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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Monatshefte für Chemie 127 (1996), S. 291-296 
    ISSN: 1434-4475
    Keywords: S-(N-(Thiocarbamoyl)benzimido)dithiocarbamic esters ; Synthesis ; 13C NMR spectroscopy ; Side reactions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The synthesis of the title compounds3 (R 1=R 2=C2H5;n-C4H9) by reactions of N-(N′,N′-diethylthiocarbamoyl)benzimidechloride (2) with sodiumdialkyldithiocarbamates (1) in acetone is described. The low yields (〈25%) are caused by the occurrence of side reactions. The structures of the compounds were confirmed by IR,1H and13C NMR, and mass spectroscopy. Side reactions were detected by13C NMR spectroscopy; the results are discussed.
    Notes: Zusammenfassung Die Synthese der Titelverbindungen3 (R 1=R 2=C2H5;n-C4H9) durch Reaktionen von N-(N′,N′-Diethylthiocarbamoyl)-benzimidoylchlorid (2) mit Natriumdialkyldithiocarbamaten (1) in Aceton wird beschrieben. Die niedrigen Ausbeuten (bis 25% d.Th.) sind durch Nebenreaktionen bedingt. Die Strukturen der Verbindungen werden durch IR-,1H-NMR-,13C-NMR-und Massenspektren bestätigt. Nebenreaktionen werden13C-NMR-spektroskopisch verfolgt und die Ergebnisse diskutiert.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1434-4475
    Keywords: 1,4-bis(pyrrol-1-yl-carbonyl)benzene ; Synthesis ; Molecular structure ; Cyclovoltammetry ; NK XANES
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The molecular structure and the cyclovoltammetric behaviour of 1,4-bis(pyrrol-1-yl-carbonyl)benzene (1) are described. The X-ray absorption spectrum of1 (NK XANES) is investigated with respect to the N1s → π* transitions in comparison with 1H-pyrrole.
    Notes: Zusammenfassung Die Molekülstruktur und das cyclovoltammetrische Verhalten von 1,4-Bis-(pyrrol-1-yl-carbonyl)benzol (1) werden beschrieben. Das Röntgenabsorptionsspektrum von1 (NK XANES) wird bezüglich der N1s → π*-Übergänge im Vergleich mit 1H-Pyrrol untersucht.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dithiazolium Salts of Halometalates - Synthesis and Structure of 3-Diethylamino-5-phenyl-1,2,4-dithiazolium-tetrachloroniccolate (II)Chlorination of NiII-coordinated 1,1-diethyl-3-benzoyl-thiourea by SOCl2 in acetonitrile yields turquoise 3-diethyl-amino-5-phenyl-1,2,4-dithiazolium-tetrachloroniccolate. Its reduction produces cis-bis-(1,1-diethyl-3-thiobenzoylthioureato)nickel(II). The mechanism of formation as well as the crystal and molecular structure of the title compound are presented.
    Notes: Die Chlorierung von an NiII innerkomplex gebundenem 1,1-Diethyl-3-benzoylthioharnstoff mittels SOCl2 führt in Acetonitril zu türkisem 3-Diethylamino-5-phenyl-1,2,4-dithiazolium-tetrachloroniccolat, aus dem durch Reduktion cis-Bis-(1,1-diethyl-3-thiobenzoyl-thioureato)nickel(II) zugänglich ist. Der Bildungsmechanismus des Dithiazoliumsalzes wird erörtert und die Kristall- und Molekülstrukturanalyse vorgestellt.
    Additional Material: 6 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 580 (1990), S. 167-174 
    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 Tris(1,1-diethyl-3-benzoyl-thioureato)ruthenium(III)The crystal and molecular structure of tris(1,1-diethyl-3-benzoyl-thioureato)-ruthenium(III) has been determined by an X-ray structure analysis. The compound crystallizes in the trigonal space group P3 with a = 16.556, c = 8.476 Å and Z = 2. The structure was solved by Patterson methods and refined to a final R value R = 0.074 for 801 observed reflections. The molecule has the symmetry C3. The coordination polyhedron is an octahedron with facial arrangement of the ligator atoms. The Ru—S and Ru—O distances are 2.293 Å and 2.047 Å, respectively.
