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  • Inorganic Chemistry  (9)
  • Synthesis  (2)
  • Arenkomplexe  (1)
  • IR Spectra  (1)
  • 1995-1999  (10)
  • 1997  (10)
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  • 1995-1999  (10)
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  • 1
    ISSN: 0044-8249
    Keywords: Arenkomplexe ; Brückenliganden ; Platin ; Silber ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 2
    ISSN: 0044-2313
    Keywords: Magnesium Compounds ; Phosphoraneiminato Complexes ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphaneimine and Phosphoraneiminato Complexes of Magnesium. The Crystal Structures of [MgBr1,25I0,75(Me3SiNPMe3)(OEt2)], [MgI2(Me3SiNPMe3)2], [Mg2I2(Me3SiNPMe2CH2)(Me3SiNPMe2CH2CH(Me)O)(OEt2)], and [MgBr(NPMe3)]4 · C7H8By reactions of the silylated phosphaneimine Me3SiNPMe3 with the Grignard reagents EtMgBr and MeMgI, respectively, the carbanionic phosphoraneiminato derivatives [XMg(CH2PMe2NSiMe3)]n (X = Br, I) can be isolated as main products. The by-products of these reactions, [MgBr1.25I0.75(Me3SiNPMe3)(OEt2)], [MgI2(Me3SiNPMe3)2] and [Mg2I2(CH2PMe2NSiMe3)(O(Me)CHCH2PMe2NSiMe3)(OEt2)] were identified by crystal structure determinations. The phosphoraneiminato complex [MgBr(NPMe3)]4 · C7H8 with hetero cubane structure is formed by a metathesis reaction of [ZnBr(NPMe3)]4 with RMgBr (R = Ph. Mes).
    Notes: Als Hauptprodukte der Umsetzungen des silylierten Phosphanimins Me3SiNPMe3 mit den Grignard-Reagentien EtMgBr und MeMgl wurden die carbanionischen Phosphaniminato-Derivate [XMg(CH2Pme2NSiMe3)]n (X = Br, I) isoliert. Als Nebenprodukte wurden [MgBr1,25I0,75(Me3SiNPMe3)(OEt2)], [Mgl2(Me3SiNPMe3)2] und [Mg2I2(CH2PMe2NSiMe3)(O(Me)CHCH2PMe2NSiMe3(OEt2)] durch röntgenographische Strukturanalysen identifiziert. Den Phosphaniminato-Komplex [MgBr(NPMe3)]4 · C7H8 mit Heterocuban-Struktur erhielten wir durch Metathese-Reaktion aus [ZnBr(NPMe3)]4 und RMgBr (R = Ph, Mes).
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1203-1204 
    ISSN: 0044-2313
    Keywords: Ytterbium Complex ; Amido Compound ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [Yb3OBr4{N(SiMe3)2}3(THF)3], an Amido Complex of Ytterbium with a Clusterlike StructureThe title compound has been prepared from YbBr3 and NaN(SiMe3)2 in THF suspension, forming yellow single crystals from hexane solutions which were characterized by a crystal structure determination. Space group P1, Z = 2, lattice dimensions at -100°C: a = 1085.4(1), b = 1410.2(1), c = 1912.0(1) pm; α = 78.62(1)°, β = 80.61(1)°, γ = 73.45(1)°, R = 0.025.In the molecular structure of [Yb3OBr4{N(SiMe3)2}3(THF)3] the three ytterbium atoms together with the μ3-oxygen atom and a μ3-bromine atom form a distorted trigonal bipyramid. In addition, three μ2-Br atoms coordinate the Yb atoms in the equatorial plane, whereas the THF molecules and the N(SiMe3)2- ligands are terminally coordinated, thus forming a distorted octahedrally surrounding of the Yb atoms.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1306-1310 
    ISSN: 0044-2313
    Keywords: Lithium Cluster ; Carbdianion ; NMR spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Li7(CHPMe2NSiMe3)3(OSiMe2nBu)]2, a Mixed-Ligand-Li14 Cluster with the Carbdianion (CHPMe2NSiMe3)2-The title compound is formed as colourless moisture and oxygen sensitive crystals by the reaction of [LiCH2PMe2NSiMe3]4 with zinc or cobalt chloride in a toluene suspension in the presence of silicongrease (-OSiMe2-)n and n-butyllithium. It is characterized by multinucleus NMR spectroscopy and by crystal structure determinations of two different crystal individuals.1. Space group P1, Z = 1, lattice dimensions at -70 °C: a = 1272.0, b = 1392.6, c = 1417.6 pm, α = 115.33°, β = 96.75°, σ = 106.81°; R = 0.042.2. Space group P21/n, Z = 2, lattice dimensions at -50 °C: a = 1424.8, b = 1457.1, c = 1997.0 pm, β = 90.32, R = 0.069.
