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  • 1
    Electronic Resource
    Electronic Resource
    Synthesis and x-ray crystal structure of tetraethylammonium bis[1, 1-dicyanoethylene-2, 2-dithiolato]platinate(II) (1987)
    Springer
    Transition metal chemistry 12 (1987), S. 172-174 
    Details
    ISSN: 1572-901X
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary [(NEt4)]2[Pt(S2C4N2)2] has been prepared from K2PtCl4 and K2S2C4N2·H2O with NEt4Cl and characterized by single crystal x-ray structural analysis. The title compound crystallizes in the monoclinic space group P21/a witha=14.800(2),b=11.679(2),c=9.497(1) Å, β=94.51(4)° andZ=2. In the complex anion Pt sits on a centre of symmetry and is coordinated by four S atoms of the ligand (S2C4N2)2− (i-mnt). The Pt−S distances are 2.315(3) and 2.316(3) Å. The intra-and interligand S−S distances are 2.807(4) and 3.682(4) Å, respectively, indicating the rectangular planar arrangement of the sulfurs about platinum. Within the isomaleonitriledithiolate there is still some suggestion of resonance indicated by the geometry of i-mnt.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01022349
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  • 2
    Electronic Resource
    Electronic Resource
    Equilibria in complexes of N-heterocyclic molecules, part 44. The thermogravimetric behaviour of a Schilt-Barbieri compound dicyanobis-(1,10-phenanthroline) iron(II) dihydrate, Fe(phen)2(CN)2 · 2H2O (1985)
    Springer
    Transition metal chemistry 10 (1985), S. 348-349 
    Details
    ISSN: 1572-901X
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The thermogravimetric behaviour of Fe(phen)2(CN)2 · 2H2O (phen = 1,10-phenanthroline) is discussed by comparison with that of phen · H2O. It is shown that the crystal water of the Schilt-Barbieri compound is released only at 323.5 °C. After water loss, the complex decomposes immediately. Covalent hydrate formation for diimines or their complexes was discussed recently(1). In general, formation of covalent hydrates, containing moieties like , should be favoured by electron-withdrawing substituents while true hydrates, containing essentially intact molecules of water, are easily formed by electron-releasing substituents. Although no covalent hydrate has yet been established in a coordinated N-heterocycle by x-ray structural analysis, there are some cases which could involve covalent hydrate formation for diimines. One such is the strange claim that Fe(phen)2(NCS)2 · H2O is diamagnetic at room temperature whereas anhydrous Fe(phen)2(NCS)2 is paramagnetic(2), though this apparently well-studied system is almost certainly complicated by the existence(3) of several distinct solid phases of composition Fephen2(NCS)2 · nH2O. The differences in the n.m.r. spectra of the compounds [Fe(LL)(CN)4]2− (LL = phen, bipy and 5,5′-Me2-bipy) in D2O are equally interesting. While the last two display the two-fold symmetry expected of the diimine ligand LL, the former shows(4) an unexpected corresponding inequivalence. Moreover, the circular dichroism spectrum of optically active Fe(phen)2(CN)2 in acid solution shows the surprising feature that a c.d. band is observed in the visible region but the absorption in the u.v. region disappears(4) completely. We have reconfirmed this finding. Despite the apparent ease of obtaining attractive crystals of the dihydrate Fe(phen)2(CN)2 · 2H2O, there have been crystallographic problems that have so far prevented the solution of this problem by x-ray diffraction methods(5), although we have been able to obtain the structure of the adduct (±)cis-[Fe(phen)2(CN)2]2Hg(CN)2. In 1,10-phenanthroline monohydrate, despite crystallographic difficulties, there is now no doubt that the unit of structure is the hydrogen-bonded true hydrate. 