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  • 1
    Electronic Resource
    Electronic Resource
    Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, LXXVII Synthese, Struktur und Reaktivität von Phosphametallacyclopropanen mit isolobalen ER- (E = N, P, As, Sb) und Fe(CO)4-Bausteinen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2171-2179 
    Details
    ISSN: 0009-2940
    Keywords: Phosphametallacyclopropanes ; Isolobal building blocks ; Lewis basic behavior ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal-Containing Heterocycles: Preparation, Properties, Reactions, LXXVII. - Synthesis, Structure and Reactivity of Phosphametallacyclopropanes with Isolobal ER (E = N,P,As,Sb) and Fe(CO)4 Building BlocksThe phosphidometallates \documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ Li_2 \left\{ {\left[ M \right]\dddot - PPh_2 } \right\} $\end{document} {[M] = (η5-C5H5)M-(CO)2}, resulting from the metal hydride complexes H[M]PPh2H [M = Cr (1), Mo (2), W (3)] by reduction with nBuLi, react with the geminal dihalides RECl2 to give the three-membered phosphametallacyclopropanes [ER = NC6F5 (M = Cr (1a), Mo (2a), W (3a)), PPh (M = Cr (1b), Mo (2b), W (3b)), PC6H11 (M = Cr (1c), Mo (2c), W (3c)), P-tBu (M = Cr (1d), Mo (2d), W (3d)), P(2,4,6-(tBu)3C6H2) (M = Cr (1e), Mo (2e), W (3e)), As(2,4,6-(tBu)3C6H2) (M = Cr (1f), Mo (2f), W (3f)), Sb-tBu (M = Cr (1g), Mo (2g))]. Reaction of Br2Fe(CO)4 with the corresponding dilithium compounds \documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ Li_2 \left\{ {\left[ M \right]\dddot - PPh_2 } \right\} $\end{document} affords the phosphido-bridged heterodimetallic complexes . According to X-ray structural analyses in 2a and 2f the P - E bond distances are shortened while the Mo - E bonds are significantly elongated compared to a single bond. (OC)5CrTHF is added to the Lewis basic E atom in 2b, 2d, and 2g with loss of THF to give P-tBu (4d), Sb-tBu (4g)]. By this reaction the antimony-containing ring 2g is kinetically stabilized. Because of the low basicity of the N atom in 2a no addition was observed. The ring skeleton of 4b and 4g, undergoes no change by Cr(CO)5 coordination as shown by X-ray structural analyses.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911241005
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  • 2
    Electronic Resource
    Electronic Resource
    Synthese und Struktur von Schwefel-, Schwefelmonoxid- und Schwefeldioxid- verbrückten dimetallischen Komplexen des Typs [M(CO)(dppm)]2(μ-S)(μ-L) und [(CO)3M'(dppm)2MX](μ-L') (M = Rh, Ir; M' = Mo, W, Mn; L = SO, SO2; L' = S, SO2; X = Cl, CO) (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2217-2222 
    Details
    ISSN: 0009-2940
    Keywords: A-Frame complexes ; SO2-bridged complexes ; S, SO, and SO2 ligands ; Insertion reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Structure of Sulfur-, Sulfur Monoxide-, and Sulfur Dioxide-Bridged Dimetallic Complexes of the Type [M(CO)(dppm)]2(μ-S)(μ-L) and [(CO)3M'(dppm)2MX](μ-L') (M = Rh, Ir; M' = Mo, W, Mn; L = SO, SO2; L' = S, SO2; X = Cl, CO)The homo- and heterodimetallic complexes [M(CO)(dppm)]2-(μ-S)(μ-SO2) (M = Rh, Ir) (2a, b), [(CO)3M'(dppm)2MCl](μ-SO2) (M' = Mo, W; M = Rh, Ir) (4a - c), and [(CO)3Mn(dppm)2- Rh(CO)] (6) by passing sulfur dioxide through their solutions. The X-ray structure analysis of 5a shows the SO2 ligand in a bridging position, whereas one CO ligand is semibridging. Treatment of the same starting materials with thiirane S-oxide does not lead to the corresponding SO-bridged dimers, with the only exception of 1b, which yields the new SO complex [(Ir(CO)(dppm)]2(μ-S)(μ-SO) (3b). Passing H2S through a solution of 6, the sulfur-bridged complex [(CO)3Mn(dppm)2- Rh(CO)](μ-S) (8) is formed, accompanied by H2 elimination.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911241012
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  • 3
    Electronic Resource
    Electronic Resource
    Die Kristallstrukturen von {Li3(12-Krone-4)2[HC(CN)2]3}, {Na(15-Krone-5)-[HC(CN)2]} und {Na[N(nBu)4][HC(CN)2]2 · THF} (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 87-92 
    Details
    ISSN: 0009-2940
