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  • 1
    Electronic Resource
    Electronic Resource
    Kristallstruktur von 5-Oxo-1,3λ4,2,4-dithiadiazol, S2N2CO, und seine Addukte mit Lewis-Säuren (1978)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 111 (1978), S. 1670-1676 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of 5-Oxo-1,3λ4,2,4-dithiazole, S2N2CO, and its Adducts with Lewis AcidsA simple synthesis of 5-oxo-1,3λ4,2,4-dithiadiazole (S2N2CO, 1) is reported. 1 crystallizes in the space group Pbca-D-2n15 and is a five-membered planar ring. Reactions of 1 in CH2Cl2 with the Lewis acids A yield the mono- and bisadducts S2N2CO · A and (S2N2CO)2 · A, where A = BF3 (2a), SO3 (2b), SbCl5 (2c), SbF2Cl3 (2d), SnCl4 (3a), and TiCl4 (3b). IR and Raman spectra are reported and possible structures of the adducts are discussed.
    Notes: Es wird eine einfache Synthese für 5-Oxo-1,3λ4,2,4-dithiadiazol (S2N2CO. 1) beschrieben. 1 kristallisiert in der Raumgruppe Pbca-D2n15 und ist ein fünfgliedriger planarer Ring. Reaktionen von 1 in CH2Cl2 mit den Lewis-Säuren A ergeben die Mono- und Bisaddukte S2N2CO · A und (S2N2CO)2 · A, wobei A = BF3 (2a), SO3 (2b), SbCl5 (2c), SbF2Cl3 (2d), SnCl4 (3a) und TiCl4 (3b) ist. IR- und Raman-Spektren werden mitgeteilt und mögliche Strukturen der Addukte diskutiert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19781110503
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  • 2
    Electronic Resource
    Electronic Resource
    Über die ersten monosubstituierten Derivate von Triboran(7). - Kristall- und Molekülstruktur von Benzoyloxytriboran(7) (1989)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 1049-1056 
    Details
    ISSN: 0009-2940
    Keywords: Triborane(7) derivatives ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Monosubstituted Derivatives of triborane(7). - Crystal and Molecular Structure of Benzoyloxytriborane(7)B6H14 generated in situ has been shown to react with carboxylic acids, monothiocarboxylic acids, dialkoxydithiophosphorus acids, and diaryldithiophosphinic acids by splitting off H2 to form the chelate-stabilized compounds of the type B3H6X, where X = RCO2, RCOS, (RO)2PS2 und R2PS2. Reactions of carboxylic acids with some triborane(7) adducts or B4H10 produce the same type of compounds. The X-ray structure determination of Ph—CO2B3H6 is reported. All compounds show fluxional behaviour on the 11B-NMR time scale.
    Notes: Generiert man B6H14 in situ in Gegenwart von Carbonsäuren, Monothiocarbonsäuren, Dialkoxydithiophosphorsäuren oder Diaryldithiophosphinsäuren, so entstehen unter H2-Abspaltung die Chelat-stabilisierten Verbindungen des Typs B3H6X, wobei X = RCO2, RCOS, (RO)2PS2 und R2PS2 sein kann. Zum gleichen Verbindungstyp gelangt man bei der Reaktion zwischen bestimmten Triboran(7)-Addukten bzw. B4H10 mit Carbonsäuren. Von Ph—CO2B3H6 wurde eine Röntgenstrukturanalyse durchgeführt. Sämtliche Verbindungen zeigen im 11B-NMR-Spektrum dynamisches Verhalten.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19891220606
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  • 3
    Electronic Resource
    Electronic Resource
    Synthese und Struktur des ersten oligomeren cyclischen Dimethylsilyl-substituierten Carbodiimids (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 2569-2571 
    Details
    ISSN: 0009-2940
    Keywords: Carbodiimide, silyl ; Structure ; Precursor ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Structure of the First Oligomeric Cyclic Dimethylsilyl-Substituted CarbodiimideNew oligomeric cyclic silylcarbodiimides 1-3 are synthesised by the reaction of the respective dichlorosilanes with cyanamide. From the resulting reaction mixture with dichloro-dimethylsilane the tetrameric compound of the hypothetical [(CH3)2Si=N-CN] is isolated. In this molecule sixteen atoms build a nearly planar ring structure with a special steric arrangement of the groups. This oligomeric silylcarbodiimides present a new kind of precursors for the pyrolytic synthesis of ceramics in the ternary system SiCN.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931261202
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  • 4
    Electronic Resource
    Electronic Resource
    On the Polymorphism of White PhosphorusDedicated to Professor Gottfried Huttner on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1235-1240 
