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  • Chemistry  (9)
  • 2,2,3,3-tetracyano7,8-dithiabicyclo[3.2.1]octanes  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Synthesis of Pyrazinoporphyrazine Derivatives Functionalised with Tetrathiafulvalene (TTF) Units: X-Ray Crystal Structures of Two Related ttf Cyclophanes and Two Bis(1,3-Dithiole-2-Thione) IntermediatesDedicated to Professor Fabian Gerson on the occasion of his retirement (1997)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 3 (1997), S. 1679-1690 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; cyclophanes ; electrochemistry ; porphyrazines ; tetrathiafulvalenes ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The pyrazinoporphyrazine system 13 (metal-free, zinc and copper derivatives) has been synthesised by tetramerisation of 2,3-dicyanopyrazine monomer unit 10. The structure of 13a-c has been established by 1H NMR spectroscopy, UV/Vis spectrophotometry, MALDI-TOF mass spectrometry, cyclic voltammetry and differential pulse voltammetry. The electrochemical redox behaviour of 13a-c is strongly solvent dependent. The expected two-stage oxidation of the tetrathiafulvalene (TTF) units of 13a-c was observed in a range of solvents; in addition, oxidation and reduction of the pyrazinoporphyrazine core of the metal-free derivative 13a was detected in benzonitrile. On excitation of 13 in the Q-band region no fluorescence was observed, which is presumably the consequence of intramolecular charge transfer between the TTF moieties and the excited state of the central porphyrazine. Molecular modelling studies on 13a and 13c are reported. During the course of this work, the novel TTF macrocycles 11 and 20 were synthesised; their X-ray crystal structures reveal severely bent TTF units, the conformations of which are discussed in detail. The X-ray crystal structures of the bis(1,3-dithiole) systems 15 and 18 have also been determined.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chem.19970031018
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  • 2
    Electronic Resource
    Electronic Resource
    Dichotomy in the reaction between cinnamyl dithiocarboxylates and tetracyanoethylene with the formation of 7,8-dithiabicyclo[3.2.1]octanes and dithioacyloxycyclopentanes (1995)
    Springer
    Russian chemical bulletin 44 (1995), S. 1735-1739 
    Details
    ISSN: 1573-9171
    Keywords: cinnamyl dithiocarboxylates ; tetracyanoethylene ; 2,2,3,3-tetracyano7,8-dithiabicyclo[3.2.1]octanes ; 3,3,4,4-tetracyano-1-dithioacyloxycyclopentanes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The reaction of cinnamyl dithiocarboxylates (1) containing electron-donating substituents at the central carbon atom of the dithioester group (R = p-MeOC6H4, EtO, andp-Tol) with tetracyanoethylene affords 2,2,3,3-tetracyano-4-endo-phenyl-7,8-dithiabicyclo[3.2.1]octanes (2) as well as isomeric 3,3,4,4-tetracyano-2-phenyl-trans-1-dithioacyloxycyclopentanes (3). Dithiabicyclooctanes2 rearrange to the corresponding cyclopentanes3 upon thermolysis.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01151301
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  • 3
    Electronic Resource
    Electronic Resource
    Syntheses and X-ray Crystal Structures of Functionalised 9,10-Bis(1,3-dithiol-2-ylidene)-9,10-dihydroanthracene Derivatives (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 51-60 
    Details
    ISSN: 1434-193X
    Keywords: Dithioles ; Anthracenes ; Lithiation ; Electron donors ; Crystal structures ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The synthesis of new derivatives of 9,10-bis(1,3-dithiol-2-ylidene)-9,10-dihydroanthracene has been achieved by two different routes. Deprotonation of 8 using LDA in THF at -78 °C, followed by in situ quenching of the lithiated intermediate 9 with N,N-dimethylformamide, N-methyl isothiocyanate and methyl chloroformate gave aldehyde, thioamide and methyl ester derivatives 10-12, respectively. Sulfur insertion into the lithiated species 9 followed by reaction of the transient thiolate anion with benzoyl chloride gave the thioester derivative 13 which served as a convenient shelf-stable precursor of other mono-functionalised derivatives of 8. Debenzoylation of 13 and trapping of the transient thiolate anion with iodomethane and 6-bromohexan-1-ol yielded 14 and 15, respectively. Reaction of cation salt 17 with the anion of anthrone 18 gave compound 20, the thiolate anion of which reacted with 6-bromohexan-1-ol to afford the alcohol derivative 21. Subsequent reactions gave alcohol derivative 25 of the title system. The unexpected product 29 was obtained from reaction of 28 with triethyl phosphite. The X-ray crystal structures of compounds 12, 14, 28, and 29 are reported. The molecules adopt a saddle-like conformation; the bis(1,3-dithiole)benzoquinone system is U-shaped through an ‘accumulating bend’ comprising the boat conformation of the central (quinonoid) ring, folding of both 1,3-dithiole rings along S···S vectors, and out-of-plane tilting of the exocyclic C=C bonds, all in the same (inward) direction.