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  • 1
    ISSN: 0044-2313
    Keywords: Sodium tellurides ; dialkyl tellurides ; X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Reactions of Sodium Telluride, Na2Te - Crystal Structure of [Na(CH3OH)3]2Te2Sodium telluride, Na2Te 1, is easily obtained by reaction of sodium with hexagonal tellurium in 1,2-dimethoxy-ethane in the presence of catalytic amounts of naphthalene. Upon exposure to oxygen 1 reacts with methanol forming [Na(CH3OH)3]2Te2 2, which crystal structure was determined. Compound 1, prepared in situ, can be conveniently converted into dialkyl tellurides, R2Te (R = C2H5, i-C3H7, CH2 = CH—CH2 3).
    Notes: Natriumtellurid, Na2Te 1, läßt sich auf bequeme Art und Weise aus Natrium und hexagonalem Tellur in 1,2-Dimethoxy-ethan als Reaktionsmedium in Anwesenheit katalytischer Mengen an Naphthalin gewinnen. Bei der Einwirkung von Sauerstoff auf 1 in Gegenwart von Methanol entsteht [Na(CH3OH)3]2Te2 2, dessen Kristallstruktur ermittelt wurde. In situ gewonnenes 1 kann auf einfache Weise in Dialkyltelluride, R2Te, übergeführt werden (R = C2H5, i-C3H7, CH2 = CH—CH2 3).
    Additional Material: 1 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 739-744 
    ISSN: 0044-2313
    Keywords: Tellurium ; Nitride Chloride ; Synthesis ; IR spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of the Tellurium Nitride Chloride [Te11N6Cl26]The title compound has been prepared by the reaction of tellurium tetrachloride with tris(trimethylsilyl)amine in boiling toluene. Pale yellow crystals of the composition [Te11N6Cl26]2 · 9C7H8 are obtained by cooling of the saturated solution. The compound was characterized by IR spectroscopy and by a crystal structure determination. Space group P1, Z = 1, structure solution with 5912 observed unique reflections, R = 0.043. Lattice dimensions at -50°C: a = 1636.2, b = 1692.7, c = 1704.1 pm, α = 60.57°, β = 69.59°, γ = 64.29°. The dominating structural element of the nitrchloride are planar Te5N3 units forming two four-member Te2N2 rings which are condensed together. Two asymmetric units [Te11N6Cl26] are linked by a centre of symmetry; the intercalated toluene molecules are without binding interactions.
    Notes: Die Titelverbindung entsteht durch Reaktion von Tellurtetrachlorid mit Tris(trimethylsilyl)amin in siedendem Toluol. Blaßgelbe Kristalle der Zusammensetzung [Te11N6Cl26]2 · 9C7H8 entstehen beim Abkühlen gesättigter Lösungen. Die Verbindung wird durch das IR-Spektrum und durch eine Kristallstrukturanalyse charakterisiert. Raumgruppe P1, Z = 1, Strukturlösung mit 5912 beobachteten unabhängigen Reflexen, R = 0,043. Gitterkonstanten bei -50°C: a = 1636,2; b = 1692,7; c = 1704,1 pm; α = 60,57 β = 69,59°; γ = 64,29°. Bestimmendes Strukturmotiv des Nitridchlorids sind planare Te5N3-Einheiten, die zwei miteinander kondensierte Te2N2-Viererringe bilden. Zwei asymmetrische Einheiten [Te11N6Cl26] sind über ein Symmetriezentrum miteiander verknüpft; die eingelagerten Toluomoleküle sind ohne bindende Wechselwirkung.
    Additional Material: 2 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1847-1853 
    ISSN: 0044-2313
    Keywords: Selenium Halides ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of SeCl3+SbCl6-, SeBr3+GaBr4-, PCl4+SeCl5-, and (PPh4+)2SeCl42- · 2 CH3CNThe crystal structures of the title compounds were determined by X-ray diffraction.SeCl3+SbCl6-: Space group P21/m, Z = 4, structure determination with 1795 observed unique reflections, R = 0.022. Lattice dimensions at -80°C: a = 940.9, b = 1066.3, c = 1234.9 pm, β = 102.79°. The compound forms ion pairs with the structure of a double octahedron with linked surfaces. SeBr3+GaBr4-: Space group Pc, Z = 2, structure determination with 1461 observed unique reflections, R = 0.058. Lattice dimensions at -60°C: a = 660.1, b = 655.3, c = 1431.3 pm, β = 101.177°. The compound crystallizes in the SCl3[AlCl4] lattice type. Between the ions there are two relatively short Se … Br—Ga contacts.PCl4+SeCl5-: Space group Ima2, Z = 8, structure determination with 1757 observed unique reflections, R = 0.029. Lattice dimensions at -50°C: a = 1651.6, b = 1201.2, c = 1166.4 pm. The SeCl5- ions are associated to chains via interionic Se—Cl … Se contacts along the crystallographic c-axis.(PPh4+)2SeCl42- · 2CH3CN: Space group P21/n, Z = 2, structure determination with 2578 observed unique reflections, R = 0.050. Lattice dimensions at -80°C: a = 1288.5, b = 726.0, c = 2585.8 pm, β = 101.65°. The compound includes planar-tetragonal SeCl42- ions, which almost meet D4h symmetry.