    Details
    ISSN: 0009-2940
    Keywords: Phosphorus ; Phase transitions ; Molecular crystal ; Crystal growth ; Low-temperature crystal structure ; Librational motion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: White phosphorus occurs in three modifications. The α form, which exists at roomtemperature, transforms reversibly to the β form at -77°C. The α · β transformation may be strongly delayed. Quenching the α form to -185°C followed by slow warming results in an exothermic reactions with formation of the γ form which transforms into the β form at -120°C in an endothermic reaction. A transition β · γ is not observed. The γ form is characterized by its powder diagram. The structure of the β form is redetermined from a single crystal at -185°C (P., α = 547.88(5), b = 1078.62(11), c = 1096.16(11)pm, α= 94.285(8), β = 99.695(7), γ = 100.680(7)., V = 623.79(10) · 106 pm3, Z = 6 formula units per cell). The P4 molecules exhibit pronounced librational motion in spite of the low temperature of investigation. The arrangement of the centers of the tetrahedra corresponds to the atom positions in the γ-plutonium structure, which is discussed in relation to the bcc structure.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300911
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  • 5
    Electronic Resource
    Electronic Resource
    Ein neuer Weg zu N-silylierten Diaminosulfanen: Die Spaltung der Si-Si-Bindung in Disilanen durch Schwefeldiimide (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 75-77 
    Details
    ISSN: 0009-2940
    Keywords: Diaminosulfanes / Disilanes / Sulfur diimides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A New Route to N-Silylated Diaminosulfanes: The Splitting of the Si — Si Bond in Disilanes by Sulfur DiimidesSulfur diimides (R1N)S(N2) (R1, R2 = tBu, SiMe3; 1a-c) and disilanes Cl2(R)Si-Si(R)Cl2 [R = Me (2), Cl (3)] react fast and quantitatively in a 1:1 ratio to give diaminosulfanes (4, 5) by cleavage of the Si-Si bond. The solid-state structure of tBu(SiMeCl2)N-S-N(SiMe3)SiMeCl2 (4b) has been studied both by X-ray crystallography and 29Si-NMR spectroscopy.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901230115
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  • 6
    Electronic Resource
    Electronic Resource
    [(BH2)6S4]2-, [(BH2)6Se4]2-: neue Chalcogenoborwasserstoff-Anionen mit Adamantanstruktur (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 427-432 
    Details
    ISSN: 0009-2940
    Keywords: Chalcogenoboron hydride structure ; Adamantane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [(BH6)2]S4]2-, [(BH2)Se4]2-: New Chalcogenoboron Hydride Anions with Adamantane StructureThe reaction of THF·BH3/NaBH4 (2: 1) with H2S produces Na[H3B-μ2-S(B2H5)] (5) with hydrogen evolution. 5 reacts with an excess of H2S to give Na2[(BH2)6S4] (3a), which is also formed in the reaction of THF·BH3 with NaSH or anhydrous Na2S. These reactions proceed via 5 and the intermediates 7 or 8 by loss of BH-4 and cyclization. The analogous compound Na2[(BH2)6Se4] (4a) is obtained by the reaction of elemental selenium with NaBH4 (1:1) in triglyme. The primary product is Na2[H3B-Se-Se-BH3] (9). Treatment of 9 at 100 - 110°C yields 4a and polymers, 3a and 4a react with CsBr to form the crystalline compounds Cs2[(BH2)6Se4]·CsBr (3b) and Cs2-[(BH2)6Se4]·CsBr (4b), characterized by X-ray structure determinations. The anions of 3b and 4b consist of an adamantane skeleton. The Br- ion is octahedrally coordinated by Cs+ ions. The Cs6Br octahedra share faces to form columns along the hexagonal c axis. The crystal structures of the isotypic compounds 3b and 4b are closely related to the structure of CsNiCl3.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240304
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  • 7
    Electronic Resource
    Electronic Resource
    Synthese von 1,2,5-Azastannaborol-Derivaten aus Schwefeldiimid-Anionen und cis-Stannyl-boryl-alkenen - Röntgenstrukturanalyse von zwei 2,5-Dihydro-1-(imino-λ4-sulfanyliden)-1,2,5-azastannaboratolen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 691-697 
    Details
    ISSN: 0009-2940