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    2,6-Dialkoxy-9,10-bis(1,3-dithiol-2-ylidene)-9,10-dihydroanthracene Derivatives: Synthesis, Electrochemistry and X-ray Crystal Structures of Neutral and Dication Species (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1199-1205 
    Details
    ISSN: 1434-193X
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: -The synthesis of 2,6-dialkoxy-9,10-bis(1,3-dithiol-2-ylidene)-9,10-dihydroanthracene derivatives 15 and 16 is described. Solution electrochemistry shows that 15 and 16 display three redox waves, representing the sequential formation of the dication, radical trication and tetracation species in an EqEqEq process. The X-ray crystal structures of neutral compounds 15 and 16 and the charge transfer complex (15)2+(TCNQ-•)2· 2MeCN are reported. The neutral molecules adopt a saddle-like conformation; the bis(1,3-dithiole)benzoquinone system is U-shaped through an ‘accumulating bend’ comprising the boat conformation of the central (quinonoid) ring and folding of both 1,3-dithiole rings. In the complex (15)2+(TCNQ-•)2· 2MeCN the anthracene system is planar and aromatic; the dithiolium cations form a dihedral angle of 78° with the anthracene plane. The TCNQ anion radicals form a stack of dimers with interplanar separations of 3.15 Å within a dimer and 3.50 Å between the dimers. The structure contains unusually short intermolecular S···N contacts [2.865(3) Å].
    Additional Material: 5 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Synthese und Röntgenstrukturanalyse von Tris(diethyldithiocarbamato) dimethylphenylphosphantechnetium(III), einem Technetium-Komplex mit der Koordinationszahl 7 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 117-122 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal and Molecular Structure of Tris(diethyldithiocarbamato)dimethylphenylphosphinetechnetium (III)The title compound Tc(S2CNEt2)3(Me2PhP) I has been prepared by the reaction of TcCl3(Me2PhP)3 with NaS2CNEt2. The crystal structure of I has been determined by single-crystal X-ray diffraction methods at room temperature. Crystals are rhombic, space group P212121, with a = 8.708(1), b = 12.012(1), c = 29.626(3) Å and Z = 4. The compound consists of discrete I molecules. The technetium atom has a seven-coordinated environment which is best described as a distorted pentagonal bipyramid. The Tc - P distance (2.330(3) Å) is remarkably short compared with other technetium complexes with mono-dentate phosphine ligands.
    Notes: Die Titelverbindung Tc(S2CNEt2)3(Me2PhP) I wurde durch Reaktion von TcCl3(Me2PhP)3 mit NaS2CNEt2 dargestellt und ihre Kristall- und Molekülstruktur durch Röntgenstrukturanalyse ermittelt. Die Kristalle sind rhombisch, Raumgruppe P212121, mit a = 8,708(1), b = 12,012(1), c = 29,626(3) Å und Z = 4. Die Verbindung besteht aus diskreten monomeren Molekülen. Das Technetiumatom hat siebenfache Koordination, die am besten als geringfügig verzerrte pentagonale Bipyramide beschrieben werden kann. Die Tc - P-Bindungslänge (2,330(3) Å) ist bemerkenswert kurz im Vergleich zu anderen Technetiumkomplexverbindungen mit einzähnigen Phosphanen.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845100317
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  • 6
    Electronic Resource
    Electronic Resource
    Röntgenstrukturanalyse von 15N-Nitridodichlorotris(dimethylphenylphenylphosphin)technetium(V) (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 129-134 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of 15N-Nitridodichlorotris(dimethylphenylphenylphosphine)technetium(V)The title compound Tc15NCl2(Me2PhP)3 I has been prepared by the reaction of mer-TcCl3(Me2PhP)3 with Na15N3. The crystal structure of I has been determined by single crystal X-ray diffraction methods at room temperature. Crystals are orthorhombic, space group Pbca, with a = 16.663(1), b = 19.219(1), c = 16.769(1) Å and Z = 8. The technetium atom is six-coor-dinate. The coordination geometry is that of a distorted octahedron with 3 phosphine ligands in meridional positions. The strong trans influence of the nitrido ligand has been noted. The Tc—Cl length trans to N is 2.665(1) Å while those trans to P is 2.441(1) Å.
