partial exchange of the alkali metal ions for tetraalkylammonium cations of Rb3P7 and Cs3P11 in liquid ammonia results in the formation of [(CH3)4N]2RbP7(NH3) (1) and [(C2H5)4N]Cs2P11 (2). The crystal structures reveal the existence of one-dimensional 1∞[RbP7]2- chains in the former and two-dimensional 2∞[Cs2P11]- layers in the latter compound. The nortricyclane cage in 1 is distorted by one-sided coordination to the Rb ions in a manner that can be related to the valence tautomerism of the free P73- anion.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290208
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    Synthesis and Structure of Tris(trialkylstannyl)- and Tris(dialkylhalostannyl)amines; Stabilization of the Sn3N Skeleton by Intramolecular Sn-X-Sn Bridges (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 175-189 
    Details
    ISSN: 0009-2940
    Keywords: Tristannylamines ; Tris(trialkylstannyl)amines ; Tris(dialkylhalostannyl)amines ; Sn-N Bond cleavage ; Sn-X-Sn Intramolecular bridges ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(triorganylstannyl)amines (R2R'Sn)3N (1, 2) with substituents R = R' = Me, Bu or R = Me and R' = iPr, tBu are obtained by metathesis from R2R'SnX and NaNH2 in liquid ammonia or by transamination of R3SnNMe2 with NH3. Tris(diorga-nylhalostannyl)amines (R2XSn)3N (3) are synthesized by stannazane cleavage of (Me3Sn)3N (1) with R2SnX2. Information from multinuclear magnetic resonance spectra ascertain the planarity of the Sn3N skeleton of type 2 and 3, as well as the relationship between the coupling constants 1J(119Sn15N) and 2J(119Sn117Sn) and the Sn-N bond length as determined by the X-ray structure analysis of 1, 3b and 3r. Compound 3b shows an almost undistorted D3h symmetry with a planar Br3Sn3N skeleton and SnN bond lengths of 1.99 Å, which beside those of 3a are the shortest found so far. According to MNDO approximate and ab initio calculations π interactions between the lone electron pair at the N atom and empty orbitals at the Sn atoms can be excluded. Therefore, the tristan-nylamines discussed here have a trigonal planar nitrogen center with its lone electron pair in a p-type orbital. Further characteristic features of the molecular structures of typ 3 compounds are the intramolecular Sn-X-Sn bridges (X = Cl, Br, I) found in the solid state as well as in solution. The molecular geometries of the tristannylamines are supported by MS fragmentation patterns as well as by infrared and Raman spectra.
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    URL: http://dx.doi.org/10.1002/cber.19961290211
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    Synthesis and Structure of Metal-Functionalized Phosphaarsiranes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 219-222 
    Details
    ISSN: 0009-2940
    Keywords: Arsaphosphapropene ; Phosphaarsiranes ; Carbonylchromium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of (η5-C5Me5)(CO)2FeAs(SiMe3)2 (1) with equimolar amounts of (bis(trimethylsilyl)methylene]chlorophosphane afforded the 1-metallo-1-arsa-2-phosphapropene (η5-C5-Me5)(CO)2FeAs(SiMe3)P=C(SiMe3)2 (2) in addition to a few crystals of dimetallophosphaarsirane (η5-C5Me5)(CO)2Fe- AsC(SiMe3)2PFe(CO)2(η5-C5Me5) (3). Treatment of 2 with an excess of [(Z)-cyclooctene]Cr(CO)5 and subsequent chromatography furnished the phosphaarsirane-[Cr(CO)5] adduct (η5-C5Me5)(CO)2Fe-ηAsC(SiMe3)2PH[Cr(CO)5] (5). The molecular structures of 3 and 5 were established by single-crystal X-ray structure analyses.
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    URL: http://dx.doi.org/10.1002/cber.19961290216
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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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    2,5-Dihydro-1,2,5-azoniasilaboratole Derivatives - Useful Starting Materials in Heterocyclic Synthesis (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 147-153 
    Details
    ISSN: 0009-2940
    Keywords: 1,1-Organoboration ; 1-Alkynylsilanes ; 1,2,5-Azoniasilaboratoles, 2,5-dihydro-, organo-substituted ; Heterocyclic synthesis ; Multinuclear NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1-Alkynyl(diethylamino)dimethylsilanes [CC̊: R = Me (1a), nBu (1b), SiMe3 (1c)] react with triethylborane stereoselectively by 1,1-ethyloboration to give the alkenes with the boryl and silyl group in cis-positions at the C=C bond. Owing to the strongly intramolecular coordinative N-B bond, these products are 2,5-dihydro-1,2,5-azoniasilaboratoles (2a-c). Protic reagents such as azoles (indole, pyrazole, imidazole, triazole, indazole, benzotriazole) react with 2 to give diethylamine and the respective N-azolyl derivatives 3-8 which contain tetracoordinate boron in the case of 4-8. Compound 7, derived from indazole, was characterized by an X-ray analysis. With ethanol, the corresponding 2,5-dihydro-1,2,5-oxoniasilaboratoles 9 are obtained. Treatment of 2 with water affords 1,2,5-oxasilaborolanes 11, presumably via an intermediate 10 with the structure of a 2,5-dihydro-1,2,5-oxoniasilaboratole. All products were characterized by their 1H-, 11B-, 13C-, 15N-, and 29Si-NMR data.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290207
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    Preparation, Properties, and Reactions of Metal-Containing Heterocycles, XCIIPart XCI: Ref.. Steric and Solvent Effects of the Different Reaction Patterns of Activated Alkynes with DiphosphamanganacyclopropanesDedicated to Professor Herbert W. Roesky on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 191-199 
    Details
    ISSN: 0009-2940
    Keywords: Bicyclic manganese compounds ; P-P bonds ; Activated alkynes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The product pattern of the reaction of the alkynes ZC≡CZ (4-11) [Z = CO2R: R = Me (4), Et (5), nPr (6), iPr (7), nBu (8), nPent (9), neo-Pent (10), cyc-Hex (11)] with the diphospha-manganacyclopropanes (1-3) depends on the polarity of the employed solvent. Whereas in n-hexane the diphosphamanganabicyclo[3.3.0]octadienones 12a-q, the diphosphamanganacyclopentenes 13a-h, and the triphosphamanganabicyclo[3.2.0]heptenones 14a-h are formed, in THF only the five-membered heterocycles 13 occur. Compound 14d is easily oxidized to the corresponding oxide 15d. According to X-ray structural analyses, both 14d and 15d crystallize in the space group P&1macr;. The Lewis basic properties of the phosphorus atom P2 in the heterocycle 1 were corroborated by reaction of 1 with THFCr(CO)5 leading to the adduct (16). Quantitative 31P{1H}-NMR investigations in CDCl3 enable the determination of the product ratio 13/12 as a function of the steric encumbrance of the ester substituents. An increase of the steric hindrance leads to the preferential formation of the mo-nocyclic compounds 13. If the steric demand at the phosphorus atom P2 is released, only the bicyclic compounds 12i-q are formed.
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    URL: http://dx.doi.org/10.1002/cber.19961290212
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    The Chemistry of Metallacyclic Alkenylcarbene Complexes, 4Part 3: Ref.[36].. Unsaturated Metallacyclic Carbene Complexes as Flexible Tools in Organic Synthesis. Novel Rearrangement and Cascade Pathways to Functionalized Alkadienes, Carbo-, and Heterocycles (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 595-602 
    Details
    ISSN: 0009-2940
    Keywords: Carbene complexes ; Organoiron compounds ; Metallacycles ; Rearrangements ; C — C coupling ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cationic metallacyclic carbene complexes of iron and cobalt bearing a terminal η3-allyl ligand are susceptible to nucleophilic attack at different sites depending on the particular set of substituents, the central metal fragment, and the nucleophile. Attack of enolates, cuprates, acetylides, or heteroatom nucleophiles like phosphanes at the metallacyclic perimeter of the iron complexes 18 provides an easy access to unsaturated organic products like 1,2- or 1,3-dienes, δ-lactones, and functionalized cyclopentenones through novel rearrangement or cascade pathways. Synthetic applications are described; factors governing reactivity/selectivity are discussed; X-ray analytical structures of novel metallacycles are provided.