    Notes: Die Kristallstrukturen der Titelverbindungen wurden röntgenographisch ermittelt.SeCl3+SbCl6-: Raumgruppe P21/m, Z = 4, Strukturlösung mit 1795 beobachteten unabhängigen Reflexen, R = 0,022. Gitterkonstanten bei -80°C: a = 940,9; b = 1066,3; c = 1234,9 pm; β = 102,79°. Die Verbindung bildet Ionenpaare mit der Struktur eines flächenverknüpften Doppeloktaeders.SeBr3+GaBr4-: Raumgruppe Pc, Z = 2, Strukturlösung mit 1461 beobachteten unabhängigen Reflexen, R = 0,058, Gitterkonstanten bei -60°C: a = 660,1; b = 655,3; c = 1431,3 pm; α = 101,17°. Die Verbindung kristallisiert im SCl3[AlCl4]-Strukturtyp. Zwischen den Ionen bestehen zwei relativ kurze Se … Br—Ga-Kontakte.PCl4+SeCl5-: Raumgruppe Ima2, Z = 8, Strukturlösung mit 1757 beobachteten unabhängigen Reflexen, R = 0,029. Gitterkonstanten bei -50°C; a = 1651,6; b = 1201,2; c = 1166,4 pm. Die SeCl5- -Ionen sind über interionische Se—Cl … Se-Kontakte entlang der kristallographischen c-Achse zu Ketten assoziiert.(PPh4+)2SeCl42- · 2CH3CN: Raumgruppe P21/n, Z = 2, Strukturlösung mit 2578 beobachteten unabhängigen Reflexen, R = 0,050. Gitterkonstanten bei -80°C: a = 1288,5; b = 726,0; c = 2585,8 pm; β = 101,65°. Die Verbindung enthält planar-quadratische SeCl42--Ionen, die nahezu D4h-Symmetrie erfüllen.
    Additional Material: 8 Ill.
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  • 4
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and NMR Spectra of λ5-Diphosphets. Structure of 2,4-Diphenyl-1,1,3,3-tetrakis (diethylamino)-1λ5, 3λ5-diphosphetePreparation, properties, and n.m.r. spectra of C2H5PF2[N(C2H5)2]2, CH2=PF[N(C2H5)2]2, and the diphosphetes {RC=P[N(C2H5)2]2}2 (R) = H (5a), CH3 [(5b)] are described. The λ5-diphosphete {HC=P(NR2)2}2 (R = CH3) reacts with BF3 · O(C2H5)2 to give which is transformed into by n-C4H9Li. The crystal and molecular structure of 2,4-diphenyl-1,3,3-tetrakis(diethylamino)-1λ5,3λ5-diphosphete 2 are reported and discussed.
    Notes: Darstellung, Eigenschaften und NMR-Spektren von C2H5PF2[N(C2H5)2]2, CH2=PF[N(C2H5)2]2 und der Diphosphete {RC=P[N(C2H5)2]2}2 (R = H )(5a), CH3 [(5b)] werden beschrieben. Das λ5-Diphosphet {HC=P(NR2)2}2 (R = CH3) reagiert mit BF3 · O(C2H5)2 zu das mit n-C4H9Li in übergeht. Die Kristall- und Molekülstruktur von 2,4-Diphenyl-1,1,3,3-tetrakis(diethylamino)-1λ5,3λ5-diphosphet 2 werden mitgeteilt und diskutiert.
