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  • 1
    Electronic Resource
    Electronic Resource
    Decabenzylgermanocen, -stannocen und -plumbocen. Synthese und Struktur von luftstabilen Metallocenen der 4. Hauptgruppe des Periodensystems der Elemente (1986)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 119 (1986), S. 2656-2667 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Decabenzylgermanocene, -stannocene and -plumbocene. Synthesis and Structure of Air-stable Metallocenes of Main Group IVGermanium diiodide, tin dichloride, or lead diacetate reacts with pentabenzylcyclopentadienyllithium (1) to give decabenzylgermanocene (2), decabenzylstannocene (3) or decabenzylplumbocene (4), respectively. The air-stable metallocenes were characterized by IR, Raman, NMR, tin-119m-Mössbauer (3), and mass spectroscopy. The X-ray structural analysis shows for all three compounds an angle of 31 to 36° between the planes of the two cyclopentadienyl rings and a shielding of the lone pair of electrons at the metal atom by three of the ten benzyl groups each.
    Notes: Germaniumdiiodid, Zinndichlorid bzw. Bleidiacetat reagiert mit Pentabenzylcyclopentadienyllithium (1) unter Bildung von Decabenzylgermanocen (2), Decabenzylstannocen (3) bzw. Decabenzylplumbocen (4). Die luftstabilen Metallocene wurden durch IR-, Raman-, NMR-, 119mSn-Mößbauer- (3) und Massenspektren charakterisiert. Die Röntgenstrukturanalyse der Verbindungen zeigt, daß die Ebenen der beiden Cyclopentadienylringe einen Winkel zwischen 31 und 36° einschließen, und daß eine Abschirmung des freien Elektronenpaares am Metallatom jeweils durch drei der zehn Benzylgruppen erfolgt.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19861190822
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  • 2
    Electronic Resource
    Electronic Resource
    Binary [Hydrotris(1,2,4-triazolyl)borate]metal Complexes [M{HB(C2H2N3)3}2] with M = Fe, Co, Cu, Zn: Synthesis, Characterization, Magnetochemistry, and X-ray Structure of [Cu{HB(C2H2N3)3}2·4CH3 (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 1379-1385 
    Details
    ISSN: 0009-2940
    Keywords: Hydrotris(triazolyl)borate ; metal complexes ; Chelate ligands ; Clathrates ; Magnetochemistry ; Spin crossover ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The bis[hydrotris(1,2,4-triazolyl)borate]metal complexes [M{HB(C2H2N3)3}2] with M = Fe (5), Co (6), Cu (7), Zn (8) are obtained from MX2 and K[HB(C2H2N3)3] (9). The complexes are characterized by IR, UV/Vis, and MS. Temperature-variable magnetic measurements show a Curie-Weiss behavior for the paramagnetic complexes 6 and 7 with a temperature-dependent magnetic moment for 6. The iron complex 5 exhibits a spin crossover from diamagnetic to paramagnetic, starting at around 270 K. Single-crystal X-ray structures of the solvates 7 · 4 CH3OH and 9 · 2 H2O have been determined. The structure of 7 · 4 CH3OH shows the Jahn-Teller distorted copper complex 7 surrounded by methanol molecules through hydrogen bonding to exocyclic nitrogen atoms of the tris(1,2,4-triazolyl)borate ligand. The crystal system for 7 · 4 CH3OH is monoclinic, space group P21/n. Compound 9 · 2 H2O is a one-dimensional coordination polymer with the potassium atom bridged by the water molecules and the tris(1,2,4-triazolyl)borate ligand and crystallizes in the orthorhombic space group Ccm21.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941270809
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  • 3
    Electronic Resource
    Electronic Resource
    Transition-Metal Complexes with the Novel Scorpionate Ligand Dihydrobis-(tetrazolyl)borate: Synthesis and Characterization of Infinite Two-Dimensional Metal-Ligand Frameworks and One-Dimensional Water SubstructuresDedicated to Professor Dr. Herbert Schumann on the occassion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 323-328 
    Details
    ISSN: 0009-2940