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    URL: http://dx.doi.org/10.1002/cber.19961290602
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    Reactions of Complex Ligands, LXXPart LXIX: Ref.[1].. An Intramolecular Alkyne Insertion/Carbonylation/Cyclization Sequence of Chromium Aminocarbene Complexes: A Novel Access to Indole and Indenoindole Skeletons (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 623-631 
    Details
    ISSN: 0009-2940
    Keywords: Carbene complexes ; Chromium complexes ; Benzannulation ; Cyclopentannulation ; Benzocarbazoles ; Indenoindoles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 2-Alkynylanilinocarbene chromium complexes 1-7 bearing a rigid arene C2 spacer between the aminocarbene and alkyne units were prepared from pentacarbonyl(aroyl)chromates(-I), acetyl bromide, and 2-alkynylanilines. They undergo intramolecular cyclization the course of which depends on the substitution pattern at the alkyne terminus. A tandem alkyne insertion into the metal-carbene bond/carbonylation sequence affords Cr(CO)3-coordinated 3-indolylketenes 8, 9, 12-14 by using a bulky substituent; the rate of the reaction increases with N-alkylation. Less bulky n-alkynylanilinocarbene complexes 4, 5 exhibit two competing carbene annulation sequences: Benzannulation leads to benzo[a]carbazoles 15, 16, whereas cyclopentannulation without prior carbonylation furnishes indeno[1,2-b]indoles 17, 18.
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    The Reaction of As4Sn (n = 3, 4) and As2S3 with (C5Me4R)2Co2(CO)2 (R = Me, Et): Fragmentation and Reassembling of Main-Group Ligands by Organometallic Complexes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 657-662 
    Details
    ISSN: 0009-2940
    Keywords: Cobalt complexes ; Arsenic sulfides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of Cp2#Co2(CO)2 1 (Cp# = Cp* or Cpx; Cp* = C5Me5: a; Cpx = C5Me4Et: b) with equimolar amounts of As4Sn (n = 3, 4) and As2S3 was investigated at different temperatures. The formation of Cp2#Co2(CO)As2S2 3, Cp2#Co2As2S3 4, Cp3#Co3As2S4 5, and Cp3#Co3As4S2 6 was observed in ratios depending on the reaction conditions. Starting from As4S4 or As4S3 and 1b insertion of a CpxCo(CO) fragment into one of the As-As bonds of the cages was achieved in low yields leading to CpxCo(CO)As4S4 2b and CpxCo(CO)As4S3 8, respectively. Structures were studied by means of IR and 1H-NMR spectroscopy and X-ray diffraction analyses. Cp2#Co2(CO)As2S2 3 may be supposed to be the key intermediate in the whole reaction sequence: On heating solutions of 3 complexes 4-6 of higher nuclearity and different connectivity within the inorganic ligand were formed.
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    URL: http://dx.doi.org/10.1002/cber.19961290611
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    Oligophosphane Ligands, XLIPart XL: A Saare, L. Dahlenburg, Z. Naturforsch. B: Chem. Sci. 1995, 50, 1009-1017.. Oxidative Additions of Transition Metal-Hydrogen Bonds: Reactions of CpM(CO)3H (M = Mo, W) with [tBuP(CH2CH2CH2PPh2)2]M′Cl(M′ = Rh, Ir)Dedicated to Professor Dr. Erwin Weiß on the occasion of his 70th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 677-682 
    Details
    ISSN: 0009-2940
    Keywords: Oligophosphane complexes ; Metal-Hydrogen bonds ; Hydrogen transfer ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of (PP2)IrCl[PP2 = tBuP(CH2CH2CH2PPh2)2] with an equimolar quantity of CpM(CO)3H (M = Mo, W) or with HCl in THF resulted in smooth protonation of the d8 substrate producing [(PP2)Ir(H)Cl]X {X- = [CpMo(CO)3]- (1), [CpW(CO)3]- (2), Cl- (3)}. Combination of (PP2)IrCl and CpM(CO)3H in a 2:1 stoichiometry gave (PP2)Ir(H)Cl2 (7) together with [(PP2)IrCO]-[Mo(CO)3Cp] (8) or [(PP2)IrCO][W(CO)3Cp] (9). The rhodium analogues (PP2)Rh(H)Cl2 (4), [(PP2)RhCO][Mo(CO)3Cp] (5), and [(PP2)RhCO][W(CO)3Cp] (6) were obtained similarly from (PP2)RhCl and CpM(CO)3H. Structural assignments for [(PP2)Ir(H)Cl]+ and (PP2)M′(H)Cl2 (M′ = Rh, Ir) as diastereomers in which the hydrido ligand and the tBu substituent on the central phosphorus atom are located on the same side or on opposite sides of the PP2 reference plane of the meridionally bound tBuP(CH2CH2CH2PPh2)2 ligand are made on the basis of (i) correlations with known structures and reactivities of similar [(RP(CH2CH2CH2PR′2)2M′(H)Cl]+ cations and (ii) an X-ray structure determination of 4. The crystal structure analysis of a [(PP2)RhCO]+ salt, closely related to 5/6 and 8/9, [(PP2)Rh(CO)][OCO2H] (10), demonstrates that in the solid state the four-coordinate [(PP2)RhCO]+ cation and its counterion exist as essentially charge-neutralized Rh⃛O-contacted ion pairs, two of which are linked by O—H⃛O bridges to centrosymmetric dimers. Ion pairing was also observed by IR spectroscopy for THF solutions of metalates 5/6 and 8/9.
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    Ir-Komplexe mit P4-Bicyclotetraphosphan und P8-Cunean als Liganden - CO-Insertion in eine Ir-P-BindungHerrn Professor Kurt Dehnicke zum 65. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 721-724 
    Details
    ISSN: 0009-2940
    Keywords: Px Ligands ; P8 Cunean ; P4 Bicyclotetraphosphane ; Iridium complexes ; CO Insertion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ir Complexes with P4 Bicyclotetraphosphane and P8 Cunean as Ligands - CO Insertion into an Ir-P BondThe reaction of [Cp*Ir(CO)2] with white phosphorus under photochemical or thermal conditions produces the bicyclotetraphosphane complexes 1 and 2 and the cunean-type complex 3. The products were characterized by NMR, IR, and mass spectroscopy as well as by X-ray structure analyses. Complex 1 reacts with CO with insertion into a Ir-P bond to form 2 and finally [Cp*Ir(CO)2].
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    Electrochemical Preparation of Nanostructured Titanium Clusters: Characterization and Use in McMurry-Type Coupling Reactions (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 741-743 
    Details
    ISSN: 0009-2940
    Keywords: Clusters ; Transmission electron microscopy ; Low-valent titanium ; Olefin formation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electrochemical preparation of nanostructured titanium clusters is possible by using a titanium sacrificial anode as the metal source and tetrabutylammonium bromide in THF as the electrolyte and stabilizer. Transmission electron microscopy shows the presence of spherical 3.0-nm-sized particles. THF solutions of these Ti clusters induce olefin-forming McMurry-type coupling of aldehydes and ketones.
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    Ionic Ozonides of Lithium and Sodium: Circumventive Synthesis by Cation Exchange in Liquid Ammonia and Complexation by CryptandsDedicated to Professor H. G. von Schnering on the occasion of his 65th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 773-777 
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    ISSN: 0009-2940
    Keywords: Ozonides ; Sodium ozonide ; Lithium ozonide ; Cation exchange ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Concentrated solutions of the ozonides LiO3 and NaO3 in anhydrous liquid ammonia were obtained for the first time by using an ion exchange reaction that starts from CsO3. No solid LiO3 or NaO3 can be precipitated. Upon removal of the solvent, the ozonide anion oxidises ammonia, resulting in the precipitation of LiOH and NaOH, respectively. This behaviour is in sharp contrast to that of solutions of KO3, RbO3 and CsO3. Proof of the existence of LiO3 and NaO3 in the solutions is provided by complexation of the cations with cryptands, which leads to solid (Li[2.1.1])O3 and (Na[2.2.2])O3. Crystal structure analysis shows that these are ionic solids containing the V-shaped O3- anion.