    Notes: Die Kristall- und Molekülstruktur von Tris(1,1-diethyl-3-benzoyl-thioureato)ruthenium(III) wurde durch Röntgenkristallstrukturanalyse bestimmt. Die Verbindung kristallisiert trigonal in der Raumgruppe P3 mit den Gitterkonstanten a = 16,556, c = 8,476 Å und Z = 2. Die Struktur wurde mittels Patterson-Methoden gelöst und bis zu einem abschließenden R-Wert R = 0,074 für 801 beobachtete Reflexe verfeinert. Das Molekül besitzt die Symmetrie C3. Das Koordinationspolyeder ist ein Oktaeder mit facialer Anordnung der Ligator-Atome. Die Ru—S- und Ru—O-Abstände betragen 2,293 Å bzw. 2,047 Å.
    Additional Material: 3 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 586 (1990), S. 79-86 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Bis(3-diethylamino-5-phenyl-1,2,4-dithiazolium)-tetrachlorocobaltat(II)The title compound 1 was prepared by reaction of Tris(1,1-diethyl-3-benzoyl-thioureato)cobalt(III) with SOCl2 in acetonitrile. 1 has been characterized by IR-spectroscopy and VIS-spectroscopy.The structure of 1 has been determined by an X-ray structure analysis. The compound crystallizes in the monoclin space group C2/c with a = 16.224; b = 11.257; c = 17.697 Å; β = 107,43° and Z = 4. The final R value was R = 0.027 for 2073 observed reflections.The cation of 1 is nearly plane with an extended delocalization of electrons. The CoCl42- anion is tetrahedral with two different long Co—Cl pairs. Interionic contacts S … Cl exists between the structural units of the cations and the anion.
    Notes: Die Darstellung der Titelverbindung 1 erfolgt aus Tris(1,1-diethyl-3-benzoyl-thioureato)-cobalt(III) mit SOCl2 in Acetonitril. 1 wird IR-spektroskopisch und durch VIS-Spektren charakterisiert.Die Struktur von 1 wurde durch Röntgenkristallstrukturanalyse bestimmt. Die Verbindung kristallisiert monoklin in der Raumgruppe C2/c mit den Gitterkonstanten a = 16,224; b = 11,257; c = 17,697 Å, β = 107,43° und Z = 4. Der abschließende R-Wert betrug R = 0,027 für 2073 beobachtete Reflexe.Das Kation von 1 ist nahezu planar und weist eine weitreichende Elektronendelokalisierung auf. Das CoCl42--Anion ist tetraedrisch strukturiert und besitzt zwei unterschiedlich lange Co—Cl-Paare. Zwischen Kation- und Anion-Struktureinheiten bestehen über S und Cl interionische Wechselwirkungen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cis-Trans Isomerism in N-Thioacyl Thiourea Chelates: The Structure of cis-Bis(l,l-diethyl-3-thiobenzoyl-thioureato)nickel(II)In addition to two crystalline modifications in which the ligands are arranged in trans position, bis(1,1-diethyl-3-thiobenzoyl-thioureato)nickel(II) forms a further modification with cis position of the ligands whose structure has been confirmed by an X-ray structure analysis. It crystallizes in the space group P21/c with a=11.316, b=17.981, c=14.331 Å,β=111.85° and Z=4. The coordination is slightly tetrahedrally distorted. Bond lengths and angles are in good agreement with those of the trans modifications. The average Ni—S bond length is 2.167 Å.
    Notes: Bis(1,1-diethyl-3-thiobenzoyl-thioureato)nickel(II) bildet neben zwei kristallinen Modifikationen, in denen die Liganden in trans-Stellung am Nickel-Atom angeordnet sind, auch eine Modifikation mit cis-Stellung der Liganden, deren Struktur mittels Röntgenstrukturanalyse bestätigt wird. Sie kristallisiert in der Raumgruppe P21/c mit den Gitterkonstanten a=11,316, b=17,981, c=14,331 Å,β=111,85° und Z=4. Die Koordination ist leicht tetraedrisch verzerrt. Bindungslängen und-winkel stimmen gut mit denen der trans-Modifikationen überein. Die mittlere Ni—S-Bindungslänge beträgt 2,167 Å.
    Additional Material: 2 Ill.