    Notes: Die Titelverbindung (farblose, feuchtigkeits- und sauerstoffempfindliche Kristalle) entsteht bei der Reaktion von [LiCH2PMe2NSiMe3]4 mit wasserfreiem Zink- oder Cobaltchlorid in einer Toluolsuspension in Gegenwart von Siliconfett (-OSiMe2-)n und n-Butyllithium. Sie wird durch Multikern-NMR-Spektroskopie und durch Kristallstrukturanalysen zweier kristallchemisch verschiedener Individuen charakterisiert.1. Raumgruppe P1, Z = 1, Gitterkonstanten bei -70 °C: a = 1272,0; b = 1392,6; c = 1417,6 pm; α = 115,33°; β = 96,75°; σ = 106,81°; R = 0,042.2. Raumgruppe P21/n, Z = 2, Gitterkonstanten bei -50 °C: a = 1424,8; b = 1457,1; c = 1997,0 pm; β = 90,32°; R = 0,069.
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  • 5
    ISSN: 0044-2313
    Keywords: Zinc Complexes ; Syntheses ; IR Spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Zincates [Na(12-Crown-4)2][Zn{N(SiMe3)2}3] and [Na(12-Crown-4)2]2[Zn(C≡C-Ph)3(THF)][Zn(C≡C-Ph)3]The homoleptic amido complex [Na(12-crown-4)2][Zn{N(SiMe3)2}3] (1) is prepared from Zn[N(SiMe3)2]2 and NaN(SiMe3)2 in toluene solution in the presence of 12-crown-4. Single crystals of 1 · 0,5 C6H14 can be obtained from diethylether/hexane solutions. 1 reacts with phenylacetylene to give [Na(12-crown-4)2][Zn(C≡C-Ph)3] (2) which forms single crystals 2 · 0.5 THF from tetrahydrofurane solutions. The complexes were characterized by IR spectroscopy and by crystal structure determinations.
    Notes: Der homoleptische Amidokomplex [Na(12-Krone-4)2][Zn{N(SiMe3)2}3] (1) entsteht aus Zn[N(SiMe3)2]2 und NaN(SiMe3)2 in Toluol-Lösung in Gegenwart von 12-Krone-4. Einkristalle von 1 · 0,5 C6H14 erhält man aus Diethylether/Hexan-Lösungen. 1 reagiert mit Phenylacetylen unter Bildung von [Na(12-Krone-4)2][Zn(C≡C-Ph)3] (2), das nach Kristallisation aus Tetrahydrofuran Einkristalle 2 · 0,5 THF bildet. Die Komplexe werden IR-spektroskopisch und durch Kristallstrukturanalysen charakterisiert.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 351-356 
    ISSN: 0044-2313
    Keywords: Organomanganese Compounds ; Phosphoraneiminato Complexes ; Syntheses ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organomanganese Phosphoraneiminato Complexes with Heterocubane StructureThe organomanganese phosphoraneiminato complexes [MnR(NPEt3)]4 (R = Me, C=C—Ph, C=C—Tol, C=C—CMe3, C=C—SiMe3) with heterocubane structures have been prepared by reaction of the bromo derivative [MnBr(NPEt3)]4 with the corresponding lithium reagents LiR in THF/hexane solution, forming shiny red, very reactive compounds which are well soluble in hydrocarbons. They were characterized by mass spectroscopy, IR spectroscopy and by crystal structure determinations. According to these the compounds form nearly perfect Mn4N4 heterocubane frameworks with m̈3-N bridges of the phosphoraneiminato groups with Mn—N bond lengths of 214.5 pm in average which leads to Mn … Mn contacts of 299.5 pm in average. The organic residues R are terminal bonded with Mn—C distances Mn—Me of 219.5 pm and Mn—C=C—R of 207.6 pm in average.