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    URL: http://dx.doi.org/10.1002/cber.19961290707
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    The First SiH22+ Complex, Dihydridotetrakis(3-picoline)silicon Dichloride-Tetrakis(chloroform), [H2Si(3pic)4]Cl2 · 4 CHCl3: Formation, Chemical Equilibria, and Structural Investigation by NMR Spectroscopy and Single-Crystal X-ray Diffraction (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 765-771 
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    ISSN: 0009-2940
    Keywords: Bis(dichlorosilyl)amine ; Dihydridotetrakis(3-picoline)silicon dichloride-tetrakis(chloroform) ; Dative Si-N interaction ; 1H1H ROESY ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bis(dichlorosilyl)amine reacts in chloroform solution with 2-picoline to give H3SiCl, H2SiCl2, and HSiCl3, whereas with 3-picoline the two hypervalent silicon compounds H2SiCl2-(3pic)2 and [H2Si(3pic)4]Cl2 · 4 CHCl3 containing hexacoordinated Si atoms are formed. These complexes are in a chemical equilibrium with each other in chloroform solution, from which crystals of [H2Si(3pic)4]Cl2 · 4 CHCl3 could be isolated. The crystal structure of the latter was determined by single-crystal X-ray diffraction. The complex can be regarded as an “contact ion trio” of [H2Si(3pic)4]2+ and two Cl- ions. The N-Si bond lengths, r(Si-N) = 196.9(3) and 197.5(3) pm, are similar to those found in neutral hexacoordinated Si complexes. The data obtained from a 1H1H ROESY experiment suggest that dissolution has no significant impact on the molecular structure of [H2Si(3pic)4]Cl2 · 4 CHCl3.
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    Synthesis and X-ray Crystal Structure of the First Mononuclear Nickel(II) Alkane Thiolate Complex with a Mixed (S,N,N,O) Ligand FieldDedicated to Professor Rolf Gleiter on the occasion of his 60th birthday (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1183-1189 
    Details
    ISSN: 0009-2940
    Keywords: Nickel complexes ; Thiolates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The six-step synthesis of a chiral, pentadentate dihydrosalen ligand, carrying a mercaptomethyl group as additional binding site, is described. When this ligand was treated with nickel(II) salts, a planar tetracoordinated nickel chelate was obtained, and not the expected pentacoordinated species. This complex was fully characterized, including X-ray crystallography. The crystal structure revealed that the nickel ion is coordinated by the thiolate anion, both the amine and the imine nitrogen atoms of the ligand, and by one phenolate anion. The second phenolic oxygen atom of the ligand does not participate in the coordination of the nickel ion. This chelate is the first mononuclear nickel(II) thiolate complex having a mixed (S,N,N,O) ligand field. Cyclic voltammetry did not indicate a reduction up to -2.1 V (vs. Fc/Fc+). In the anodic range, no reversible but two irreversible oxidation processes were observed.
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    Crystal Structures and Preparation of K2AgVS4 and Rb2AgVS4 by Using the Molten Flux Method: Low-Dimensional Materials with Infinite Metal-Ion-Centered Tetrahedra Chains (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1207-1210 
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    ISSN: 0009-2940
    Keywords: Low-temperature synthesis ; Reactive flux method ; Quaternary vanadium sulfide ; Low-dimensional materials ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The quaternary sulfides K2AgVS4 and Rb2AgVS4 crystallize as dark violet needle-like crystals with a metallic lustre. Infinite Ag- and V-centered tetrahedra sharing common edges are running parallel to the crystallographic a axis. The chains are separated by K+ or Rb+ ions which are in an eightfold environment. The tetrahedra are occupied in an ordered fashion. The Ag-V interatomic distances amount to 2.904(1) and 2.910(1) A, respectively, which is significantly larger than the sum of the ionic radii of Ag+ and V5+. Whereas the V-S distances are in the normal range, the average (Ag-S) distances are the shortest reported so far indicating strong covalent bonding between monovalent Ag+ and S2-. In addition, the title compounds represent very rare examples of AgS4 polyhedra with equidistant Ag-S bonds. The geometrical parameters within the tetrahedra chains are only slightly affected when K+ is replaced by the larger Rb+ demonstrating the rigidity of the bonding properties within the tetrahedra. The compounds are isotypic with the quaternary copper sulfide K2CuVS4 and the selenides K2CuMSe4 (M=Nb, Ta).
    Additional Material: 4 Tab.
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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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    The Chemistry of 1,3,5-Triazacyclohexane Complexes, 4Part 3: Ref.[1].. Strained 1,3,5-Triazacyclohexane Complexes of Copper(I) and Copper(II) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1327-1333 
    Details
    ISSN: 0009-2940
    Keywords: Triazacyclohexanes ; Copper complexes ; Triphenylphosphane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In this paper we report on the synthesis and the crystallographic characterization of η3-1,3,5-triazacyclohexane (R3TAC) complexes of copper(I) and copper(II). The complexes [{Me3TAC)CuCl2}2] (1), [(iPr3TAC)CuCl2] (2), [{(PhCH2)3TAC}Cu(PPh3)](BF4) (3), and [(iPr3TAC)Cu(PPh3)]-(BF4) (4) were characterized by X-ray crystallography. The highly strained and bent Cu-N bonds are longer than in the corresponding complexes of other amine ligands. One methylene carbon atom of the ring comes close to the copper atom (2.55-2.65 Å). However, investigation of the ring deuterated complexes by IR and X-ray crystallography ([D6]2) showed no clear evidence for attractive C-H-Cu interactions.
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    Novel Inorganic (Carbon-Free) Chelate Rings: Tris(chelate) Compounds of [N-(Diphenylphosphinoselenoyl)-P,P-diphenylphosphinoselenoic amidato-Se, Se′] with MIII (M = Sb, Bi, In) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 919-923 
    Details
    ISSN: 0009-2940
    Keywords: Phosphazene metallacycles ; [N-(Diphenylphosphinoselenoyl)-P,P-diphenylphosphinoselenoic amidato-Se,Se′] chelates ; Inorganic carbon-free chelate rings ; Octahedral MSe6 core (M = Sb, Bi, and In) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The [(SePPh2)2N]- ligand 1c forms stable tris(chelates) with the SbIII, BiIII, and InIII ions. The crystal and molecular structures of the resulting compounds 3, 4, and 5 were determined by X-ray diffractometry. The coordination geometry around the metal centers can be described as a distorted octahedron. This feature and the results obtained by comparing the structures with their sulfur and oxygen analogs lead us to conclude that in both SbIII and BiIII compounds the arrangement around the metals suggests a stereochemically nonactive electron lone pair.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290807
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    Preparation, Properties, and Reactions of Metal-Containing Heterocycles, XCVPart XCIV: Ref.[1].. Transition-Metal-Mediated Cyclocotrimerization of Selenophosphinites with Activated AlkynesDedicated to Professor Rudolf Taube on the occasion of his 65th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 945-951 
    Details
    ISSN: 0009-2940
    Keywords: Cyclocotrimerization ; Selenophosphinites ; Alkynes, activated ; Selenophenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Selenophosphinito complexes (OC)4Mn(η2-Se\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}PR21) (2a, b) [R1 = cyc-Hex (a), tBu (b)] are formed by the reaction of BrMn(CO)5 with the phosphane selenides R21HPSe (1a, b) in the presence of the auxiliary base Et(iPr)2N. According to an X-ray structural analysis, 2a crystallizes in the space group \documentclass{article}\pagestyle{empty}\begin{document}$ P\bar 1 $\end{document} with Z = 2. The dimeric complex [(OC)4Mn(μ-Se\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}PMe2)]2 (4c) is not obtained in a straightforward way. Compound 4c is only obtained via the intermediate Br(OC)4Mn-Se\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}P(H)Me2 (3c) by HBr elimination with nBuLi. Complex 3c is formed by replacement of carbon monoxide in BrMn(CO)5 by Me2HPSe (1c). A dissociative equilibrium between [(OC)4 Mn(μ-Se\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}PMe2)]2 (4c) and the monomeric species (OC)4Mn(\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}2-Se\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}PMe2) was not observed. The cyclocotrimerization of the 〉P\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ \dddot - $\end{document}Se function with the activated alkynes ZC≡CZ [Z = CO2R2; R2 = Me (d), Et (e), iPr (f), cyc-Hex (g)] was successful only in the case of the cyclohexyl derivative 2a to give the selenaphosphamanganabicycloheptadienes 5d - g. An X-ray structural analysis proved that 5d crystallizes in the space group \documentclass{article}\pagestyle{empty}\begin{document}$ P\bar 1 $\end{document} with Z = 2. Under CO pressure 5d was degraded to the selenophene 6.