    Keywords: Lithium dicyanomethanide ; Sodium dicyanomethanide ; Dicyanomethanides, lithium, sodium, tetrabutylammonium salts ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Crystal Structures of {Li3(12-crown-4)2[HC(CN)2]3}, {Na(15-crown-5)[HC(CN)2]}, and {NaN(nBu)4[HC(CN)2]2 · THF}The preparation and the crystal structures of the title compounds 1 - 3 are described. 1 forms a polymeric chain structure, in which one of the lithium ions is linked by Li…NCC(H)CN… bridges. The remaining lithium ions form (12-crown-4)Li[NCC(H)CN] units, which are coordinated by one of the nitrogen atoms of the dicyanomethanide ions with the lithium ions of the chain. 2 forms an ion pair, in which the sodium ion is coordinated by the five oxygen atoms of the crown ether molecule and by one nitrogen atom of the dicyanomethanide ion. 3 has a threedimensional network, in which the sodium ions are coordinated in a distorted tetrahedral manner by the nitrogen atoms of the dicyanomethanide ions. In the cavities of the network the tetrabutylammonium ions and the THF molecules are found.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250114
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  • 4
    Electronic Resource
    Electronic Resource
    Neuartige basische Liganden für die homogenkatalytische Methanolcarbonylierung, XXXVIII. Synthese, Eigenschaften und fluktuierendes Verhalten von (Ether-Phosphan)palladium-Komplexen (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 2255-2260 
    Details
    ISSN: 0009-2940
    Keywords: Ether-phosphines ; Palladium complexes ; Fluxional behavior ; Hydrogenation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Novel Basic Ligands for the Homogeneous Catalytic Carbonylation of Methanol, XXVIII.  -  Synthesis, Properties and Fluxional Behavior of (Ether-Phosphine)palladium ComplexesCl2Pd(COD) (1) (COD = 1,5-cyclooctadiene) reacts with 1 equiv, of the (ether-phosphine) ligand Ph2P∼D (2a-c) (D = CH2C4H7O (a), CH2C4H7O2 (b), CH2CH2OCH3 (c)] to give the dimeric complexes [μ-ClPdCl(Ph2P∼D)]2 (3a-c) (P∼D = η1-P-coordinated). According to the field-desorption mass spectra which show only one peak for the monomeric moieties ClPd(Ph2P∼D), 3a-c have a very weak Pd2Cl2 bridge. trans-Cl2Pd(Ph2P∼D)2 (4a-c) is obtained either from 3a-c and 2a-c by cleaving the Pd2Cl2 bridge or from 1 and 2 equiv. of the ligands 2a-c. 4c crystallizes in the monoclinic space group P21/c with Z = 2. AgClO4 selectively abstracts one Cl⊖ ligand from 4a-c which results in the formation of the cationic complexes [trans-(Ph2P∩D)(Ph2P∼D)PdCl]⊕ (5a-c) (P∩D = η2-D,P-coordinated) containing one chelated and one η11-P-bonded (ether-phosphine) ligand. 5a-c show fluxional behavior which is demonstrated by temperature-dependent 31P{1H}-NMR investigations. The coalescence points have been determined and are at 253 (5a), 303 (5b), and 283 K (5c). The activation enthalpies ΔG
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901231205
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  • 5
    Electronic Resource
    Electronic Resource
    Stereoelectronic and Steric Effects in the Synthesis and Recognition of Diastereomeric Ethers by NMR and EPR SpectroscopyHerrn Professor Ernst Buyer zum 65. Geburtstag gewidmet. (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 857-865 
    Details
    ISSN: 0009-2940
    Keywords: Quinone methides ; Stereoelectronic effects ; Chiral recognition ; EPR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (2,6-Di-tert-butyl-4-hydroxyphenyl)-alkyl-carbinols I are easily dehydrated in the presence of catalytic amounts of a mineral acid to form the corresponding phenyl-alkyl-carbocations Ia. These cations can be reversibly deprotonated to the quinone methides Ib, therefore, an equilibrium between both reactive compounds is assumed. In the absence of nucleophiles a reaction of these intermediates with the starting carbinol is observed leading to symmetrical ethers Id. In alcoholic solution the solvent acts as a nucleophilic compound and the formation of an unsymmetrical ether Ie is observed predominantly. If the nucleophile contains a chiral carbon atom diastereomers are formed in this reaction which are observed in variable concentrations depending on the reaction time. The assignment of these isomers to the meso and racemic compound has been achieved by NMR investigations in solution in