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  • 7
    ISSN: 0044-2313
    Keywords: Nickel(II) chelates ; syntheses ; crystal structures ; FAB mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Di- and Trinuclear Nickel(II) Chelates of Bis-bidentate N-AcylselenoureasBis-bidentate isophthaloyl-bis(selenoureas) form with nickel(II) ions under deprotonating conditions macrocyclic dinuclear metal chelates. This was confirmed by X-ray crystal structure analysis of the cyclo-di[nickel-μ-[1,1,1′,1′-tetraisobutyl-3,3′-iso-phthaloyl-bis-selenoureato(2-)Se,O:O′, Se′]], 2. The compound 2 crystallizes in the monoclinic space group P 21/c with a = 11.673 (1); b = 19.834 (2); c = 13.606 (1) Å; β = 107.45 (1)° and Z = 2. The final R value was R = 0.081 for 3049 observed reflections.Bis-bidentate terephthaloyl-bis(selenoureas) give under the same conditions macrocyclic trinuclear nickel(II) chelates.Both types of the complexes are characterized by FAB mass spectra.
    Notes: Bis-bidentate Isophthaloyl-bis(selenoharnstoffe) bilden mit Nickel(II)-Ionen unter deprotonierenden Bedingungen makrocyclische Zweikernchelate. Dies wurde durch Röntgenkristallstrukturanalyse des cyclo-Di[nickel-μ-[1,1,1,′,1′-tetraisobutyl-3,3′-iso-phthaloyl-bisselenoureaoto(2-)-Se, O:O′, Se′]], 2, bestätigt. Die Verbindung 2 kristallisiert monoklin in der Raumgruppe P 21/c mit den Gitterkonstanten a = 11,673 (1); b = 19,834 (2); c = 13,606 (1) Å; β = 107,45 (1)° und Z = 2. Der abschließende R-Wert betrug R = 0,081 für 3049 beobachtete Reflexe. Bis-bidentate Terephthaloyl-bis(selenoharnstoffe) ergeben unter den gleichen Bedingungen makrocyclische Dreikernnickel(II)-chelate.Beide Komplextypen wurden durch FAB-Massenspektren charakterisiert.
    Additional Material: 4 Ill.
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  • 8
    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 Trimetallamacrocyle: cyclo-Tri[nickel-μ-[1,1,1′,1′-tetraethyl-3,3′-terephthaloyl-bis-thioureato(2-)-S,O:O′,S′]]The structure of the title compound has been determined by an X-ray structure analysis. The compound crystallizes in the triclinic space group P1 with a = 13.900, b = 15.403, c = 16.615 Å, δ = 84.01, β = 70.61, γ = 89.64° and Z = 2. The solution of the structure was performed by direct methods. The final R value was R = 0.073 for 2824 observed reflections. The molecule has a cyclic structure consisting of three molecules of the quadridentate ligand and three nickel atoms. The formed ring is a 27-membered trimetallamacrocycle. The nickel atoms form a nearly equilateral triangle with distances of 10.25 Å, 10.45 Å and 10.45 Å. The molecule is relatively planar.
    Notes: Die Struktur der Titelverbindung wurde durch Röntgenkristallstrukturanalyse bestimmt. Die Verbindung kristallisiert triklin in der Raumgruppe P1 mit den Gitterkonstanten a = 13,900, b = 15,403, c = 16,615 Å, δ = 84,01, β = 70,61, γ = 89,64° und Z = 2. Die Lösung der Struktur erfolgte mit direkten Methoden. Der abschließende R-Wert betrug R = 0,073 für 2284 beobachtete Reflexe. Das Molekül besitzt eine zyklische Struktur, bestehend aus drei Molekülen des quadridentaten Liganden und drei Nickel-Atomen. Der gebildete Ring ist ein 27gliedriger Trimetallamacrocyclus. Die Nickel-Atome bilden ein nahezu gleichseitiges Dreieck mit Abständen von 10,25 Å, 10,45 Å und 10,45 Å. Das Molekül ist relativ planar.
    Additional Material: 2 Ill.