    Additional Material: 2 Ill.
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    Copper Coordination Polymers with Infinite Chloride Ion Channels and Different Directions of the Jahn-Teller Distortion, Built from Tris(1,2,4-triazolyl)borate as a Modified Tris(pyrazolyl)borate LigandDedicated to Prof. Dr. Jörn Müller on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 991-995 
    Details
    ISSN: 0009-2940
    Keywords: Coordination polymers ; Ion channels ; Copper compounds ; Bond-stretch isomerism ; Hydrated chlorine ions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [Co{HB(C2H2N3)3}2] reacts with an excess of CuCl2 in hot water with formation of ∞2[Cu2Cl2{μ3-HB(C2H2N3)3}2 · 2 H2O] (7) or ∞3{[Cu2{μ4-HB(C2H2N3)3} (μ-OH)2]Cl · 6 H2O} (8), depending on the reaction time. 8 can also be obtained from [Cu{HB(C2H2N3)3}2] and CuCl2 in aqueous ammonia. The 2-D double-layer-type coordination polymer 7 crystallizes in the orthorhombic space group P212121. The two different Cu(II) centers in the lattice are distinguished only be the direction of the Jahn-Teller distortion. The following corresponding distances for the CuClN5 coordination sphere were found Cu1/Cu2-Cl = 2.572(2)/2.328(2), Cu1/Cu2-N = 2.585(5)/2.077(4); 2.000(4)/1.979(5); 2.100(5)/2.734(5); 2.005(4)/1.994(4); 2.024(5)/2.369(5). In the 3-D coordination polymer 8 one of the two different Cu centers is chelated by the three endodentate nitrogen donors, while the other Cu center is coordinated by three exodentate nitrogen atoms. The coordination sphere is completed in both cases by two hydroxo bridges to symmetry-related Cu centers. The metal-ligand connectivity creates infinite channels with helical walls which contain the solvated chloride anions.
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    Synthesis, Structure and Vibrational Spectra of Ba14InP11 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1015-1023 
    Details
    ISSN: 0009-2940
    Keywords: Ba14InP11 ; Zintl phase ; Tetraphosphidoindate(III) anions ; Asymmetric [P3]7- polyanions ; Interpenetrating hierarchical frameworks ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ba14InP11 was prepared from the elements in a sealed stainless steel ampoule at 1345 K. The compound is black, brittle and very sensitive to air and moisture. Ba14InP11 crystallises in the tetragonal Ca14AlSb11 type (space group I41/acd, No. 142; a = 17.097 (2) Å, c, = 8, Pearson code tI208). The structure contains isolated P3-, linear [P3]7- and tetrahedral [InP4]9- anions. The X-ray structure analysis and the vibrational spectra show that the [P3]7- polyanion is strongly asymmetric with d(P-P) = 2.28 Å and 4.10 Å, corresponding to a [P2]4- dumbbell weakly coupled to a single p3- anion. The tetraphosphidoindate(III) anion [InP4]9- is slightly compressed along the 4 axis, with bond lenght d(In-P) = 2.71 Å. It is shown that the structure is hierarchically related to that of Cu2O, with two interpenetrating frameworks, in which the O and Cu atoms are replaced by condensed [InP4/2] tetrahedron and [BaP4P2/2] octahedra, respectively. Both frameworks are meso configured, containing alternate R and S fragments. The other Ba cations envelop the P6 octahedra and P3 triads forming condensed cubes, tetragonal antiprisms and bicapped trigonal prisms. Therefore, the structure also forms a heterogeneous framework of centred PBa8/2tap tetragonal antiprisms and BaBa8/2cub cubes, consisting of two interpenetrating enantiomorphic nets (R and S) similar to those in the cubic phase RhBi4.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290907
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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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    Metal Complexes with Tetrapyrrole Ligands, LXXII Cerium(IV) Sandwich Complexes with Porphyrin Ligands Linked by Aliphatic and Quinone-Containing Bridges (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1073-1081 
    Details
    ISSN: 0009-2940
    Keywords: Cerium(IV) bisporphyrinates ; Sandwich complexes ; Diporphyrins ; Porphyrin quinone systems ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Starting from 5-(4-hydroxyphenyl)-10,15,20-tris(4-methylphenyl)porphyrin (1a), the new bis(porphyrinylphenoxy)alkanes 4a-c were synthesized by ether formation with the α,ω-dibromoalkanes Br(CH2)nBr (n = 9,10; 3a, b) and 1,4-bis(3-bromopropyl)-2,5-dimethoxybenzene (3c). The bis-[(porphyrinylphenoxy)propyl]hydroquinone dimethyl ether 4c derived from 3c was converted into the diporphyrin-quinone 4e by methyl ether cleavage with BBr3 and subsequent oxidation with ammonium cerium(IV) nitrate. The bisporphyrins 4a-c, e were metalated with cerium(III) acetylacetonate to yield the new cerium porphyrin sandwich complexes 5a-c, e which carry the alkane links in vicinal positions at the porphyrin rings. 5a-c, e were characterized by UV/Vis, IR, 1H-NMR spectroscopy and cyclic voltammetry. The quinone-bridged cerium sandwich complex 5e contains the quinone moiety in a distinct non-coplanar orientation relative to the porphyrin ligands of the double-decker system. The length of the lateral chains may have a dramatic effect on the first and second oxidation potentials, E3 and E2, of the porphyrin rings: for 5b having 10 aliphatic C atoms in the chain, E3 and E2 are higher by 0.26 and 0.24 V, respectively, as compared with 5a having only 9 aliphatic C atoms. E3 and E2 for the latter are rather close to values for species with dipropylbenzene chains (i.e. in 5c and 5e) or without lateral bridges.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290915
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    Azidopentazole is Probably the Lowest-Energy N8 Species - A Theoretical Study (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1157-1159 
    Details
    ISSN: 0009-2940
    Keywords: N8 Isomers ; Azidopentazole ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ab initio molecular orbital calculations at the quadratic configuration interaction [QCISD(T)/6-31G(d)] and coupled-cluster theory [CCSD(T)/DZP] levels based on MP2/6-31G(d) optimized geometries show that azidopentazole is likely to be the global minimum of the N8 isomers lying 13 and 18 kcal/mol below the acyclic diazidyldiimide and the cyclic pentalene analogue, respectively. Azidopentazole is characterized by a significant energy barrier to ring closure and is expected to be stable with respect to cycloreversion and thus constitutes the most realistic N8 target for a synthetic preparation.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19961291003
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    Activation of Bis(trimethylsilyl) Peroxide and tert-Butyl Hydroperoxide with Oxo and Peroxo Complexes of Vanadium, Molybdenum, and Tungsten for the Sulfoxidation of Thianthrene 5-Oxide (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1177-1182 
    Details
    ISSN: 0009-2940
    Keywords: Thianthrene 5-oxide ; Peroxide, bis(trimethylsilyl) ; Hydroperoxide, tert-butyl ; Oxygen transfer ; Peroxo complexes ; Catalysis ; Vanadium ; Molybdenum ; Tungsten ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bis(trimethylsilyl) peroxide (BTSP) and tert-butyl hydroperoxide (tBuOOH) were activated by various oxo and peroxo complexes of molybdenum, tungsten, and vanadium as catalysts for the sulfoxidation of thianthrene 5-oxide (SSO). A screening of a number of phosphane oxide and amine oxide ligands revealed that BTSP was most efficiently activated by the [MoO5(OPtBu3)] complex. The best results for tBuOOH as oxygen source were achieved with the vanadates [VO(OR)3] (R = tBu, iPr). Comparative selectivity and rate data for the stoichiometric and catalytic sulfoxidations of SSO mediated by the MoO5L complex (L = OPtBu3, OPnOct3, ONnBu3, ONnOct3) suggest that the bisperoxo metal complex is the active oxygen transfer species.
