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  • 1
    Electronic Resource
    Electronic Resource
    Trithiooxalat als variabler Brückenligand - Kristall- und Molekülstruktur von μ-Trithiooxalato-bis[bis(triphenylphosphan)kupfer(I)]Professor Eberhard Hoyer zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1236-1240 
    Details
    ISSN: 0044-2313
    Keywords: Trithiooxalate ; Dinuclear Complex ; Copper(I) ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trithiooxalate as Varying Bridging Ligand - Crystal and Molecular Structure of μ-Trithiooxalato-bis[bis(triphenylphosphane)copper(I)]Due to its design, trithiooxalat (trto) as a multidentate, chalcogen-rich ligand allows different coordination possibilities. In contrast to the corresponding dinuclear silver complex [(Ph3P)2Ag]2(trto), which is side-on(S,S′)/end-on(S′,S″) coordinated, the title complex is exclusively side-on (S,S′ and S″,O) coordinated involving the oxygen donor atom. [(Ph3P)2Cu]2(trto) crystallizes in the triclinic space group P1 (No. 2) with a = 10.195(2), b = 13.090(3), c = 13.450(3) Å, α = 116.10(2)º, β = 90.10(2)º, γ = 101.49(2)º, and Z = 1. The bridging ligand with its nonsymmetrical donor atom set is disordered around the centre of symmetry (inversion centre).
    Notes: Trithiooxalat (trto) bietet als vielzähniger, chalkogenreicher Ligand aufgrund seiner Struktur und seines Donoratomsatzes vielfältige Koordinationsmöglichkeiten. Im Gegensatz zum entsprechenden Silber-Zweikernkomplex [(Ph3P)2Ag]2(trto), der simultan side-on(S,S′)/end-on(S′,S″) koordiniert, liegt im Titelkomplex ausschließlich side-on(S,S′ bzw. S″,O) Koordination unter Einbeziehung des Sauerstoff Donoratoms vor. [(Ph3P)2Cu]2(trto) kristallisiert in der triklinen Raumgruppe P1 (No. 2) mit a = 10,195(2) Å, b = 13,090(3) Å, c = 13,450(3) Å, α = 116,10(2)º, β = 90,10(2)º, γ = 101,49(2)º und Z = 1. Der bezüglich seines. Donoratomsatzes unsymmetrische Brückenligand ist um das Symmetriezentrum (Inversionszentrum) fehlgeordnet.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220722
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  • 2
    Electronic Resource
    Electronic Resource
    Photolysereaktionen an Thiooxalat-Zweikernkomplexen - Kristall- und Molekülstruktur von Hydrogensulfidopyridinbis(triphenylphosphan)kupfer(I)Professor Lothar Beyer zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 129-134 
    Details
    ISSN: 0044-2313
    Keywords: Tetrathiooxalate ; Trithiooxalate ; 1,1-Dithiooxalate ; Photolytic Reactions ; Moleculer Structure ; Copper(I) Complexes ; Extended Hückel Calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Photolytic Reactions of Binuclear Thiooxalate Complexes - Crystal and Moleculer Structure of Hydrogensulfidopyridinebis(triphenylphosphane)copper(I)Solutions of the binuclear, thiooxalato bridged complexes with capping triphenylphosphane ligands are lightsensitive and decompose mainly with decomposition of the bridging thiooxalate. From μ-1,1-Dithiooxalatobis[bis(triphenylphosphane)copper(I)], [{(Ph3P)2Cu}2(i-dto)], in dichloromethane the binuclear copper(I) complex μ-dichlorotris(triphenylphosphane)dicopper(I), [(Ph3P)2CuCl2Cu(Ph3P)], with the total lost of the bridging thiooxalato ligand is formed. μ-Trithiooxalato-bis-[bis(triphenylphosphane)copper(I)], [{(Ph3P)2Cu}2(trto)], decomposes in pyridine with the formation of hydrogensulfidopyridinebis(triphenylphosphane)copper(I), [(Ph3P)2(py)CuSH]. This complex crystallizes in the triclinic space group P1, with the unit cell parameters a = 9,488(2) Å, b = 10,472(3) Å, c = 19,351(3) Å, α = 85,03(2)°, β = 86,99(2)° and γ = 68,36(2)°. Contrast ngly, the bridging thiooxalate ligand in the corresponding binuclear tetrathiooxalate complex, [{(Ph3P)2Cu}2(tto)], obviously remains unchanged. The proposed reaction pathways are supported by the results of Extended Hückel Calculations.