    Keywords: Poly(azolyl)borates, metal complexes of ; Bis(tetrazolyl)borate, metal complexes of ; Metal-nitrogen coordination ; Coordination polymers ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Dihydrobis(tetrazolyl)borate metal compounds of the composition [M(L)2{μ-H2B(CHN4)2}2]n for M = Mn, Fe, Co, Zn, Cd with L = H2O and for M = Cu with L = NH3 are obtained from metal salts and K[H2B(CHN4)2]. Single-crystal X-ray studies reveal the formation of two-dimensional rhombic grid sheets through the bridging action of the bis(tetrazolyl)borate ligands. Each metal atom is octahedrally coordinated with two trans L ligands and four H2B(CHN4)-2 nitrogen donors. Two additional, hydrogen-bonded water molecules occupy the rhombic openings in the compounds with M = Mn, Fe, Co, Zn, and Cd. The water of crystallization is held in place through hydrogen bonding from the water ligands and to the nitrogen atoms to give a substructure of parallel kinked water chains. Temperature-variable magnetic measurements show a Curie-Weiss behavior for the paramagnetic complexes with M = Mn, Fe, Co, and Cu.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280402
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  • 4
    Electronic Resource
    Electronic Resource
    Tetraphenylcyclopentadien und (4-tert-Butylphenyl)tetraphenylcyclopentadien: Synthese und Charakterisierung ihrer Alkalimetallsalze und Metallocene von Germanium, Zinn und Blei (1988)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 121 (1988), S. 207-218 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetraphenylcyclopentadiene and (4-tert-Butylphenyl)tetraphenyl-cyclopentadiene: Synthesis and Characterization of their Alkali-Metal Salts and Metallocenes of Germanium, Tin, and LeadTetraphenylcyclopentadiene (1) and (4-tert-butylphenyl)tetraphenylcyclopentadiene (11), their alkali-metal salts (2-4 and 12, 13, respectively) and their air-stable metallocenes of germanium (5, 15), tin (6, 16) and lead (7, 17) were synthesized and characterized by IR, Raman, 1H-NMR, 13C-NMR, and mass spectra as well as by X-ray powder diagrams. Comparative 13C-NMR studies including tetraphenylcyclopentadienyl bromide (8), (4-tert-butylphenyl)tetraphenylcyclopentadienol (9), and (4-tert-butylphenyl)tetraphenylcyclopentadienyl bromide (10) prove a delocalisation of the negative charge from the C5 ring into the nonparallel phenyl ligands.
    Notes: Von Tetraphenylcyclopentadien (1) und (4-tert-Butylphenyl)tetraphenylcyclopentadien (11) wurden die Alkalimetallsalze (2-4 bzw. 12, 13) und die luftstabilen Metallocene von Germanium (5, 15), Zinn (6, 16) und Blei (7, 17) synthetisiert und durch IR-, Raman-, 1H-NMR, 13C-NMR und Massenspektren sowie durch Röntgenpulverdiagramme charakterisiert. Vergleichende 13C-NMR-Studien unter Einbeziehung von Tetraphenylcyclopentadienylbromid (8), (4-tert-Butylphenyl)tetraphenylcyclopentadienol (9) und (4-tert-Butylphenyl)tetraphenylcyclopentadienylbromid (10) beweisen eine Delokalisierung der negativen Ladung des C5-Ringes in die nicht parallel angeordneten Phenylgruppen.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19881210203
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  • 5
    Electronic Resource
    Electronic Resource
    Decaphenylgermanocen, -stannocen und -plumbocen sowie Pentaphenylstannocen: Synthese, Eigenschaften und CPMAS-Metall-NMR-Messungen (1988)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 121 (1988), S. 1745-1751 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Decaphenylgermanocene, -stannocene, and -plumbocene and Pentaphenylstannocene:Synthesis, Properties, and CPMAS-Metal-NMR MeasurementsAn improved synthesis is described for pentaphenylcyclopentadienol (1), pentaphenylcyclopentadienyl bromide (2), pentaphenylcyclopentadiene (3), and pentaphenylcyclpentadienyllithium (4a). Decaphenylgermanocene (5), -stannocene (6), and -plumbocene (7) as well as pentaphenylstannocene (8) are prepared. Complete analytical data (IR, Raman, X-ray powder, NMR, mass, and 119mSn-Mößbauer spectra) are given. 119Sn- and 207Pb-CPMAS NMR measurements of various stannocenes and of the plumbocenen 7 are reported for the first time.