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    URL: http://dx.doi.org/10.1002/cber.19961291006
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    Fluxionality and Phosphane Arm-off Reactions of Octahedral Rhodium(III) Complexes with the Tripodal Polyphosphane MeC(CH2PPh2)3 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1199-1206 
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    ISSN: 0009-2940
    Keywords: Rhodium(III) complexes ; Triphos complexes ; Arm-off dissociation ; Fluxional behaviour ; Dialkyldithiocarbamate complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of [RhCl3(triphos)] or [Rh(MeCN)3(triphos)](CF3SO3)3 [triphos= MeC(CH2PPh2)3] with Na(S2C-NEt2) affords the complexes [RhCl(S2CNEt2)(triphos)]Cl (1) and [Rh(S2CNEt2)(MeCN)(triphos)](CF3SO3)2 (2). Whereas 1 is stereochemically rigid in solution at 25°C, 2 and the analogous complex [Rh(S2CNBz2)(MeCN)(triphos)](CF3SO3)2 (3) exhibit a rapid exchange of their phosphorus environments. In contrast, the 31P-NMR spectra of both 2 and 3 at -30°C consist of well-resolved A2MX spin systems. k2P-coordinated complexes of the type [Rh(S2CNR2)2(triphos-k2P)]+ (R = Et 4, R = Me 5) with ABX spin systems may be obtained by treatment of the starting compounds with two equivalents of the respective dialkyl dithiocarbamate. The dangling phosphane arm can be readily oxidised to a phosphane oxide as in [Rh(S2CNEt2)2(triphosO-k2P)]Cl (6) [triphosO = O=P(Ph)2CH2C(Me)(CH2PPh2)2]. The analogous compound [Rh(mpy)2(triphosO-k2P)]Cl (7) (Hmpy = 2-mercaptopyridine) was isolated as the OC-6-13 isomer with trans-positioned sulphur atoms, a siting which is in accordance with a reaction mechanism involving a phosphane arm-off k3P' k3P dissociation equilibrium.
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    Electrophilic Substitution at the NB9 and NB11 closo-SkeletonsDedicated to Professor Kurt Dehnicke on the occasion of his 65th birthday (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1227-1231 
    Details
    ISSN: 0009-2940
    Keywords: Aza-closo-decaboranes, halogenation of, methylation of ; Aza-closo-dodecaboranes, halogenation of, methylation of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The aza-closo-boranes ArNB9H9 (1, Ar = p-ClC6H4) and MeNB11H11 (2) were brominated, iodinated, or methylated under Friedel-Crafts conditions to give ArNB9H4Br5 (3), ArNB9H7I2 (4), ArNB9H4Me5 (7), MeNB11H10Br (5), MeNB11H10I (6), and MeNB11H5Me6 (9), respectively. The upper boron belt adjacent to nitrogen is not involved in the substitution reactions with 1 and 2. The antipodal position and the lower belt are attacked by electrophiles in the case of 1; the antipodal position is the preferred one in the case of 2. By prolongated action of triflic acid on the methylated species 7 and 9, one methyl group is replaced by the triflate group to give ArNB9H4Me4(OTrf) (8) and MeNB11H5Me5-(OTrf) (10) with this group in the positions 6 and 12, respectively. The NMR data indicate the cluster symmetries Cs (4, 8), C4v (3, 7), and C5v (5, 6, 9, 10). Crystal structure investigations of 5 (space group Cc) and 10 (space group C2/c) showed that the molecular dimensions of the NB11 skeleton are comparable to those of closo, -(PhCH2)NB11H11.
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    A Palladium-Catalyzed Domino Coupling Process Leading to Annelated PentafulvenesDedicated to Professor Dr. Peter Sartori on the occasion of his 65th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1265-1269 
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    ISSN: 0009-2940
    Keywords: Domino coupling reactions ; Pentafulvenes ; Catalysis ; Palladacycles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Annelated pentafulvenes 2, 10, 13, and 14 are efficiently accessible by a palladium-catalyzed domino coupling process of aryl substituted vinylic bromides 1, 9, 11, and 12, 5-Membered palladacycles 3 are discussed as key intermediates.
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    URL: http://dx.doi.org/10.1002/cber.19961291019
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    Zinc Complexes of Amino Acids and Peptides, 8[Part 7: Ref.[1].]. Difunctional Dipeptides Containing Cysteine or Histidine: Solution Behavior and Zinc Complextion (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1243-1249 
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    ISSN: 0009-2940
    Keywords: Dipeptides ; Cysteine ; Histidine ; Zinc complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The dipeptides Ac-Cys-Val-OH (1a) and Ac-His-Val-OH (1b), H-Gly-Cys-OEt (2a) and H-Val-His-OEt (2b) as well as Z-Asp-Cys-OH (3a) and Z-Asp-His-OH (3b) (Z = benzyloxycarbonyl) were prepared, and their zinc complexation was investigated by potentiometric methods. They have in common that in addition to the cysteine thiolate or the histidine imidazole the second amino acid offers one donor function. The complex stabilities are very close to those of the corresponding difunctional derivatives of the single amino acids cysteine or histidine. This indicates the presence of seven- to ten-membered chelate rings.
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    URL: http://dx.doi.org/10.1002/cber.19961291016
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    Palladium-Catalyzed Reactions in Industry, 4[Part 3: Ref.[1].]. Synthesis of New Palladium Catalysts: First Isolation and Characterization of all Intermediates in a Cyclopalladation Reaction (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1259-1264 
    Details
    ISSN: 0009-2940
    Keywords: Palladium ; Phosphanes ; Catalysis ; Cyclopalladation reaction ; Metallacycles ; CH activation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In order to synthesize chiral palladacycles for stereoselective C-C coupling reactions we studied the cyclopalladation of P-chiral phosphanes 2 and 3. New palladium complexes of the type L2PdX2 (6, 8) and LXPd-μ-X2-PdXL (5, 9, X = Cl; L = 2, 3) were isolated. A detailed study of the reactivity of all intermediates towards cyclopalladation proved the mechanism of cyclometalation reactions of o-tolylphosphanes for the first time. Different deuteration experiments clearly demonstrated the higher reactivity of dimeric palladium complexes towards metalation compared to monomeric species. In agreement with this observation only 5 and 9 gave the cyclopalladated products 4 and 10 as revealed by FAB mass spectrometric investigations. Under the described reaction conditions the synthesis of the corresponding palladacycles 4, 10 is not possible because cyclometalation is a reversible process with LXPd-μ-X2-PdXL as thermodynamic more stable products. The results demonstrate the importance of free coordination sites on the metal atom for cyclometalation reactions or more general CH activation processes.