1,10-Phenanthroline, despite being a substituted quinoline, seems not to form a classical Reissert compound, but the evidence for the (invariably assumed) simple structure of the Schilt-Barbieri compounds [Fe(LL)2(CN)2] is not strong. For example, there seems to be no report of an unsolvated solid. We therefore decided to compare the thermogravimetric behaviour of phen · H2O and Fe(phen)2(CN)2 · 2H2O. The compound phen · H2O is commercially available (BDH Chemicals Ltd. Poole, England) while Fe(phen)2(CN)2 · 2H2O was obtained by the method of Schilt(6). On continuous heating under a atmosphere of dinitrogen, the water of phen · H2O is released at 93 °C. The resulting anhydrous 1,10-phenanthroline is still stable, m.p. 117 °C (see Figure 2). The water molecules (one-step mechanism) of Fe(phen)2(CN)2 · 2H2O are, however, released at the remarkably high temperature of 323.5 °C followed by an immediate decomposition of the anhydrous phase (see Figure 3). Other than the possibility of very strong hydrogen bonds being present in the structure of Fe(phen)2(CN)2 · 2H2O, covalent hydrate formation could account for this unexpected behaviour. Further investigations on these Schilt-Barbieri compounds are in progress.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01036399
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  • 3
    Electronic Resource
    Electronic Resource
    mini-chiuz (1993)
    Weinheim : Wiley-Blackwell
    Chemie in unserer Zeit 27 (1993), S. 170-187 
    Details
    ISSN: 0009-2851
    Keywords: Chemistry ; Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/ciuz.19930270402
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  • 4
    Electronic Resource
    Electronic Resource
    Synthese, thermisches Verhalten und Kristallstruktur von von [Ni(NH3)6][S(O)C=C(CN)2] · 1,5, H2O, einem Salz mit Nickel(II)-hexammin-Kationen (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 147-153 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Thermal Analysis, and X-Ray Crystal Structure of [Ni(NH3)6][S(O)C=C(CN)2] · 1.5 H2O, a Salt with the Nickel (II) Hexammine CationThe compound [Ni(NH3)6][S(O)C=C(CN)2] · 1.5 H2O is obtained by reaction of solutions of nickel acetate tetrahydrate in ammonia and K2[S(O)C=C(CN)2] · H2O in water. The salt crystallizes with the monoclinic space group P 21/a. The lattice constants are a = 15.183(1), b = 13.084(1), c = 14.386(1) Å, β = 100.96(7)° and Z = 8.The X-ray structure revealed two crystallographically independent nickel hexammine cations besides pseudochalcogenolate anions. The latter are associated with water molecules and exhibit strong delocalized π-electron systems.The thermal decomposition proceeds in three different steps. The first and second step refer to evolution of ammonia while in a third step H2O is squeezed out. This results in a decomposition of the substance.
    Notes: Die Verbindung [Ni(NH3)6][S(O)C=C(CN)2] · 1,5H2O ist durch Reaktion einer ammoniakalischen Lösung von Nickelacetat-Tetrahydrat mit K2[S(O)C=C(CN)2] · H2O, gelöst in Wasser, zugänglich. Das Salz kristallisiert monoklin mit der Raumgruppe P 21/a. Die Gitterkonstanten betragen a = 15,183(1), b = 13,084(1), c = 14,3886(1) Å, β = 100,96(7)° und Z = 8.Nach der Röntgenstrukturanalyse (R = 0,07, Rw = 0,06 für 1109 beobachtete Reflexe) liegen jeweils zwei kristallographisch verschiedene Nickelhexamminkationen neben Pseudochalkogenoanionen vor. Letztere sind ausschließlich mit Hydratwassermolekülen assoziiert und weisen mit ihren Bindungslängen auf stark delokalisierte π-Elektronensysteme hin.Die thermogravimetrische Analyse zeigt einen stufenförmigen Abbau der Solvensmoleküle, wobei zunächst in zwei Schritten Ammoniak entweicht. Der Abspaltung des Hydratwassers schließt sich die Zersetzung der Substanz an.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885650116