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  • 9
    ISSN: 0044-2313
    Keywords: Copper, nickel complexes of N-acyl-thiourea derivatives ; acid dissociation constants ; complex stability constants ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrophilic Substituted N-Acyl-thioureas  -  Acidity and Stability of Complexes in Dioxane/Water MixturesSome derivatives of N-acyl-thioureas containing hydroxy, ester or sulfonic acid groups as well as their copper(II) and nickel(II) complexes have been synthesized. Acid dissociation constants and complex stability constants have been measured pH-potentiometrically in dioxane/water mixtures ranging from 75 to 0% (v/v) dioxane involving main group and subgroup metal ions as well. The partially remarkable changes of the constants in varied solvent mixtures are discussed.
    Notes: Eine Reihe N-Acyl-thioharnstoffe mit Hydroxy-, Ester- oder Sulfonsäuregruppen und ihre Kupfer(II)- und Nickel(II)-Komplexe wurden erstmals synthetisiert und ihre Säuredissoziationskonstanten pH-potentiometrisch in Dioxan/Wassergemischen (Dioxangehalt 75 - 0 Vol.-%) bestimmt. Die Stabilitätskonstanten der Komplexe mit 1-, 2- und 3-wertigen Metallionen aus Haupt- und Nebengruppen des PSE wurden ebenfalls ermittelt. Die z. T. drastischen Veränderungen der Konstanten bei Variation der Lösungsmittelzusammensetzung werden diskutiert.
    Additional Material: 2 Ill.
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  • 10
    ISSN: 0044-2313
    Keywords: Chelates, Gadolinium(III) ; Stability Constants ; 1H-NMR Relaxivity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chelate Formation of N-Tris(2-aminoethyl)amine-N′,N′,N″,N″,N‴,N‴-hexaacetic Acid (H6TTAHA) and N-(Pyrid-2-yl-methyl)ethylenediamine-N,N′,N′-triacetic Acid (H3PEDTA) with Gadolinium(III) - Syntheses, Stability Constants, and NMR-RelaxivitiesThe chelate formation of N-tris(2-aminoethyl)amine-N′,N′,N″,N″,N‴,N‴-hexaacetic acid (H6TTAHA) and N-(pyrid-2-yl-methyl)ethylenediamine-N,N′,N′-triacetic acid (H3PEDTA) with gadolinium(III) has been studied potentiometrically in aqueous solution at 25°C and μ = 0.1 (KCl). [Gd(TTAHA)]3-: 1gβM/ML = 19.0; {H[Gd(TTAHA)]}2-: 1gKH/MHL = 8.30; [Gd(PEDTA)]: 1gβM/ML = 15.56. Both 1 : 1 gadolinium(III) complexes were isolated as Na2H[Gd(C18H24N4O12)] · 3.5 H2O and [Gd(C14H16N3O6)] · 3 H2O, respectively. Their 1H-NMR relaxivities [1 · mmol-1 · s-1] ({H[Gd(TTAHA)]}2-: 9.5; [Gd(PEDTA)]: 8.8) offer promising applications for 1H-NMR imaging.
    Notes: Die Komplexbildung von N-Tris(2-aminoethyl)amin-N′,N′,N″,N″,N‴,N‴-hexaessigsäure (H6TTAHA) und N-(Pyrid-2-yl-methyl)ethylendiamin-N,N′,N′-triessigsäure (H3PEDTA) mit Gadolinium(III) wurde in wässeriger Lösung bei 25°C und μ = 0,1 (KCl) potentiometrisch untersucht. [Gd(TTAHA)]3-: 1gβM/ML = 19,0; {H[Gd(TTAHA)]}2-: 1gKH/MHL = 8,30; [Gd(PEDTA)]: 1gβM/ML = 15,56. Die 1 : 1-Gadolinium(III)-Komplexe wurden im Fall der H6TTAHA als Dinatriumsalz Na2H[Gd(C18H24N4O12)] · 3,5 H2O, bei der H3PEDTA als Neutralkomplex [Gd(C14H16N3O6)] · 3 H2O erhalten. Ihre NMR-Protonenrelaxivitäten [1 · mmol-1 · s-1] ({H[Gd(TTAHA)]}2-; 9,5; [Gd(PEDTA)]: 8,8) eröffnen Anwendungen als Kontrastmittel für die Kernspintomographie.
    Additional Material: 3 Ill.
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