    Keywords: cis-Stannyl-boryl-alkenes ; Sulfur diimide anions ; Multinuclear NMR ; 1,2,5-Azastannaboratoles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis of 1,2,5-Azastannaborole Derivatives from Sulfur Diimide Anions and cis-Stannyl-boryl-alkenes - X-ray Crystallographic Study of Two 2,5-Dihydro-1-(imino-λ4-sulfanylidene)-1,2,5-azastannaboratoles(E)-3-(Diethylboryl)-2-(chlorodimethylstannyl)-2-pentene (1) reacts with the sulfur diimide anions 3 [R - NSN-K+, R=tBu (a), Me3Si (b), tBu2P (c)] in a 1:1 ratio, and with 4 (K+;-NSN-K+) in a 2:1 ratio, to give various heterocycles. The first products of the reaction between 1 and 3 [2,5-dihydro-1-(imino-λ4-sulfanylidene)-1,2,5-azastannaboratoles 5a, b, c] are isolated at -30°C and characterized by X-ray crystallography. The compounds 5a,b rearrange into the borole derivates 6a,b (with an additional N—Sn coordination) by transfer of an ethyl group from the boron to the sulfur atom. Ethylene is eliminated from compound 6a (not 6b) to give the diaminosulfane derivative 7a. The 2:1 reaction between 1 and 4 affords an unstable intermediate 8 with a fluxional structure, leading to 9 in which an EtS moiety bridges a borole ring (analogous to 6 but without the additional N - Sn coordination) and a boratole ring (analogous to 5). All compounds are characterized by 1H-, 11B-, 13C-, 15N- (in part), 29Si- and 119Sn-NMR spectra.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240404
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  • 8
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur von PbMo5O8; ein reduziertes Oxomolybdat mit Mo10O28-Oktaederdoppeln (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 49-63 
    Details
    ISSN: 0044-2313
    Keywords: Oxomolybdates ; cluster ; crystal structure ; HRTEM ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of PbMo5O8; a reduced Oxomolybdate with Mo10O28 Double OctahedraThe crystal structure of the new phase PbMo5O8 contains oligometric Mo clusters which consist of two edge-sharing Mo6 octahedra connected according to Mo10O6iO4/2i-iO16/2i-a. The compound is isotypic with LaMo5O8. Isolated, divalent Pb atoms are located in the “channels” of the monoclinic structure (a = 999.3(2) pm, b = 924.7(1) pm, c = 753.6(2) pm, β = 109.39(2)°, P21/a. Compared to the compound In 11Mo40O62 the Mo—O distances (average 206 pm) and the Mo—Mo distances within the octahedral units (average 275 pm) are slightly decreased by 1 and 4 pm, respectively. The very short Mo—Mo distances (278 pm) between the cluster units which are not observed in In11Mo40O62 (320 pm) are due to excess electrons in these inter-cluster bonds which would otherwise occupy antibonding cluster states.
    Notes: Mit der neuen Phase PbMo5O8 wurde ein weiteres Beispiel für oligomere Mo-Cluster aus zwei kantenverknüpften Mo6-Oktaedern gefunden, die nach Mo10O6iO4/2i-iO16sol;2i-a verknüpft sind. Die Verbindung ist isotyp zu LaMo5O8. In den „Kanälen“ der monoklinen Struktur a = 999,3(2) pm, b = 924,7(1) pm, c = 753,6(2) pm, β = 109,39(2)°, P21/a) findet man isolierte, zweiwertige Pb-Atome. Gegenüber der Verbindung In11Mo40O62 sind die Mo—O-Abstände mit durchschnittlich 206 pm nur gering um 1 pm und die Mo—Mo-Abstände innerhalb der oktaedrischen Baueinheiten mit durchschnittlich 275 pm ebenfalls nur schwach um 4 pm verkürzt. Allerdings findet man mit 278 pm sehr kurze Mo—Mo-Abstände zwischen den Clustereinheiten, die so nicht bei In11Mo40O62 (320 pm) beobachtet werden können. An diesen inter-Cluster-Bindungen sind überschüssige Elektronen beteiligt, die andernfalls antibindende Clusterzustände besetzen würden.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916020106
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  • 9
    Electronic Resource
    Electronic Resource
    Ti9Se2 - Eine Verbindung mit kolumnaren ∞1[Ti9]-BaueinheitenProfessor Herbert Jacobs zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 630-634 
    Details
    ISSN: 0044-2313
    Keywords: Metal-rich titanium selenide ; preparation ; single crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Metal-Rich Titanium Selenide Ti9Se2The new compound Ti9Se2 has been prepared as hitherto most metal-rich phase in the system titanium-selenium. It crystallizes in the orthorhombic space group Pbam (No. 55) with a = 691.7(2), b = 1 550.5(9), c = 345.4(2) pm. The structure consists of ∞1[Ti9]-strings which are described within the concept of condensed clusters. The Se atoms are coordinated by tricapped trigonal prisms of Ti atoms.