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    URL: http://dx.doi.org/10.1002/cber.19961291018
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    Controlled Hydrolysis of Tripodal Titanium Amido Halides: The Influence of the Ligand Periphery upon the Basicity of the Amido-N FunctionsDedicated to Professor Dr. Markus Wieber on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1287-1291 
    Details
    ISSN: 0009-2940
    Keywords: Titanium amido complexes ; Tripodal ligands ; μ-Oxo complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Hydrolysis of the tripodal amidotitanium halides H3CC(CH2NSiMe3)3TiX (X = Cl: 1a; Br: 1b) in the presence of Et3N affords the linear μ-oxo-bridged complex [H3CC(CH2NSiMe3)3Ti]2 (μ-O) (3) which was characterized by X-ray crystallography. Treatment of H3CC(CH2NiPr)3TiX (X = Cl: 2a; Br: 2b), obtained in low yields, under the same conditions only leads to decomplexation of the amido ligand. Under conditions of very slow exposure to H2O the primary addition product of water across two Ti-N bonds in 2a could be isolated and was characterized as [H3CC(CH2-i(μ-Cl)]2(μ-O) (4), the crystal structure analysis establishing a triply bridging central Ti(μ-O)(μ-Cl)2 Ti unit. Deprotonation with two molar equivalents of nBuLi and subsequent LiCl elimination afforded the μ-oxo complex [H3CC(CH2NiPr)3Ti]2(μ-O) (5).
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19961291023
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    Zur Transformation des P4-Tetraeders durch Ni-KomplexeFrau Professor Marianne Baudler zum 75. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1307-1310 
    Details
    ISSN: 0009-2940
    Keywords: Px ligands ; Nickel complexes ; Bent cyclo-P4 complex ; Ni2P4 distorted prismane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Transformation Pathway of the P4 Tetrahedron by Ni Complexes
    Notes: The thermal reaction of [Cp*NiCO]2 with white phosphorus in the presence of [Cr(CO)5(thf)] at 70°C produces the bent cyclo-P4 ligand complex 4 and the Ni2P4 prismane 5. However under photochemical conditions additional products such as cyclo-P3 complexes 6 and the Ni2P2 tetrahedrane 7 are also formed. 4 and 5 were characterized by NMR, IR, and mass spectroscopy as well as by X-ray structure analysis. The structures of these products and the experimentals verification of the conversion of 4 into 5 or into 6 and 7 as well as the cubane analog 12 gives evidence for a transformation pathway starting from P4 tetrahedron via a possible bicyclotetraphosphane intermediate to give the bent P4 complex 4. From 4 several pathways are possible; the main route is to form the Ni2P4 prismane 5. Photochemically a P3/P1 fragmentation also occurs, albeit in low yield, to give 5 and 6.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291026
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    Structural Chemistry of Alkali Metal PhenylhyrazidesDedicated to Professor Rudolph Gompper on the occasion of his 70th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1335-1344 
    Details
    ISSN: 0009-2940
    Keywords: Lithium hydrazide, N-phenyl-N,N′-bis(trimethylsilyl)- ; Lithium hydrazide, N,N′-diphenyl-N′-(trimethylsilyl)- ; Sodium hydrazide, N,N′-diphenyl-N-(trimethylsilyl)- ; Caesium hydrazide, N-phenyl-N′,N′-bis(trimethylsilyl)- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The crystal and molecular structures of a series of N-phenyl-substituted lithium hydrazides were determined in order to investigate possible Li···Ph π interactions. These are pronounced when there are no donor molecules present to solvate the Li centers. An η6-Li···Ph interaction is particularly distinct in tetrameric (Me3Si)2N-N(Ph)Li but also in trimeric Ph2N-N(SiMe3)Li Deprotonation of N,N′ -diphenylhydrazine with butyllithium in ether resulted in the formation of Ph(Li)N-N(Ph)Li · 2 LiNPh2 · 2 OEt2 with phenyl group migration and N-N bond cleavage by a redox process. An increase of the size of the cations, as shown for Ph(Me3-Si)N-N(Ph)Na · NH3 and the caesium salt (Me3-Si)2N-N(Ph)Cs · nTHF, results in increased coordination of the metal ion to the phenyl group. The caesium compound forms a three-dimensional network. Channels along the c axis are partially filled with THF molecules.
    Additional Material: 11 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291105
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    Direct Synthesis of Organometallics, IVPart III: Ref.[1].. The Mechanism of the Activation of Aromatic Hydrocarbons with Lithium Atoms: Spectroscopic Results and Their Ab initio Interpretation (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1369-1371 
    Details
    ISSN: 0009-2940
    Keywords: C—H bond activation ; Lithium atoms ; Mechanism ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In the presence of THF, lithium atoms are known to be able to activate benzene derivatives under cryogenic reaction conditions. This synthesis affords solid lithium hydride and ring-metalated products selectively. For the determination of the reaction mechanism, the cocondensation reaction was repeated on a reduced scale in a 77-K cryostate, which allowed the measurement of UV/Vis and IR spectra. The spectroscopic results exclude any generation of free electrons; their interpretation suggests that small solvated lithium clusters activate the hydrocarbon bonds. A model reaction was developed by using the spectroscopic results and ab initio calculations. Thus, benzene was added to a Li2 cluster, which reduces the carbon-hydrogen bond to the phenyl anion and hydride on the surface without the formation of free radicals. In the last step the intermediate mixed organolithium species dismutate to solid lithium hydride and phenyllithium.The reduction process on the cluster surface is facilitated by coordinating THF to the lithium, which results in a higher redox potential. The complete mechanism is discussed in the terms of geometries of the intermediates and reaction enthalpies in connection with the experimental values. Thus, a distinct new reaction pathway for a substitution on the benzene ring is established.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291109
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    (Allyl)zirconium(IV) Complexes with the N,N′ -bis(trimethylsilyl)benzamidinato (“siam”) Ligand  -  Molecular Structures and η1-η3 Interconversions of the Allyl GroupsDedicated to Professor R. Gleiter on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1389-1393 
    Details
    ISSN: 0009-2940
    Keywords: Benzamidinate ; Zirconium complexes ; Allyl ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Complexes of the type (siam)2Zr(allyl)2 (1a) and (siam)Zr(allyl)nClm are described (2a: n = 1, m = 2; 2b: n = 2, m = 1; 2c: n = 3, m = 0; siam: N,N′ -bis(trimethylsilyl)benzamidinato group). The molecular structure of 1a shows that both allyl groups are differently bonded. One allyl ligand is η3-, the other η1-coordinated. The X-ray crystal structure of the tris-(allyl) complex 2c shows a chiral molecule with two η3-allyl ligands. The third allyl ligand is coordinated in a mode intermediate between η3 and η1, thus serving as a model for an intermediate in the η3-η1 intramolecular rearrangement of the allyl ligands observed in solution. Temperature-dependent 1H- and 13C-NMR spectra of 1a, 2b and 2c indicate a rapid η1-η3 rearrangement of the allyl groups at 60°C. At -50°C two different coordination modes of the allyl groups can be observed in the case of 2b and 2c.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291113
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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.19961291201
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    The Mechanism of the Double Bond Cleavage in the Titanium Zeolite-catalyzed Oxidation of α-Methylstyrene by Hydrogen Peroxide: the β-Hydroperoxy Alcohol as Intermediate (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1453-1455 
    Details
    ISSN: 0009-2940
    Keywords: Zeolites ; Titanium ; Epoxidation ; Double bond cleavage ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It is unequivocally shown that acetophenone, an oxidation product in the titanium zeolite-catalyzed oxidation of α-methylstyrene, derives from 2-hydroperoxy-2-phenyl-1-propanol as intermediate, which was detected and isolated in this reaction for the first time.
    Additional Material: 2 Tab.