    Additional Material: 5 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 588 (1990), S. 147-166 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Remarks to the Synthesis of Difluorophosphoranes. n-Butyl-bis(dimethylamino)alkyliden-phosphoranes. Complex {(CO)4FeC[OSi(CH3)3]CH=P(n—C4H9) [N(CH3)2]2}Diethylamino-diethylaminosulfanyl-difluoro-i-butyl-phosphorane 3 is formed in the synthesis of bis(diethylamino)-difluoro-i-butyl-phosphorane from the corresponding phosphane by fluorination with SF4 as a by-product. Synthesis, NMR spectra, and reactions of n-butyl-bis(dimethylamino)alkylidene phosphoranes are reported. n-Butyl-bis(dimethylamino)-trimethylsilylmethylidenphosphorane, 17, reacts with Fe(CO)5 to give the tetracarbonyliron complex 19. The result of the X-ray structural analysis of 19 is reported and discussed.
    Notes: Diethylamino-diethylaminosulfanyl-difluor-i-butyl-phosphoran 3 entsteht als Nebenprodukt bei der Synthese von Bis(diethylamino)-difluor-i-butyl-phosphoran aus dem entsprechenden Phosphan durch Fluorierung mit SF4. Synthese, NMR-Spektren und Reaktionen von n-Butyl(bisdimethylamino)alkylidenphosphoranen werden berichtet. n-Butyl-bis(dimethylamino)-trimethylsilylmethylidenphosphoran, 17, reagiert mit Fe(CO)5 zu dem Tetracarbonyleisen-Komplex 19. Das Ergebnis der Röntgenstrukturanalyse von 19 wird mitgeteilt und diskutiert.
    Additional Material: 2 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 131-136 
    ISSN: 0044-2313
    Keywords: Octaselenido niccelate complex ; synthesis ; X-ray structure ; FIR spectrum ; magnetic behaviour ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Na(12-Crown-4)2]2[Ni(Se4)2] · DMF; Synthesis, Crystal Structure, and Magnetic BehaviourThe title compound has been prepared from NiCl2 and sodium polyselenide in dimethylformamide solution in the presence of 12-crown-4, forming black crystal needles. They were characterized by an X-ray structure determination, by FIR spectroscopy as well as by the magnetic behaviour.[Na(12-crown-4)2]2[Ni(Se4)2] · DMF crystallizes monoclinically in the space group P21, 3650 observed unique reflections, R = 0.046. Lattice dimensions at -80°C: a = 1020.3(2); b = 1889.5(2); c = 1498.7(3) pm; β = 108.29(1)°. The compound has an ionic structure, in which the sodium atoms of the [Na(12-crown-4)2]+ cations are coordinated by the oxygen atoms of the crown ether molecules in an antiprismatic fashion. The nickel atom of the anion [Ni(Se4)2]2- is surrounded by four selenium atoms of the tetraselenide chelates in an almost planar environment. The DMF molecules are inserted in the lattice without a bonding interaction. The magnetic susceptibility observed in the temperature interval 4.2 to 330K can be interpreted by means of a 3E ground term and D2 as local symmetry, which was established by X-ray crystallography.
    Notes: Die Titelverbindung wurde aus wasserfreiem Nickel(II)-chlorid und Natriumpolyselenid in Dimethylformamid in Gegenwart von 12-Krone-4 in Form schwarzer Kristallnadeln hergestellt und durch eine röntgenographische Strukturanalyse, durch das FIR-Spektrum und durch sein magnetisches Verhalten charakterisiert.[Na(12-Krone-4)2]2[Ni(Se4)2] · DMF kristallisiert monoklin in der Raumgruppe P21, 3650 beobachtete unabhängige Reflexe, R = 4,6%. Die Gitterkonstanten sind bei -80°C: a = 1020,3(2); b = 1889,5(2); c = 1498,7(3) pm; β = 108,29(1)°. Die Verbindung hat ionischen Aufbau. In den Kationen [Na(12-Krone-4)2]+ sind die Natriumatome durch die acht Sauerstoffatome der beiden Kronenethermoleküle antiprismatisch umgeben. In dem Anion [Ni(Se4)2]2- ist das Nickelatom nur annähernd planar von den vier Selenatomen der beiden Tetraselenidchelate koordiniert. Die DMF-Moleküle sind in das Gitter ohne bindende Wechselwirkung eingelagert.Die im Temperaturbereich von 4,2 bis 330 K beobachtete Abhängigkeit der magnetischen Suszeptibilität läßt sich unter der Annahme eines 3E-Grundterms und der röntgenographisch ermittelten lokalen Symmetrie D2 am Nickelatom verstehen.