combination with their solid-state structures determined by X-ray crystallography. These results indicate a remarkable thermodynamic stabilization of the symmetrical ethers in the racemic form whereas the meso compounds are favored if the products are formed under kinetic control. In both cases the diastereomer ratio is determined by steric repulsion and the generalized anomeric effect. - A bonding interaction of lone pairs of the ether oxygen with the π system of the corresponding phenoxyl ring was also observed by EPR investigations. This electron delocalization contributes remarkably to the mechanism responsible for the distinction of the diastereomeric radicals by different β-proton coupling constants.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250417
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  • 6
    Electronic Resource
    Electronic Resource
    Tris(trimethylsilyl)arsan als Edukt für Tri- und Tetraferrioarsonium-Salze; Kristallstruktur von [{Cp(CO)2Fe}3AsOH]B(C6H5)4 (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 251-256 
    Details
    ISSN: 0009-2940
    Keywords: Arsonium salts, tri- and tetraferrio- / Arsane, tris(trimethylsilyl)- / Permetalated tetrahedral main group elements ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(trimethylsily1)arsane as a Starting Compound for Tri- and Tetraferrioarsonium Salts; Crystal Structure of [{Cp(CO)2Fe}3AsOH]B(C6H5)4Tris(trimethylsilyl)arsane (1) reacts with an excess of CpFe(O)2Cl (2) to give tetraferrioarsonium chloride [{Cp(CO)2Fe}4As]Clk (4a), which may be converted into the corresponding tetraphenylborate 4b by Na[B(6H5)4]. In the Presence of water one organometallic ligand is hydrolysed to yield the triferriohydroxyarsonium tetraphenylborate 5 which crystallizes in the triclinic space group P&1bar; and shows a trigonal pyramidal configuration at the arsenic atom.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901230205
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  • 7
    Electronic Resource
    Electronic Resource
    η1-P- und η2-OP-gebundene (Ether-phosphan)osmium(II)-Komplexe und ihre gegenseitige Umwandlung (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 541-550 
    Details
    ISSN: 0009-2940
    Keywords: Ether phosphanes ; Osmium(II) complexes ; Conversion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: η1-P- and η2-OP-Bonded (Ether-Phosphane)Osmium(II) Complexes and their Mutual ConversionReactions of cis-Br2Os(CO)4 with the (ether-phosphane) ligands 2a-f results in the formation of the cis,cis,trans-complexes Br2Os(CO)2(P ∼ O)2 (3a-f). 3b crystallizes in the mono-clinic space group P21/c with Z = 4. Irradiation of 3a-f leads to the cleavage of a further CO group and the formation of an Os—O bond to give the mono(chelate) complexes Br2Os(CO)-(PO) PO (5a-f), with one of the O,P ligands being bidentate. 5a-f exist as mixtures of different trans-P (A,B) and cis-P isomers (C-G). Dependent on the fact that a reversible cis/trans equilibrium or an irreversible trans → cis transformation is possible or that no trans-P isomers are present at any temperature, 5a-f may be classified in three categories. Inter-conversion of the isomers A-G results from dissociation of the η1-P coordinated ether-phosphane and concomitant occurrence of the 16e- species Br2Os(CO)(PO) (8). From temperature-dependent 31P{1H}-NMR spectroscopic investigations the temperature for the reversible opening of the metal-oxygen contact is determined. The reversible opening leads to the complexes Br2Os(CO)(PO)2 (9) with a vacant coordination site depending on the Os-O bonding strength. 5a-f react with CO to give all-trans-Br2Os(CO)2(PO)2 (4a-f). The action of the ether-phosphanes 2a-f on OsBr2(PPh3)4 (7) affords the bis(chelate) complexes Br2Os(PO)2 (6a-f) which add carbon monoxide to form all-trans-4a-f.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250303
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  • 8
    Electronic Resource
    Electronic Resource
    Preparation and Crystal Structures of Gold(I) Complexes of a Series of Benzenethiolates: Pair Formation by Gold-to-Gold Interactions of (Benzenethiolato)(triphenylphosphane)gold(I) (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 605-610 
    Details
    ISSN: 0009-2940