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    Tripodliganden mit Neopentangrundgerüst und zwei verschiedenen Donorfunktionen CH3C(CH2PPh2)2(CH2SR): Synthese, Struktur, Redoxchemie und Spektroskopie von Komplexen des Typs tripodM{ortho-(X)(Y)C6H4}Prof. Dr. Jörn Müller zum 60. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1587-1601 
    Details
    ISSN: 0009-2940
    Keywords: Tripod ligands ; Donor groups, mixed (P, S) ; Cobalt sulfur compounds ; Iron sulfur compounds ; Five-coordination of cobalt and iron ; Redox chemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tripod Ligands with Neopentane Frame and two Different Donor Groups CH3C(CH2PPh2)2(CH2SR): Synthesis, Structure, Redox Chemistry, and Spectroscopy of the Complexes tripodM{ortho-(X)(Y)C6H4}Prof. Dr. Jörn Müller zum 60. Geburtstag gewidmet.Neopentane-based tripod ligands CH3C(CH2PPh2)2(CH2Z) (Z = SBn, SH, S-) form pentacoordinate compounds [tripodM{ortho(X)(Y)C6H4}]m 1-4 with ortho-phenylene-bridged coligands (X)(Y)C6H4 (X, Y = O-, S-, NH-) and Co(II), Co(III), Fe(II), or Fe(III) as the metal centers. The structures of these complexes are very similar to those observed for CH3C(CH2PPh2)3 as the tripod ligand. The redox potentials, however, for the corresponding one-electron oxidation and reduction processes are highly affected by the change in the tripod donor groups. Both potentials are shifted by a maximum of 700 mV upon replacement of a PPh2 donor group by a sulfur-centered donor with the difference between the potential of the oxidation step and the potential of the reduction step staying almost constant for the whole series of compounds. This difference of around 1.7 eV nicely corresponds to the energy of the HOMO-LUMO chargetransfer bands observed around 2 eV for all of the compounds. It may be inferred therefore that both observations (electron spectroscopy and cyclic voltammetry) refer in a similar way to the HOMO-LUMO gap of the compounds. It is shown that the formation of [tripodCo(III){ortho-(NH)2C6H4}]+(BF4-) from ortho-phenylenediamine as the source of the coligand involves precoordination of the amine ligand followed by deprotonation of the coordinated ligand. The capability of the tripodCo(II) template to form five-coordinate compounds with diamines is further corroborated by the characterization of [tripodCo(en)]2+ (52+). In addition to the standard analytical data, EPR, UV/Vis, cyclovoltammetric data and X-ray structure analyses are presented where appropriate.
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    URL: http://dx.doi.org/10.1002/cber.19961291229
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    [4 + 1] Cycloadditions of the Rhodium Di(methoxycarbonyl) Carbenoid to 2-Siloxy-1,3-dienes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 73-75 
    Details
    ISSN: 0009-2940
    Keywords: 2-Siloxy-1,3-dienes ; Dimethyl diazomalonate ; Rhodium(II) acetate ; [4 + 1] Cycloadditions ; Cyclopentene derivatives ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The rhodium(II) acetate catalyzed reaction of dimethyl diazomalonate with 2-siloxy-1,3-dienes 1a-1d and 1h furnished cyclopentene derivatives 4a-4d and 4h in moderate yields. The mechanism of this unusual [4 + 1] cycloaddition is discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290115
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    Activation of Carbon Dioxide, VIPart V: Ref.. Ligand Effects in the Catalytic Hydrogenation of Carbon Dioxide to Formic Acid Using in situ Catalysts Formed from [{(cod)Rh(μ-Cl)}2] and Monodentate and Bidentate Phosphorus Ligands (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 91-96 
    Details
    ISSN: 0009-2940
    Keywords: Carbon dioxide, catalytic hydrogenation of ; Ligand effects ; Rhodium catalysts ; Formic acid ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Highly active catalysts for the hydrogenation of CO2 to formic acid in DMSO/NEt3 are formed in situ from [{(cod)Rh(μ-Cl)}2] and various monodentate or bidentate ligands with phosphorus as the donor atom. Formic acid concentrations up to 2.3 · 0.2 mol l-1 can be obtained in less than 6 hours at ambient temperature under a total initial pressure of 40 atm by using rhodium concentrations of 5 · 10-3 mol l-1. The changes in catalytic activities observed upon structural changes of monodentate ligands are discussed in terms of classical ligand parameters like basicity and steric demand of the PR3 group, while with bidentate ligands R2P(CH2)nPR2 the chain length n plays a dominant role for the activity of the catalyst. The effects cannot be explained by a direct impact of the ligand on catalytically active intermediates only, but influences on the formation of these species must also be taken into account.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290118
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    Hybrid Diborolyl/Dicarbaboranyl Triple-Deckers: [(μ5-Cyclopentadienyl)cobalt][μ,η5-1,3-diborolyl)cobalt[dicarba-heptacarboranyl and -nonacarboranyl ComplexesDedicated to Prof. H. Roesky on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 213-217 
    Details
    ISSN: 0009-2940
    Keywords: Triple-decker complexes ; Cobaltadicarba-closo-octaborane ; Cobaltadicarba-closo-decaborane ; Rearrangements ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The three-component reactions of the sandwich anion [(η5-C5H5)Co(η5-Et4MeC3B2)]- (4-H)- and various dicarbaborane anions with metal halides are described. Thus, (4-H)-, nido-4,5-C2B6H9- (5), and CoCl2 form the 30VE triple-decker [η5-C5H5)Co(μ,η5-Et4MeC3B2)Co(η5-2,3-C2B5H7)] (6). An analogous three-component reaction of (4-H)-, arachno-4,5-C2B7H-2 (7), and CoCl2 yields [(η5-C5H5)Co(μ,η5-Et4-MeC3B2)Co(η5-6,9-C2B7H9)] (8), which rearranges on heating (57°C) to give the 1,6-isomer [(η5-C5H5)Co(μ,η5-Et4-MeC3B2)Co(η5-1,6-C2B7H9)] (9) with an activation energy of 127 · 10 kJ/mol. The thermodynamically most stable 1,10-isomer [(η5-C5H5)Co(μ,η5-Et4MeC3B2)Co(η5-1,10-C2B7H9)] (10) is formed by heating of 9 at 180°C. An alternative route to 9 is provided by the reaction of arachno-6,8-C2B7H12- (11) with (4-H)- and CoCl2. The analogous reaction with RhCl3 leads to [(η5-C5H5)Co(μ,η5-Et4MeC3B2)Rh(1,6-C2B7H9)] (15) and unexpectedly to closo-2-(η5-C5H5)Co(1,6-C2B7H9) (12). The constitutions of the described compounds are derived from their 1H-, 11B-, 13C-NMR data as well as mass spectral data. The X-ray structure analyses of 10 and 12 show the expected metal complexes with a CoC2B7H9 framework. In 10 the carbon atoms occupy the capping positions of a bicapped square antiprism. The short Co-Co distance of 3.20 Å is in agreement with the 30VE configuration of 10. In both 10 and 12, the distance from the cobalt to the four-coordinate C4 is the shortest Co-to-cage atom distance.
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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.19961290301
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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).
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    URL: http://dx.doi.org/10.1002/cber.19961290504
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    A Synthetic and Theoretical Study of the Aggregation of Amidoaluminium Hydrides: Solid-State Structure of the Trimethylamine Adduct [(Me3Si)2NA1(Cl)(H) · NMe3] (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 545-549 
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    ISSN: 0009-2940
    Keywords: Alane ; Association ; Hydride ; Amido ; Amide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The amidoaluminium hydride complexes [(Me3Si)2NA1(X)(H) · NMe3], X = H (1), Cl (2), were prepared by the metallation of bis(trimethylsilyl)amine by Al(X)(H)2 · NMe3 (X = H and Cl). The molecular structure of 2 as a monomeric Lewis base adduct with four-coordinate aluminium centres and terminal amido groups was confirmed by X-ray crystal structure determination. We also find that bis(trimethylsilyl)amine forms a thermally stable adduct of alane, (Me3Si)2N(H) · AlH3 (3). Ab initio molecular orbital calculations on the possible products arising from these reactions yielding 1 and 2 revealed that the amido-bridged species, {(μ-H2N)Al(X)H}2 (X = H and Cl), are favoured over nitrogen donor Lewis base adduct formation, H2NAl(X)(H) · NH3 (X = H and Cl), and then chloro-bridged, {H2NAl(μ-X)(H)}2, (X = Cl only), and hydrido-bridged species, {H2NAl(X)(μ-H)}2 (X = H and Cl).