    Notes: Die Lösungen thiooxalatverbrückter Zweikernkomplexe mit terminalen Triphenylphosphanliganden sind lichtempfindlich und zersetzen sich überwiegend unter Zerfall des Thiooxalato-Brückenliganden. μ-1,1-Dithiooxala-to-bis[bis(triphenylphosphan)-kupfer(I)], [{(Ph3P)2Cu}2(i-dto)], bildet in Dichlormethan unter Verlust des Thiooxalato-Brückenliganden den chloroverbrückten Kupfer(I)-Zweikernkomplex μ-Dichlorotris(triphenylphosphan)dikupfer(I), [(Ph3P)2CuCl2Cu(Ph3P)]. μ-Trithiooxalato-bis[bis(triphenyl-phosphan)kupfer(I)], [{(Ph3P)2Cu}2(trto)], zersetzt sich in Pyridin unter Bildung von Hydrogensulfidopyridin-bis(triphenylphosphan)kupfer(I), [(Ph3P)2 (py)CuSH]. Der gebildete Komplex kristallisiert in der triklinen Raumgrupe P1, mit dem Elementarzellenparametern a = 9,488(2) Å, b = 10,472(3) Å, c = 19,351 (3) Å, α = 85,03(2)°, β = 86,99(2)° und γ = 68,36(2)°. Im Unterschied dazu bleibt beim entsprechenden Tetrathiooxalat-Zweikernkomplex, [{(Ph3P)2Cu}2(tto)], der Thiooxalato-Brückenligand offensichtlich erhalten. Die angenommenen Reaktionswege konnten durch quantenchemische Berechnungen (EHT) gestützt werden.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230121
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  • 3
    Electronic Resource
    Electronic Resource
    Metallchelate ungesättigter geminaler Dichalcogenoliganden mit gemischten S,Se-Ligatoren Kristall- und Molekülstruktur von Tetra-n-butylammonium-bis(1,1-dicyanoethylen-2,2-thioselenolato)nickelat(II), [(n-C4H9)4N]2[Ni(SSeC—C(CN)2)2] (1981)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 477 (1981), S. 71-84 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal Chelates of Unsaturated Geminal Dichalcogeno Ligands Containing S as well as Se Ligators. Crystal and Molecular Structure of Tetra-n-butylammonium-bis(1,1-dicyanoethylene-2,2-thioselenolato)nickelate(II), [(n-C4H9)4N]2[Ni(SSeC—C(CN)2)2]Synthesis and properties of chelates of the thioseleno ligands 1,1-dicyanoethylene-2,2-thioselenolate (bis-chelates with Ni2+, Pd2+, Pt2+, Cu2+, Au3+, Zn2+, Cd2+, Se2+, Te2+, UO22+; tris-chelate mit Cr3+, Fe3+, Co3+, Rh3+, In3+; 1:1-chelate mit Cu+, Au+), cyanthioselenocarbimate (bis-chelates with Ni2+, Pd2+) and 0-β-methoxyethyl-thioselenocarbonate (bis-chelates with Ni2+, Pd2+, Pt2+, Zn2+; tris-chelate mit Cr3+, Co3+, Rh3+) are reported. The X-ray crystal structure of [(n-C4H9)4N]2[Ni(SSeC—C(CN)2)2] shows a planar NiS2Se2 arrangement. From the space group P21/c (a = 14,043(1) Å, b = 8.704(1) Å, c = 20.647(2) Å, β = 108.56(1)°) and Z = 2 follows a trans position of the thioseleno ligands. The same magnitude of the C-S and C-Se distance refers to a hindrance of the equalization of the bonding in the chelate. The structure is compared with those of similar compounds.