    Keywords: Gold(I) complexes ; Gold(I) thiolates ; Thiolato complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chloro(triphenylphosphane)gold(I) reacts readily with benzenethiol C6H5SH and a series of sterically hindered (2,4,6-trialkylbenzene)thiols 2,4,6-R3C6H2SH in the presence of NEt3 to yield stable gold(I) complexes Ph3PAu(S - 2,4,6-C6H2R3) [R=H (1), Me (2), Et (3), iPr (4)]. The crystal structures of these complexes have been determined by single-crystal X-ray diffraction analysis. In all compounds the gold atoms are linearly two-coordinate with very similar bond lengths and angles. - While complexes 2 - 4 with bulky thiolate ligands are monomeric in the crystal lattice, complex 1 has been found to form pairs of molecules with intermolecular gold - gold contacts of 313.5(5) pm. The Mössbauer spectra of the complexes exhibit large isomer shifts (I.S.), ranging from 3.06 to 3.72 mm s-1, and quadrupole splittings (Q.S.), ranging from 7.90 to 8.68 mm s-1. These data can be attributed to the strong electron-donating properties of the benzenethiolate ligands. The gold - gold contacts in complex 1 lead to I.S. and Q.S. values which are slightly smaller than those of 2 - 4. The Au - S distances do not show a major influence of the S - Au - P pairing in complex 1 as compared to complexes 2 - 4.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260310
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  • 9
    Electronic Resource
    Electronic Resource
    Disproportionierung von Schwefeldioxid am Molybdän(0)-Komplex trans-[(dppe)2Mo(N2)2] Molekülstruktur von trans-[(dppe)2Mo(S)O]·SO2·H2SO4 (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 979-982 
    Details
    ISSN: 0009-2940
    Keywords: Chalkogenido complex, mixed, of molybdenum ; Disproportionation of SO2 ; Sulfur, dioxide, monoxide ; Oxidative addition of SO ; Molybdenum complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Disproportionation of Sulfur Dioxide by the Molybdenum(0) Complex trans-[(dppe)2Mo(N2)2]. Molecular Structure of trans-[(dppe)2Mo(S)O]·SO2·H2S04Sulfur dioxide disproportionates into sulfur monoxide and sulfuric acid, when it is passed through a solution of the molybdenum(0) complex trans-[(dppe)2Mo(N2)2] (1) in toluene. Whereas SO undergoes an oxidative addition reaction onto the intermediate 14 VE-complex fragment (dppe)2Mo to give the mixed dichalkogenidomolybdenum(IV) complex trans-[(dppe)2Mo(S)O] (3), both molecules H2SO4 and intact SO2 remain in the solvating sphere. According to an X-ray structural analysis 3 crystallizes in the monoclinic space group P21/n and shows an octahedral configuration at the central molybdenum atom with the oxo and sulfido ligands in trans positions; the two solvent molecules ethanol and toluene are also incorporated into the crystal lattice.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901230508
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  • 10
    Electronic Resource
    Electronic Resource
    Synthesis, X-Ray Crystal Structure, and Fluxional Behaviour of fac-[Ru(CH3CO2)2(PPh3)3] · 2 CH3CO2H (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2691-2695 
    Details
    ISSN: 0009-2940
    Keywords: fac-[Ru(O2CCH3)2(PPh3)3] · 2 CH3CO2H ; Tris(triphenylphosphane)ruthenium(II) ; Polymerization ; Bicyclo[2.2.1]hept-2-ene ; Ruthenium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [Ru2(μ-O2CCH3)4(O2CCH3)] reacts with excess triphenylphosphane in acetic acid to give fac-[Ru(O2CCH3)2(PPh3)3] · 2CH3CO2H (1), which crystallizes in the triclinic space group P 1- with Z=2. The three phosphane ligands are in the sterically congested facial configuration, and the distorted octahedral geometry around the metal is completed by a unidentate and chelating acetate. A variable temperature 31P{1H}-NMR study of the complex in CH2Cl2 showed the three phosphanes to be inequivalent at low temperature. On raising the temperature two separate coalescence processes are observed, ultimately making all of the phosphanes equivalent at room temperature. Complex 1 shows slight catalytic activity for the ring-opening polymerization of bicyclo[2.2.1]hept-2-ene (norbornene).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911241209
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