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290511
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    On the Chemistry of Gallium, 8Part 7: Ref.[1].. Synthesis and Structure of [Tris(trimethylsilyl)silyl]-Substituted Gallanes and Gallates (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 561-569 
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    ISSN: 0009-2940
    Keywords: Silylgallanes ; Gallium compounds ; Hydroxygallium compounds ; Gallium alkoxides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of lithium tris(trimethylsilyl)silanide · 3 THF with R2GaCl (R = 2,2,6,6-tetramethylpiperidino, Me, Cl) yields tmp2GaSi(SiMe3)3 (3) and R2Ga(THF)Si(SiMe3)3 (R = Me, Cl) (7, 9). Both gallium nitrogen bonds in 3 are cleaved by protic reagents. Depending on the acidity of these agents, either oligomeric gallanes [(RO)2GaSi(SiMe3)3]n (R = Et, H, n = 2, 3) (11, 12) or tetramethylpiperidinium gallates [X3GaSi-(SiMe3)3]- (X = OPh, Cl) (13, 14) are formed. Hydroxide 11 adds lithium hydroxide to afford the mixed lithium gallium hydroxide 15. Single-crystal X-ray diffraction studies confirm the suggested constitutions. The gallium-silicon bond can adopt values between 236 and 247 pm. Here electronic influences of the substituents on the gallium center are of great importance as well as their steric demand. This is underlined by quantum chemical calculations on the ab initio (SCF) level.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290514
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    Palladium-Copper-Catalyzed Coupling of Tricarbonylchromium-Complexed Phenylacetylene with Iodoarenes - A Facile Access to Alkynyl-Bridged Cr(CO)3-Complexed Benzenes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 607-613 
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    ISSN: 0009-2940
    Keywords: Arene complexes ; Chromium compounds ; Alkynes ; Catalysis ; Coupling reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The palladium-copper-catalyzed coupling of the tricarbonyl-chromium-complexed chlorobenzene 1 with (trimethylsilyl)-acetylene gives tricarbonyl{η6-[(trimethylsilyl)ethynyl]-benzene}chromium(0) (2) in high yield. After desilylation of 2 tricarbonyl[η6-(ethynylbenzene)]chromium(0) (3) is obtained quantitatively. Using the palladium-copper-catalyzed methodology, we can readily introduce Cr(CO)3-complexed phenylethynyl units by a multifold coupling of 3 with iodobenzene, 1,2-, 1,3-, 1,4-di- and 1,3,5-tiiodobenzene (4a-e) or 1 to give polynuclear Cr(CO)3-complexed (phenylethynyl)benzenes 5a-e and doubly Cr(CO)3-complexed tolane 6 in good to moderate yield. The crystal structure analyses of μ3-{η6:η6:η6[1,3,5-benzenetriyltris(2,1-ethynediyl)]tris(benzene)}tris[tricarbonylchromium(0)] (5e) and μ-{η6:η6-[1,2-ethynediylbis(benzene)]}bis[tricarbonylchromium(0)] (6) reveal that the tricarbonylchromium tripods in the same molecule are arranged in antiparallel syn-eclipsed conformations. The Eglington coupling of 3 affords a doubly Cr(CO)3-complexed diphenylbutadiyne 7 in excellent yield.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290604
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    Preparation, Properties, and Reactions of Metal-Containing Heterocycles, XCIIIPart XCII: E. Lindner, P. Fisahn, R. Fawzi, M. Steimann, Chem. Ber. 1996, 129, 191-199.. Diosma[5.n.5.n]ortho-, -meta-, and -paracyclophanes (n = 0-2)Dedicated to Professor Erwin Weiss on the occasion of his 70th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 639-645 
    Details
    ISSN: 0009-2940
    Keywords: Metallacyclophanes ; Osmium complexes ; Iron complexes ; Oxocyclophanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of the ortho-, meta-, and para-bis(triflates) [(F3CSO2OCH2CH2C6H4)2(CH2)n] with n = 0 (ortho: 1a), n = 0, 1 (meta: 1b, d), and n = 0-2 (para: 1c, e, g) with [Os(CO)4]2- results in the formation of the diosma[5.n.5.n]-ortho-, -meta-, and -paracyclophanes with n = 0 (ortho: 2a), n = 0, 1 (meta: 2b, d), and n = 0-2 (para: 2c, e, g). On reaction of the bis(triflates) 1a, b with the dianionic [Fe(CO)4]2- the corresponding ferracyclophanes are formed only in situ. Carbon monoxide insertion into the Fe-C s̰ bonds of the ferracycles affords the ketones 6a, b. The structures of 2a and 2e were investigated by X-ray structural analysis. Compounds 2a and 2e crystallize in the space group P21/c with Z = 8 and P1 with Z = 2, respectively.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290608
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  • 196
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    Hexacoordinated Group-14 Elements with Phosphorus Donor Ligands: Syntheses and Structures of Cl2E[C(PMe2)2(SiMe3)]2 (E = Si, Ge, Sn) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 671-676 
    Details
    ISSN: 0009-2940
    Keywords: Hexacoordination ; Silicon ; Germanium ; Tin ; Phosphinomethanide Ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The group-14 tetrahalides ECl4 (E = Si, Ge, Sn) react with two equivalents of Li[C(PMe2)2(SiMe3)] to give the trans-hexacoordinated complexes Cl2E[C(PMe2)2(SiMe3)]2, which were characterized spectroscopically and by structure determinations in the solid state. The complexes were found to crystallize with or without tetrahydrofuran (THF) molecules, depending on the presence or absence of this solvent. In the case of the silicon complex, the structures of both crystal forms were determined, showing slightly different molecular structures of the complexes in the solid state. Without cocrystallized THF, Cl2Si[C(PMe2)2(SiMe3)]2 has no crystallographically imposed molecular symmetry, while in the presence of THF its crystallographic symmetry is C2h (2/m). The tin and germanium complexes were crystallized either with and without THF molecules, respectively, their crystal structures being isotypic with the respective ones of the silicon complex. In all cases, small amounts of the cis-hexacoordinated isomers were also observed in solution, but only in the case of the silicon complex, it was isolated in pure form. It rearranges to the trans isomer at ambient temperature. trans-Cl2Si[C(PMe2)3]3, trans-Cl2Si[C(PPh2)2(SiMe3)]2 and cis-Me2-Si[C(PMe2)2(SiMe3)]2 were likewise obtained.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290613
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  • 197
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    New β-Amino Alcohols as Chiral Ligands for the Catalytic Enantioselective Reduction of Prochiral Ketones and the Nucleophilic Addition of Diethylzinc to BenzaldehydeDedicated to Dr. Werner Schwarze. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 691-695 
    Details
    ISSN: 0009-2940
    Keywords: β-Amino alcohols ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New optically active β-amino alcohols, derived from various acyclic and cyclic amino acids with alkyl groups on the carbinol carbon atom, were used in the enantioselective reduction of prochiral ketones. The attachment of alkyl groups to the nitrogen atom of the catalyst (R)-1b was shown to influence favorably the enantioselectivity of the addition of diethylzinc to benzaldehyde. In both cases the resulting secondary alcohols were obtained in moderate to high optical yields.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290616
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  • 198
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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.19961290701
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  • 199
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    Self-Assembly of a Triple-Stranded meso-Helicate from Two Iron(II) Ions and Three [CH2]3-Bridged Bis(2,2′-bipyridine) Ligands (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 829-832 
    Details
    ISSN: 0009-2940
    Keywords: Self-assembly ; meso-Helicate ; Binuclear coordination compounds ; 2,2′-Bipyridines ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,3-Bis(5′-methyl-2,2′-bipyrid-5-yl)propane (3) can be synthesized by a two-step procedure starting from 3-picoline (1). In a spontaneous self-assembly process 3 forms the binuclear triple-stranded meso-helicate [(3)3Fe2][PF6]4 on addition of iron(II) salts. The (Λ,Δ) structure can be shown by symmetry considerations based on NMR spectroscopy and is due to the conformational restrictions of the [CH2]3 spacer.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290714
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  • 200
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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.19961290801
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