    Notes: Die organisch substituierten Phosphanimi nato-Komplexe des Mangan(II) mit Heterocubanstruktur [MnR(NPEt3)]4 (R = Me, C=C—Ph, C=C—Tol, C=C—CMe3, C=C—SiMe3) werden durch Reaktion des Bromoderivates [MnBr(NPEt3)]4 mit den entsprechenden Lithium-Reagentien LiR in THF/Hexan als leuchtend rote, sehr reaktive, in Kohlenwasserstoffen leicht lösliche Verbindungen erhalten. Sie werden durch die Massen- und IR-Spektren sowie durch Kristallstrukturanalysen charakterisiert. Danach werden je vier Manganatome über je vier m̈3-N-Atome der Phosphan-iminato-Gruppen zu nur wenig verzerrten m̈3-N4-Kuben mit Mn—N-Abständen von im Mittel 214,5 pm verbrückt, was zu Mn … Mn-Kontakten von 299,5 pm führt. Die Reste R sind terminal gebunden mit Mn—C-Abständen Mn—Me von 219,5 pm und Mn—C=C—R von im Mittel 207,6 pm.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1035-1036 
    ISSN: 0044-2313
    Keywords: Titanium compound ; Phosphorane iminato derivatives ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetrakis(triphenylphosphoraneiminato)titanium, [Ti(NPPh3)4]The title compound has been prepared by the reaction of [TiCl2(NPPh3)2] with methyllithium and cyclopentadienyllithium, respectively, in hexane solution. [Ti(NPPh3)4] · 3 C7H8 crystallizes from toluene solution to form colourless, only slightly moisture sensitive crystals which were characterized by a crystal structure determination. Space group I41/a, Z = 8, lattice dimensions at -80°C: a = b = 2160.7(2), c = 3334.2(3) pm, merohedral (110) twin, R = 0.077. The compound forms monomeric molecules with tetrahedrally coordinate titanium atoms and bonding parameters of TiN = 187.3 pm, PN = 155.1 pm, TiNP 150.4° in average.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1375-1379 
    ISSN: 0044-2313
    Keywords: Tellurium Nitride Chloride ; Synthesis ; 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 Ionic Tellurium Nitride Chloride[Te3N2Cl5(SbCl5)]+SbCl6-The title compound has been prepared by the reaction of Te2NCl5 with antimony pentachloride in CH2Cl2 suspension. It is characterized by IR spectroscopy and by a crystal structure determination. Space group P21/c, Z = 4, lattice dimensions at -70°C: a = 1535.6, b = 1259.5, c = 1572.4 pm, β = 109.30°, R = 0.031. The compound forms an ionic pair with the central group of a (TeNCl)2 molecule in which the tellurium atoms are linked by the nitrogen atoms to give a planar Te2N2 four-membered ring. One of the nitrogen atoms is coordinated by a TeCl3+ unit, the other one by an antimony pentachloride molecule. According to the IR spectra a structure like [Te2N2Cl2(TeCl4)2] is proposed for Te2NCl5.
    Notes: Die Titelverbindung wird durch Reaktion von Te2NCl5 mit Antimonpentachlorid in Dichlormethan hergestellt und durch das IR-Spektrum und eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, Gitterkonstanten bei -70°C: a = 1535,6; b = 1259,5; c = 1572,4 pm, β = 109,30°; R = 0,031. Die Verbindung bildet ein Ionenpaar, dessen Kation als zentrales Bauelement ein (TeNCl)2-Molekül enthält, in dem die Telluratome mit den Stickstoffatomen zu einem planaren Te2N2-Vierring verknüpft sind. Eines der N-Atome ist mit einem TeCl3+-Ion, das andere mit einem SbCl5-Molekül koordiniert. Aus dem Vergleich der IR-Spektren wird für Te2NCl5 eine Struktur gemäß [Te2N2Cl2(TeCl4)2] vorgeschlagen.