    Notes: Ein verbesserter Syntheseweg für Pentaphenylcyclopentadienol (1), Pentaphenylcyclopentadienylbromid (2), Pentaphenylcyclopentadien (3), und Pentaphenylcyclopentadienyllithium (4a), die Darstellung von Decaphenylgermanocen (5), -stannocen (6) und -plumbocen (7) sowie von Pentaphenylstannocen (8) wird beschrieben. Die vollständigen analytische Daten (IR-, Raman-, Röntgenpulver-, NMR-, Massen- und 119mSn-Mößbauer-Spektren) werden angegeben. Es werden 119Sn- und 207Pb-CPMAS-NMR-Messungen von verschiedenen Stannocenen und dem Plumbocen 7 mitgeteilt.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19881211008
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  • 6
    Electronic Resource
    Electronic Resource
    Metal-Metal Bonding in Paramagnetic Chromium(III) Complexes - An MO-Theoretical Case Study (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 631-643 
    Details
    ISSN: 0009-2940
    Keywords: Chromium(III) alkyls ; Paramagnetism ; Calculations, MO ; Metal - Metal bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electronic structures of the edge-sharing bioctahedral chromium(III) dimers {C5H5Cr(CH3)(μ1-Cl)}2 (2) and {Me5C5Cr(CH3)(μ1-CH3)}2 (4* (Cp* derivative), 4 (Cp derivative)), the trinuclear complex {C5H5Cr(μ1-Cl)}3(μ1-CH) (3), and the face-sharing bioctahedral chromium(III) compounds {Me5C5Cr}2(μ1-CH2) (6*, 6) [{Me5C5Cr}2(μ1-CH3)3]+ (7*, 7) have been studied MO-theoretically by the extended Hückel method. Proceeding from 2 over 3 to 4*, or from 6* to 7* a 3-center/4-electron chloride or methylene bridge is replaced by a 3-center/2-electron methyl group (a methylidyne cap in the trimer). The 3c/2e bridges give rise to an increased metal - metal overlap population due to Cr - Cr bonding within the core levels. In the series of 2 - 3 - 4* this is accompanied by a decrease in the Cr - Cr distance (329 - 284 - 260 pm) and effective magnetic moment, μeff (2.53 - 2.05 - 1.53 μB per Cr at room temp.). The latter can be ascribed to an increased splitting within the chromium d-block because of the shorter metal-metal separation. The bioctahedra 6* and 7* feature even shorter Cr - Cr contacts than 4* (239 and 242 pm), primarily because of their face-sharing geometry. However, their effective magnetic moments (per Cr) are 2.33 and 1.32 μB at room temp. The high magnetic moment for 6* can be understood from the orbital interactions in the frontier orbital metal d block: A face-sharing bioctahedron shows one σ, two δ, and no π type overlap, while an edge-sharing bioctahedron (4) has σ, π, and δ interaction between the metals. In the former this destabilizes only σ* sufficiently to prevent occupation by electrons (leaving five orbitals for six electrons, possible spin multiplicities S=0, 1, 2) while for the latter both σ* and π* are destabilized beyond electron occupation (leaving four MOs for six electrons, possible spin multiplicities S=0, 1). 4*, 6* and 7* are unusual examples of metal - metal bonded complexes containing octahedral CrIII ions.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260313
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  • 7
    Electronic Resource
    Electronic Resource
    A Second Modification of Potassium Fluorenide and the Structure of Potassium 9-tert-Butylfluorenide: Effect of Crystallization Conditions and Substituents on Solid-State Contact Ion Pair Interactions (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 1603-1607 
    Details
    ISSN: 0009-2940
    Keywords: Potassium compounds ; Fluorenide, potassium salt ; Fluorenide, 9-tert-butyl, potassium salt ; Solid-state organization ; Polymorphism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Crystallization of potassium fluorenide or 9-tert-butylfluorenide [formed from potassium metal and fluorene or 9-tert-butylfluorene in tetramethylethylenediamine (tmeda)] from a mixture of tmeda, tetrahydrofuran (THF) and diethyl ether yields [K(tmeda)2][C13H9] (1) or {[K(THF)2][μ-C13H8(tBu)][K(tmeda)][μ-C13H8(tBu)]}∞ (2). Compound 1 is a monomeric solvated ion pair with one η5-coordinated fluorenyl and two chelating tmeda ligands and crystallizes in the monoclinic space group C2/c. Compound 1 is an example of polymorphism in organo-potassium compounds, as a polymeric structure of 1 obtained under slightly different crystallization conditions has been reported earlier. Compound 2 forms a polymeric chain with potassium coordinated to two anellated six-membered rings from two bridging 9-tert-butylfluorenyl systems and alternatingly solvated by one chelating tmeda or two THF. The crystal system for 2 is monoclinic, space group P21/c. A comparative AM1 study on the fluorenyl and 9-tert-butylfluorenyl anion suggests a steric origin for the haptotropic potassium shift in 2. 1H- and 13C-NMR data for 1 and 2 as well as for 9-tert-butylfluorene are reported.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260716