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  • 5
    Electronic Resource
    Electronic Resource
    Synthesen, Strukturen und thermische Abbaureaktionen von TlI-, PbII- und SeII-Komplexen mit 2,2-Dicyanethylen-1,1-diselenolat (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 1565-1570 
    Details
    ISSN: 0009-2940
    Keywords: Diselenolates ; Thallium complexes ; Lead complexes ; Selenium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Preparation, Structures, and Thermal Decomposition Reactions of Complexes Consisting of TlI, PbII, and SeII and 2,2-Dicyanoethylene-1,1-diselenolateThe 2,2-dicyanoethylene-1,1-diselenolate-containing compounds (AsPh4)2[Tl2(Se2C=C(CN)2)2], (AsPh4)2[Pb(Se2C=C-(CN)2)2], and (NBu4)2[Se(Se2C=C(CN)2)2] have been prepared and characterized by single-crystal structure analysis. The molecular structures of the complex anions 1-3 are significantly influenced by the presence of stereochemically active lone pairs. 1 is dimeric with an Se4Tl2 octahedral centre with a Tl-Tl distance of 3.547(4) Å and an average Tl-Se bond length of 3.143(4) Å. In 2 Pb constitutes the centre of a distorted pseudo-trigonal bipyramid PbSe4E [Pb-Seave = 2.948(3) Å] with one equatorial position obviously occupied by the lonepair E. In 3 the ligands are coordinated to the central Se, which is situated in a centre of symmetry, in an undistorted way giving rise to a Ψ-octahedral SeSe4E2 geometry [Se-Seave = 2.617(2) Å]. The compounds (AsPh4)2 · 1, (AsPh4)2 · 2 and (NBu4)2 · 3 have been decomposed thermally to yield TlSe, PbSe as well as Se. The observed contamination of TlSe and PbSe with As is avoided by using (NBu4)2 · 1 and (NBu4)2 · 2 as precursor materials.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250709
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  • 6
    Electronic Resource
    Electronic Resource
    Untersuchungen im quasi-binären System LiI/2,2′-Bipyridin (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 483-486 
    Details
    ISSN: 0044-2313
    Keywords: Melt diagram ; Lithium iodide ; Bipyridine ; Solvate structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigations in the Quasi-Binary System LiI/2,2′-BipyridineThe compounds [LiI(bpy)4.5] (1), [LiI(bpy)2] (2), [LiI(bpy)] (3) and [LiI(bpy)0.5] (4) can be obtained as congruently melting solvates of melts of LiI and 2,2′-bipyridine (bpy) under an argon atmosphere. Single crystals of 1 and 4 suitable for X-ray structure analysis have been grown from the melt, while 2 and 3 yield only fine-crystalline powders. 1 is a typical solvate complex with bpy coordinated to Li. In 4 there are ion-pairs coordinated by bpy associated to polymeric chains.
    Notes: Im Schmelzdiagramm LiI/2,2′-Bipyridin (bpy) treten vier Dystektika auf. Die diesen zugeordneten kongruent schmelzenden Verbindungen [LiI(bpy)4.5] (1), [LiI(bpy)2] (2), [LiI(bpy)] (3) und [LiI(bpy)0.5] (4) können unter Argon kristallin aus der Schmelze gezüchtet werden. Die Röntgenstrukturanalyse zeigt für 1 einen typischen Solvenskomplex mit durch bpy solvatisiertem Li. In der Struktur von 4 treten dagegen Polymerketten aus solvatisierten Ionenpaaren auf. Die Verbindungen 2 und 3 fallen feinkristallin an und konnten strukturell bisher noch nicht untersucht werden.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230176
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  • 7
    Electronic Resource
    Electronic Resource