    Notes: Die Titelverbindung Tc15NCl2(Me2PhP)3 I wurde durch Reaktion von mer-TcCl3(Me2PhP)3 mit Na15N3 dargestellt und ihre Kristall- und Molekülstruktur durch Röntgenstrukturanalyse ermittelt. Die Kristalle sind orthorhombisch, Raumgruppe Pbca, mit a = 16,663(1), b = 19,219(1), c = 16,769(1) Å und Z = 8. Das Technetiumatom hat verzerrt oktaedrische Koordinationsgeometrie mit meridionaler Anordnung der Phosphine. Infolge des ausgeprägten trans-Effektes des Nitridoliganden ist der Tc—Cl-Bindungsabstand in trans-Stellung zum Nitridoliganden um 0,22 Å größer als jener, der sich in trans-Stellung zum Phosphinliganden befindet.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885640118
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  • 7
    Electronic Resource
    Electronic Resource
    On the Kinetics of Chemical Reactions in Solids Under Shock Compression (a review) (1993)
    Weinheim : Wiley-Blackwell
    Propellants, Explosives, Pyrotechnics 18 (1993), S. 100-105 
    Details
    ISSN: 0721-3115
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Consideration is given to physical and chemical methods useful for a proceeding time of chemical reactions under compression due to impact and, also, to diffusion-process peculiarities. Experimental data enable us to conclude that solid-phase reactions may be accomplished for times of the order 1-10 μs. The mechanism governing enhanced diffusion rate at the moment of impact has been proposed and experimentally confirmed.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prep.19930180210
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  • 8
    Electronic Resource
    Electronic Resource
    On the Nature of Boron Nitride E-Phase (1993)
    Weinheim : Wiley-Blackwell
    Propellants, Explosives, Pyrotechnics 18 (1993), S. 352-355 
    Details
    ISSN: 0721-3115
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A review of the works, in which the E-phase of boron nitride had been obtained under various physical treatments, revealed that in all cases during the formation or isolation of the E-phase the sample can be impurified with oxygen. An X-ray spectral study of crystalline E-phase obtained in the present work proved it to be a solid solution of the type BN1 - xOx containing B-B bonds.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prep.19930180608
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  • 9
    Electronic Resource
    Electronic Resource
    Effect of High Dynamic Pressure on the Structure of Solids (1987)
    Weinheim : Wiley-Blackwell
    Propellants, Explosives, Pyrotechnics 12 (1987), S. 206-208 
    Details
    ISSN: 0721-3115
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The influence of shock waves on crystal macrostructure and its physical and technological consequences are discussed. The size of crystal particles grain corresponding to the transition of solid into amorphous state is estimated. The magnitudes of microstrains in crystals during their grinding are calculated. It is shown that under shock-wave treatment the grain size and microstrain are usually about 10 times differed from the values in amorphous substances. The possibility of amorphization during chemical interaction under shock compression is shown. Phase transformations with change of stoichiometry under shock waves prove a perspective synthetic method.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prep.19870120606
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  • 10
    Electronic Resource
    Electronic Resource
    Effect of shock-thermal treatment on mechanical properties of steels (1989)
    Weinheim : Wiley-Blackwell
    Propellants, Explosives, Pyrotechnics 14 (1989), S. 238-240 
    Details
    ISSN: 0721-3115
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The shock-treatment permit to achieve high mechanical characteristics of steels. The interpretation of this effect is based on the possibility to change the carbon solubility in iron under these conditions. Measurements of the quality factors (internal friction in power-1) confirm this assumption.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prep.19890140604
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