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  • 8
    Electronic Resource
    Electronic Resource
    Coronene-Potassium(THF)2(tmeda): X-Ray Structure and MNDO Calculations of a Half-Sandwich Contact Ion Pair as a Model for Potassium(Adsorbate)-Graphite Surface Interactions (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 1251-1253 
    Details
    ISSN: 0009-2940
    Keywords: Coronene(1-), radical anion ; Potassium compounds ; Graphite model studies ; Calculations, MNDO ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Crystallization of potassium(1+) and the radical ion coronene(1-) from a mixture of tetramethylethylenediamine (tmeda), tetrahydrofuran (THF), and diethyl ether yields a monomeric solvated ion pair 1 with potassium unsymmetrically π-coordinated to an external ring of the polyaromatic system according to an X-ray structure determination and in agreement with a MNDO theoretical investigation.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941270712
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  • 9
    Electronic Resource
    Electronic Resource
    Berichtigung zu dem Beitrag (1988)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 121 (1988), S. 1869-1869 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19881211029
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  • 10
    Electronic Resource
    Electronic Resource
    Transition-Metal Complexes with the Novel Poly (1,2,4-triazolyl)borate Ligands [HnB(C2H2N3)4 - n]- (n = 1 and 2): Synthesis and Characterization of Metal Complexes of Dihydrobis(1,2,4-triazolyl)borate as One- or Two-Dimensional Coordination Polymers with Six-Membered Ring Water Substructures and the Structure of Two-Dimensional Liquid and Solid Water As Organized in the Intercalate [Ni{HB(C2H2N3)3}2] · 6 H2O (X-ray Studies at 293 and 160 K)Dedicated to Prof. Dr. Hubert Schmidbaur on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 235-244 
    Details
    ISSN: 0009-2940
    Keywords: Poly(triazolyl)borates, metal complexes of ; Coordination polymers ; Water, cluster model ; Water, two-dimensional structure ; Hydrogen bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 1:2 manganese (5), nickel (6), and copper complex (7) with the novel dihydrobis(1,2,4-triazolyl)borate ligand (2) were synthesized and structurally characterized. Single-crystal X-ray studies reveal the formation of highly solvated coordination polymers of the formula {[M(H2O)2{μ-H2B(C2H2N3)2}2] · n H2O}∞ for M = Mn and Cu. In 5 (M = Mn; n = 4) a two-dimensional metal-ligand framework is built by means of the bridging action of 2. These metal-ligand grid sheets sandwich water layers which comprise individual six-membered rings. Compound 7 (M = Cu; n = 6) can be described as a linear metal-ligand chain with two borate ligands bridging two copper centers. These one-dimensional coordination polymers are separated by one-dimensional arrays of water molecules in the form of edge-sharing six-membered rings. In both structures the water of crystallization is held in place both by hydrogen bonding from the aqua ligands and by hydrogen bonding to the nitrogen atoms of the borate ligand. Bis[hydrotris(1,2,4-triazolyl)borato]nickel, [Ni{HB(C2H2N3)3}2] (8), was obtained from NiCl2 and the potassium salt of [HB(C2H2N3)3]- (1). Single-crystal X-ray structures of the solvate 8 · 6 H2O were determined at 293 and 160 K. The water molecules are arranged in two-dimensional layers with only weak (hydrogen bonding) interactions to the adjacent layers of the complex molecules. The room temperature structure (orthorhombic, space group Cmca) shows a highly disordered water structure being indicative of a dynamic equilibrium between small conglomerates and free molecules. Upon cooling an ordering occurs in the water layer leading to a phase transition in the crystal, and in the low-temperature structure at 160 K (orthorhombic, space group Pmnb) the hydrogen atoms and bonding network of the water structure could be determined. This structure is best described as being composed of individual rings or chain segments. The material surface morphology after loss of the water of crystallization was studied by scanning electron microscopy and the structural pattern correlated with the crystal packing.
    Additional Material: 12 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280306
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