    Formation of Tetranuclear Chelate(4-) Ions of Divalent Metals (Mn, Co, Ni) with Idealized T Symmetry by Spontaneous Self-assembly“Adamantanoid” Chelate Complexes, Part 2. This work was supported by the Deutsche Forschungsgemeinschaft and the Fonds der Chemischen Industrie. Part 1:[3].Dedicated to Professor Paul von Ragué Schleyer on the occasion of his 60th birthday (1990)
    Weinheim : Wiley-Blackwell
    Angewandte Chemie International Edition in English 29 (1990), S. 311-314 
    Details
    ISSN: 0570-0833
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/anie.199003111
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  • 8
    Electronic Resource
    Electronic Resource
    Strukturen neuer SeII- und TeII-Komplexe mit 2,2-Dicyanethylen-1,1-dithiolat, 2,2-Dicyanethylen-1,1-thioselenolat und 2,2-Dicyanethylen-1,1-diselenolat (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1483-1488 
    Details
    ISSN: 0044-2313
    Keywords: Selenium complexes ; tellurium complexes ; dicyanethylenedithiolate ; dicyanethylenethioselenolate ; dicyanethylenediselenolate ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structures of New SeII and TeII Complexes Containing 2,2-Dicyanethylene-1,1-dithiolate, 2,2-Dicyanethylene-1,1-thioselenolate, and 2,2-Dicyanethylene-1,1-diselenolate(NBu4)2{Se[S2C=C(CN)2]2} (I), (AsPh4)2 · {Te[SSeC=C(CN)2]2} (II), and (NBu4)2{Te[Se2C=C(CN)2]2} (III) containing the bidentate chelate ligands 2,2-dicyanethylene-1,1-dithiolate i-mnt, 2,2-dicyanethylene-1,1-thioselenolate i-mnts, and 2,2-dicyanethylene-1,1-diselenolate i-mns have been prepared and characterized by X-ray structure analysis. The central units consist of [M(X—X)2E2]2- (M = Se, Te; X—X = ligand; E = lone-pair) with fourfold coordinated SeII and TeII, respectively. The complex anions [Se(i-mnt)2E2]2- as well as [Te(i-mnts)2E2]2- show a trapezoide distortion with d(Se—S) = 2.276(5); 2.287(5); 2.803(5); 2.789(5) Å and d(Te—Se) = 2.611(2); 2.617(3); d(Te—S) = 2.889(5); 2.935(4) Å. In III there are centrosymmetric complex anions [Te(i-mns)2E2]2- with nearly identical Te—Se-bond-lengths: 2.674(3) and 2.692(2) Å. These Te—Se bonds are elongated compared to usual Te—Se bonds.
    Notes: (NBu4)2{Se[S2C=C(CN)2]2} (I), (AsPh4)2 · {Te[SSeC=C(CN)2]2} (II) und (NBu4)2{Te[Se2C=C(CN)2]2} (III) mit den zweizähnigen Liganden 2,2-Dicyanethylen-1,1-dithiolat i-mnt, 2,2-Dicyanethylen-1,1-thioselenolat i-mnts und 2,2-Dicyanethylen-1,1-diselenolat i-mns wurden dargestellt und durch Einkristallstrukturanalysen charakterisiert. In den zentralen M(X—X)2E2-Einheiten (M = Se, Te; X—X = Ligand, E = freies Elektronenpaar) liegt vierfach koordiniertes SeII bzw. TeII vor. Die Komplexanionen [Se(i-mnt)2E2]2- und [Te(i-mnts)2E2]2- sind trapezförmig verzerrt mit d(Se—S) = 2,276(5); 2,287(5); 2,803(5); 2,789(5) Å und d(Te—Se) = 2,611(2); 2,617(3); d(Te—S) = 2,889(5); 2,935(4) Å. In III liegen dagegen zentrosymmetrische Komplexanionen [Te(i-mns)2E2]2- mit nahezu gleichlangen Te—Se-Bindungen vor: 2,674(3) und 2,692(2) Å. Die Te—Se-Bindungen sind dabei gegenüber gewöhnlichen Te—Se-Bindungslängen deutlich aufgeweitet.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200828
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  • 9
    Electronic Resource
    Electronic Resource
    Vierkernige Chelat(4-)-Ionen zweiwertiger Metalle (Mn, Co, Ni) mit idealisierter T-Symmetrie durch spontane Selbstorganisation„Adamantanoide“ Chelatkomplexe, 2. Mitteilung Diese Arbeit wurde von der Deutschen Forschungsgemeinschaft und dem Fonds der Chemischen Industrie gefördert. - 1. Mitteilung: [3].Professor Paul von Ragué Schleyer zum 60. Geburtstag gewidmet (1990)
    Weinheim : Wiley-Blackwell
    Zeitschrift für die chemische Industrie 102 (1990), S. 292-295 
    Details
    ISSN: 0044-8249
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/ange.19901020309
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