    Additional Material: 6 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 691-696 
    ISSN: 0044-2313
    Keywords: Magnesium complexes ; diazadiene ligands ; radical anions ; endiamides ; X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Properties and Crystal Structures of Magnesium Diazadiene ComplexesReactions of phenyl-substituted 1,4-diaza-1,3-butadienes (DAD) RN=CPh—CPh=NR (R = C6H5) 1a, C6H4-4-CH3 1b, C6H4-4-OCH3 (1c) with magnesium in dimethoxyethan lead to complexes of the type [Mg(DAD)2(DME)] 2a-c, with DAD ligands in form of radical anions. Furthermore, highly reactiv complexes of the composition [Mg(DAD)(DME)2] 3a-c could be obtained. The crystal structures of 2a, 3a and 3c were determined.
    Notes: Die Reaktion phenylsubstituierter 1,4-Diaza-1,3-butadiene (DAD) RN=CPh—CPh=NR (R = C6H5 1a, C6H4-4-CH3 1b, C6H4-4-OCH3 1c) mit Magnesium in Dimethoxyethan (DME) führt zu Verbindungen des Typs [Mg(DAD)2(DME)] 2a-c, in denen die DAD-Liganden als Radikalanionen gebunden sind. Außerdem enstehen äußerst reaktive Komplexe der Zusammensetzung [Mg(DAD)(DME)2] 3a-c. Die Kristallstrukturen von 2a, 3a und 3c wurden aufgeklärt.
    Additional Material: 3 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 534 (1986), S. 27-30 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Notice on the Reaction between Phosphorus Trichloride and Hydrogen SulfideThe reaction between phosphorus trichloride and hydrogen sulfide in the presence of a base yields P4S3 and [PS2Cl2]- besides other products. A reaction scheme is proposed.
    Notes: Die Reaktion zwischen Phosphortrichlorid und Schwefelwasserstoff in Gegenwart einer Base liefert P4S3 und [PS2Cl2]- neben anderen Produkten. Es wird ein Reaktionsweg vorgeschlagen.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 554 (1987), S. 146-150 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N.M.R. Investigation of Methylphosphonium ChlorideThe n.m.r. spectra of [CH3PH3]Cl in aqueous hydrochloric acid as solvent and of [OP(CH3) (OCH2CH2Cl)OCH2—]2 in C6D6 und CD2Cl2 are described. 31P n.m.r. resonances with a line width at half height of 55 Hz are found for the H2O—HCl solutions of [CH3PH3]Cl in the solid state at 183 K.
    Notes: Die NMR-Spektren von [CH3PH3]Cl in wäßrigen HCl-Lösngen und von [OP(CH3) (OCH2CH2Cl)OCH2—]2 in C6D6 und CD2Cl2 werden beschrieben. Als Festkörper vorliegende (183 K) wäßrig-salzsaure Lösngen von [CH3PH3]Cl zeigten 31P-Resonanzlinien mit einer Halbwertsbreite von 55 Hz.
    Additional Material: 3 Tab.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 23-38 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fluoro Substituted and other New CarbodiphosphoranesSyntheses and properties of the carbodiphosphoranes [(CH3)2N]3P=C=P(CH3)[N(CH3) 2]2, (3), [(CH3)2N]2(F)P=C=P(F) [N(CH3)2]2, (7), and (C6H5)2(F)P=C=P(F)(C6H5) 2, (11), are discribed. The compounds 3, 7, and 11 as well as [(C2H5)2N]3P=C=P(CH3) [(C2H5)2N]2 are characterized by their 1H, 13C, 19F, and 31P n.m.r. and mass spectra. The crystal and molecular structures of 7 are reported.
    Notes: Synthese und Eigenschaften der Carbodiphosphorane [(CH3)2N]3P=C=P(CH3)[N(CH3)2]2, (3), [(CH3)2N]2(F)P=C=P(F)[N(CH3)2]2, (7), und (C6H5)2(F)P=C=P(F)(C6H5) 2, (11), werden beschrieben. Die Verbindungen 3, 7 und 11 sowie [(C2H5)2N]3P=C= P(CH3)[(C2H5)2N]2 sind durch ihre 1H-, 13C-, 19F- und 31P-NMR-Spektren sowie durch ihre Massenspektren charakterisiert. Die Kristall- und Molekülstruktur von 7 werden mitgeteilt.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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