    Notes: Die erstmals dargestellte Verbindung Ti9Se2 ist die bislang metallreichste Phase im binären System Titan-Selen. Sie kristallisiert in der orthorhombischen Raumgruppe Pbam (Nr. 55) mit a = 691.7(2), b = 1 550.5(9), c = 345.4(2) pm. Die Struktur enthält ∞1[Ti9]-Baueinheiten, die im Konzept kondensierter Metallcluster beschrieben werden. Die Se-Atome sind von einem dreifach überkappten trigonalen Prisma aus Ti-Atomen umgeben.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220410
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  • 10
    Electronic Resource
    Electronic Resource
    Gd4I6CN: Ein Carbidnitrid mit Ketten aus Gd6(C2)-Oktaedern und Gd6N2-TetraederdoppelnProfessor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1889-1897 
    Details
    ISSN: 0044-2313
    Keywords: Gadolinium Iodide Carbide Nitride ; Gadolinium Bromide Carbide Nitride ; Yttrium Iodide Carbide Nitride ; Lanthanum Iodide Carbide Nitride ; preparation ; X-ray single crystal structure investigation ; crystal structure ; condensed cluster ; chain of condensed octahedra and double tetrahedra ; C—C single bond ; Gd6(C2) octahedron ; Gd6N2 double tetrahedron ; Y10(C2)2 double octahedron ; Y6N2 double tetrahedron ; α-Gd4I6CN, β-Gd4I6CN, Y6I9C2N, α-Gd4Br6CN, α-La4I6CN ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Gd4I6CN: A Carbide Nitride with Chains of Gd6(C2) Octahedra and Gd6N2 Double TetrahedraThe compound α-Gd4I6CN is prepared by reaction of Gd, GdI3, C, and GdN (1:2:1:1 mole ratio) at 1 170 K in sealed Ta tubes. It is obtained as brown red, transparent needles which are air and moisture sensitive. The structure of α-Gd4I6CN contains Gd6 octahedra centered by C2 groups and double tetrahedra centered by N atoms. The units are alternatingly connected via common edges to form chains (Gd2Gd4/2C2) (Gd2/2Gd2/2N)2 parallel [001]. The linear chains are surrounded by I atoms above all free edges of the metal polyhedra and linked according to (Gd2Gd4/2C2) (Gd2Gd4/2N2)I4/2I8I2 in the a - b plane.We also found β-Gd4I6CN, which is formed in a monotropic transition from the α-form. In the structure the chains of Gd octahedra and tetrahedra as described for α-Gd4I6CN are more densely packed.The structure of Y6I9C2N is composed by chains of pairs of Y-octahedra and Y-tetrahedra, respectively. The octahedra are centered by C2 groups, the tetrahedra by N-atoms.We also synthesized the compounds Gd4Br6CN und La4I6CN by tempering at 1 220 K. They are isotypic with α-Gd4I6CN.
    Notes: α-Gd4I6CN wird durch Reaktion von Gd, GdI3, C und GdN (Molverhältnis 1:2:1:1) bei 1 170 K im verschlossenen Ta-Tiegel erhalten. Es bildet braunrot durchscheinende Nadeln, die gegen Luft und Feuchtigkeit empfindlich sind. Die Struktur von α-Gd4I6CN enthält durch C2-Einheiten zentrierte Gd6-Oktaeder und Doppel aus N zentrierten Tetraedern, Gd6N2. Abwechselnd sind Oktaeder und Tetraederdoppel über gemeinsame Kanten zu Ketten (Gd2Gd4/2C2) (Gd2/2Gd2/2N)2 verknüpft, die parallel [001] ausgerichtet sind. Diese eindimensionalen Einheiten sind über allen freien Kanten durch Iodatome koordiniert und untereinander nach dem Schema (Gd2Gd4/2C2) · (Gd2Gd4/2N2)I4/2I8I2 in der a - b-Ebene verknüpft.Daneben existiert noch ein β-Gd4I6CN, das sich monotrop aus der α-Form bei 1 300 K bildet. Dessen Struktur zeichnet sich durch eine dichtere Packung der für die α-Form beschriebenen Gd-Oktaeder-Tetraederketten aus.In der Struktur von Y6I9C2N sind die Ketten aus Doppeln sowohl C2-zentrierter Oktaeder als auch N-zentrierter Tetraeder der Y-Atome aufgebaut.Weiter erhielten wir die mit α-Gd4I6CN isotypen Verbindungen Gd4Br6CN und La4I6CN durch Tempern der Ausgangsverbindungen bei 1 220 K.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946201109
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