    Notes: Synthese und Eigenschaften von Chelaten mit den Thioselenoliganden 1,1-Dicyanoethylen-2,2-thioselenolat (Bis-Chelate mit Ni2+, Pd2+, Pt2+, Cu2+, Au3+, Zn2+, Cd2+, Se2+, Te2+, UO22+; Tris-Chelate mit Cr3+, Fe3+, Co3+, Rh3+, In3+; 1:1-Chelate mit Cu+, Au+), Cyanthioselenocarbimat (Bis-Chelate mit Ni2+, Pd2+) und O-β-Methoxyethyl-thioselenocarbonat (Bis-Chelate mit Ni2+, Pd2+, Pt2+, Zn2+; Tris-Chelate mit Cr3+, Co3+, Rh3+) werden berichtet. Die Röntgenkristallstrukturanalyse der Verbindung [(n-C4H9)4N]2[Ni(SSeC—C(CN)2)2] zeigt eine planare NiS2Se2-Anordnung. Aus der Raumgruppe P21/c (a = 14,043(1) Å, b = 8,704(1) Å, c = 20,647(2) Å, β = 108,56(1)°) und Z = 2 folgt eine trans-Stellung der beiden Thioselenoliganden. Die gleiche Größe des C-S- und C-Se-Abstandes weist auf eine Behinderung des Bindungsausgleichs im Chelat hin. Die Struktur wird mit der ähnlicher Metallchelate verglichen.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19814770608
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  • 4
    Electronic Resource
    Electronic Resource
    Kristall- und Molekülstruktur von Bis(N, N-diethyl-2-benzoylthioacetamidato)kupfer(II) (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 513 (1984), S. 114-122 
    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 Bis(N, N-diethyl-2-benzoylthioacetamidato)copper(II)Bis(N, N-diethyl-2-benzoyl-thioacetamidato)copper(II) has been investigated by X-ray structure analysis. It crystallizes in the triclinic space group P1 with a = 10.709, b = 12.150, c = 15.651 Å, α = 90.13, β = 103.73, γ = 98.30° and with 3 formula units per unit cell. The structure was solved by heavy atom technique. The final R value was 0.04 for 4151 symmetry independent reflections. The crystal contains two symmetry independent molecules. One of them shows a nearly planar cis-arrangement of the ligator atoms but the other has an exactly planar trans-arrangement. The chelate rings show a distorted planarity in both molecules. The results of the structure determination confirm the conclusions from the EPR crystal spectrum.
    Notes: Bis(N, N-diethyl-2-benzoyl-thioacetamidato)kupfer(II) wurde mittels Röntgenkristallstrukturanalysc untersucht. Es kristallisiert triklin in der Raumgruppe P1 mit den Gitterkonstanten a = 10,709, b = 12,150, c = 15,651 Å, α = 90,13, β = 103,73, γ = 98,30° und 3 Formeleinheiten pro Elementarzelle. Die Lösung der Struktur erfolgte mittels der Schweratommethode. Der abschließende R-Wert betrug R = 0,04 für 4151 symmetrieunabhängige Reflexe. Der Kristall enthält zwei symmetrieunabhängige Moleküle, von denen eines eine nahezu planare cis-Anordnung der Ligatoren, aufweist, während des andere eine exakt planare trans-Anordnung hat. Die Chelatringe zeigen in beiden Molekülen eine gestörte Planarität. Die Ergebnisse der Strukturbestimmung bestätigen die Vermutungen aus dem EPR-Kristallspektrum.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845130612
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  • 5
    Electronic Resource
    Electronic Resource
    Zur Struktur von N-Benzoylthiobenzamid (1983)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 498 (1983), S. 139-152 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure of N-BenzoylthiobenzamideN-Benzoylthiobenzamide forms two polymorphic modifications of which the crystal and molecular structures have been determined by X-ray structure analysis. In both modifications the molecules exist as NH tautomeres, but there are differences with regard to their rotameric configurations. In the monoclinic modification both symmetry independent molecules have a Z,Z′ configuration. The triclinic modification also contains two symmetry independent molecules, but now a Z,Z′ and an E,Z′ configuration exist. All four molecules deviate appreciably from planarity. The results of both structure determinations are compared with each other and with the structure of monothiodibenzoylmethane.
    Notes: N-Benzoylthiobenzamid bildet zwei polymorphe Modifikationen, deren Kristall- und Molekülstrukturen mittels Röntgenkristallstrukturanalyse ermittelt wurden. In beiden Formen liegen die Moleküle als NH-Tautomere vor. Unterschiede bestehen hinsichtlich der rotameren Konfigurationsverhältnisse. In der monoklinen Modifikation liegen beide symmetrieunabhängigen Moleküle in einer Z,Z′-Konfiguration vor. In der triklinen Modifikation, die ebenfalls zwei symmetrie-unabhängige Moleküle enthält, sind sowohl eine Z,Z′- als auch eine E,Z′-Konfiguration realisiert. Alle Moleküle weichen stark von der Planarität ab. Die Ergebnisse der beiden Strukturbestimmungen werden miteinander und mit der des Monothiodibenzoylmethans verglichen.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19834980319
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  • 6
    Electronic Resource
    Electronic Resource
    Kristall- und Molekülstruktur eines neuartigen Dimetallamacrocyclus: cyclo-Di[quecksilber-μ-[1,1,1′,1′-tetraethyl-3,3′-terephthaloyl-bis-thioureato(2-)-S:S′]] (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 578 (1989), S. 198-204 
    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 a Novel Dimetallamacrocycle: cyclo-Di[mercury-μ-[1,1,1′,1′-tetraethyl-3,3′-terephthaloyl-bis-thioureato(2-)-S:S′]]The structure of the title compound has been determined by an X-ray structure analysis. The compound crystallizes in the monoclinic space group P21/n with a = 13.437, b = 9.270, c = 18.791 Å, β = 100.65° and Z = 2. The solution of the structure was performed by Patterson methods. The final R value was R = 0.090 for 3089 observed reflections. The molecule has a cyclic structure consisting of two molecules of the ligand which coordinate only by the sulphur atoms and two mercury atoms. The formed ring is a 26-membered dimetallamacrocycle. The intramolecular Hg-Hg distance is 10.39 Å. The molecule has the symmetry Ci.