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  • 9
    ISSN: 0044-2313
    Keywords: Silylated λ5-Phosphazenes ; Synthesis ; NMR spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of the Silylated λ5-Phosphazenes R—C(CH2PPh2NSiMe3)3 with R = H and CH3The title compounds are obtained by Staudinger reaction from the corresponding tripodal phosphanes R—C(CH2PPh2)3 and trimethylsilylazide. Both complexes are characterized by their IR and NMR spectra and by crystal structure analyses.H—C(CH2PPh2NSiMe3)3 (1): Space group P21/c, Z = 4, structure determination with 7833 independent reflections, R = 0.055. Lattice dimensions at -50°C: a = 1399.5, b = 2311.4, c = 1678.9 pm, β = 112.92°.CH3—C(CH2PPh2NSiMe3)3 (2): Space group P1, Z = 2, structure determination with 9251 independent reflections, R = 0.057. Lattice dimensions at -50°C: a = 1276.5, b = 1386.9, c = 1790.2 pm; α = 85.55°, β = 69.39°, γ = 62.99°.1 and 2 form monomeric molecules which are distinguished by their conformation.
    Notes: Die Titelverbindungen werden durch Staudinger-Reaktion aus den entsprechenden tripodalen Phosphanen R—C(CH2PPh2)3 und Trimethylsilylazid hergestellt und durch ihre IR- und NMR-Spektren sowie durch Kristallstrukturanalysen charakterisiert.H—C(CH2PPh2NSiMe3)3 (1): Raumgruppe P21/c, Z = 4, Strukturbestimmung mit 7833 unabhängigen Reflexen, R = 0,055. Gitterkonstanten bei -50°C: a = 1399,5; b = 2311,4; c = 1678,9 pm; β = 112,92°.CH3—C(CH2PPh2NSiMe3)3 (2): Raumgruppe P1, Z = 2, Strukturbestimmung mit 9251 unabhängigen Reflexen, R = 0,057. Gitterkonstanten bei -50°C: a = 1276,5; b = 1386,9; c = 1790,2 pm; α = 85,55°; β = 69,39°; γ = 62,99°.1 und 2 bilden monomere Moleküle, die sich durch ihre Konformation unterscheiden.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 224-230 
    ISSN: 0044-2313
    Keywords: Zirconium ; Hafnium ; Phosphaneiminato Complexes ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphoraneiminato Complexes of Zirconium and Hafnium with Clusterlike StructuresThe tetrachlorides of zirconium and hafnium react with excess phosphaneimine Me3SiNPMe3 at 220°C in the presence of sodium fluoride by cleaving FSiMe3 to form the ionic complexes [Zr3Cl6(NPMe3)5]+[Zr2Cl6(NPMe3)3]- and [Hf3Cl6(NPMe3)5]+[Hf2Cl7(NPMe3)2]-. According to crystal structure analyses in the cations the three metal atoms together with three μ2-NPMe3- groups and two NPMe3- groups with μ3-function are forming trigonal bipyramids. In the anion of the zirconium complex the Zr atoms are linked by three μ2-N bridges, whereas in the anion of the hafnium compound bridging is effected by two μ2-N bridges and one μ2-Cl bridge. Primary products in the reaction of MCl4 (M = Zr, Hf) with silylated phosphaneimines are donor-acceptor complexes like [ZrCl4(Me3SiNPPh3)] which has been characterized crystallographically as an example. In the molecular complex the Zr-atom is coordinated in a trigonal bipyramidal fashion.
    Notes: Die Tetrachloride von Zirconium und Hafnium reagieren mit überschüssigem Phosphanimin Me3SiNPMe3 bei 220°C in Gegenwart von Natriumfluorid unter Abspaltung von FSiMe3 und Bildung der komplexen Ionenverbindungen [Zr3Cl6(NPMe3)5]+[Zr2Cl6(NPMe3)3]- und [Hf3Cl6(NPMe3)5]+[Hf2Cl7(NPMe3)2]-. Nach Kristallstrukturanalysen bilden in den Kationen die drei Metallatome zusammen mit drei NPMe3--Gruppen mit μ2-N-Funktion und zwei NPMe3--Gruppen mit μ3-N-Funktion trigonale Bipyramiden. Im Anion des Zirconium-Komplexes sind die Zr-Atome über drei μ2-N-Brücken verknüpft, während im Anion der Hafnium-Verbindung die Hf-Atome über zwei μ2-N-Brücken und eine μ2-Cl-Brücke verbunden sind. Primärprodukte bei der Reaktion von MCl4 (M = Zr, Hf) mit silylierten Phosphaniminen sind Donor-Akzeptor-Komplexe, von denen das Beispiel [ZrCl4(Me3SiNPPh3)] kristallographisch charakterisiert wurde. In dem Molekül-Komplex ist das Zr-Atom trigonal-bipyramidal koordiniert.
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