    Notes: Die Struktur der Titelverbindung wurde durch Röntgenkristallstruktur-analyse bestimmt. Die Verbindung kristallisiert monoklin in der Raumgruppe P21/n mit den Gitterkonstanten a = 13,437, b = 9,270, c = 18,791 Å, β = 100,65° und Z = 2. Gelöst wurde die Struktur mittels Patterson-Methoden. Der abschließende R-Wert betrug R = 0,090 für 3089 beobachtete Reflexe. Das Molekül besitzt eine zyklische Struktur, die sich aus zwei Molekülen des nur über die Schwefel-Atome koordinierenden Liganden und zwei Quecksilber-Atomen zusammensetzt. Der gebildete Ring ist ein 26gliedriger Dimetallamacrocyclus. Der intramolekulare Hg-Hg-Abstand beträgt 10,39 Å. Das Molekül besitzt die Symmetrie Ci.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895780123
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  • 7
    Electronic Resource
    Electronic Resource
    Synthesis of trans,trans-[MoX2py4][MoX4py2], trans-[MoX2py4]Br3, and structural identification of trans, trans-[MoX2py4][MoX4py2] (X = Cl, Br; py = pyridine) (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 2124-2128 
    Details
    ISSN: 0044-2313
    Keywords: molybdenum(III) chloro and bromo pyridine complexes ; preparation ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung von trans, trans-[MoX2py4][MoX4py2], trans-[MoX2py4]Br3 und Struktur von trans, trans-[MoX2py4][MoX4py2] (X = Cl, Br; py = Pyridin)Trans,trans-[MoX2py4][MoX4py2] (A: X = Cl; B: X = Br; py = Pyridin, C5H5N) sind die Nebenprodukte der Reaktion zwischen (NH4)2[MoX5 · H2O] (X = Cl, Br) und mit Methanol verdünntem Pyridin. Beide Verbindungen kristallisieren monoclin, P21/n mit Z = 2 und A: a = 12.568(1), b = 9.430(1), c = 14.952(1) Å und β = 100.81(1)°; B: a = 12.551(2), b = 9.533(2), c = 15.366(2) (Å) und β = 99.35(1)°.Die Kationen und Anionen sind Symmetriezentren. Die Ebenen der trans zueinander angeordneten Pyridin-Moleküle sind planparallel. Mittlere Mo—X- und Mo—N(Pyridin)-Abstände sind: (Kation) 2.41, 2.21 Å (A); 2.54, 2.21 Å (B); (Anion) 2.44, 2.20 Å (A); 2.58, 2.20 Å (B).Der anionische Teil kann mit Brom zu trans-MoX4py2 oxydiert werden. Gleichzeitig sind Kationen als trans-[MoX2py4]Br3 isolierbar.Die Verbindungen wurden auch durch die chemische Analyse, Infrarot-Spektroskopie und Konduktometrie charakterisiert.
    Notes: Trans,trans-[MoX2py4][MoX4py2] (X = Cl, A; Br, B; py = pyridine, C5H5N) are the side products of reaction of between (NH4)2[MoX5 · H2O] (X = Cl,Br) with pyridine diluted with methanol.Both trans,trans-[MoX2py4][MoX4py2] are monoclinic, P21/n space group, with z = 2 and: a = 12.568(1), b = 9.430(1), c = 14.952(1) Å and β = 100.81(1)° (A); a = 12.551(2), b = 9.533(2), c = 15.366(2) (Å) and β = 99.35(1) (B).Cations and anions are located on the symmetry centers and have eclipsed conformation of the trans located pyridine ligands. Average Mo—X and Mo—N (pyridine) bonds are; (cation) 2.41, 2.21 Å (A); 2.54, 2.21 Å (B); (anion) 2.44, 2.20 Å (A); 2.58, 2.20 Å (B).Anionic part of the compounds can be oxidised by bromine to trans-MoX4py2, which precipitates from the solution. Cation can be isolated from the solution in the form of trans-[MoX2py4]Br3 (X = Cl, Br).The compounds were also characterised by chemical analysis, infrared spectroscopy and conductivity measurements.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966221222
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