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  • Inorganic Chemistry  (18)
  • Phosphoraneiminato Complexes  (2)
  • IR spectra
  • 1995-1999  (18)
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Year
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 253-257 
    ISSN: 0009-2940
    Keywords: Lithiated phosphane imines ; Phosphane imines, lithiated ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Lithiated Phosphane Imines. Synthesis and Crystal Structures of [LiCH2PMe2NSiMe3]4 and [LiCMe2P(iPr)2NSiMe3]2The title compounds were prepared by the reaction of Me3-SiNPMe3 and Me3SiNP(iPr)3, respectively, with n-Butylli-thium at 20°C in n-hexane solution. They form white, moisture- and oxygen-sensitive crystals, which were characterized by IR spectroscopy and by crystal structure determinations. - [LiCH2PMe2NSiMe3]4 (1) forms a Li4 tetrahedron, the faces of which are capped with CH2 groups with average Li-C distances of 233 and 251 pm, while the nitrogen atoms occupy the corners of the Li4 tetrahedron. - [LiCMe2P(iPr)2N-SiMe3]2 (2) forms molecules of symmetry C2 in which the lithium atoms have coordination number three by two carbon atoms and one nitrogen atom with Li-C distances of 215.2 and 237.9 pm and Li-N of 192.8 pm.
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  • 2
    ISSN: 0009-2940
    Keywords: Amido complexes ; Titanium(III) compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Syntheses, Properties, and Crystal Structures of the Titanium(III) Amido Complexes Ti[N(SiMe3)2]3, [TiCl2{N(SiMe3)2}(THF)2], and [Na(12-Crown-4)2][TiCl2{N(SiMe3)2}2]TiCl3(THF)3 reacts with NaN(SiMe3)2 to furnish [TiCl2{N(SiMe3)2}(THF)2] (1), whereas in the presence of 12-crown-4 the ionic amido complex [Na(12-crown-4)2][TiCl2{N(SiMe3)2}2] (5) is obtained besides [Na(12-crown-4)2][TiCl4(THF)] (4). On the other hand, the titanium(III) amido complex Ti[N(SiMe3)2]3 (2), the crystal structure of which was solved, reacts with NaN(SiMe3)2 in the presence of 12-crown-4 with deprotonation of one of the methyl groups to give the carbometalated complex [Na(12-crown-4)2][Ti{N(SiMe3)2}2{N(SiMe 3CH2)}] (3).
    Additional Material: 4 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 355-359 
    ISSN: 0009-2940
    Keywords: Aluminium compounds ; Gallium compounds ; Indium compounds ; Trimethylfluoro metalates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cesium-Fluorine Four-Membered Rings as Structural Motive in Cesium Triorganofluoro Metalates of Group 13The reactions of AlMe3, GaMe3, and InMe3 with CsF in acetonitrile furnish the corresponding trimethylfluoro metalates Cs[Me3MF] (1: M = Al, 2: M = Ga, 3: M = In). The salt-like compounds 1 - 3 were characterized by NMR, IR, and MS techniques as well as by X-ray structure analysis. Cs2F2 four-membered rings are the structure-dominating units in all three compounds. Compound 1 consists of puckered layers of weakly associated Cs2F2 rings parallel to (100), while the four-membered rings in 2 form infinite ladder-type chains. The Cs-F rings in 3 build up a heterocubane with a Cs4F4 core by ring stacking.
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  • 4
    ISSN: 0009-2940
    Keywords: Amido Complexes ; Manganese Compounds ; Iron Compounds ; Cobalt Compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Syntheses and Crystal Structures of the Amido Complexes [Na(12-Crown-4)2][M{N(SiMe3)2}3] with M = Mn, Fe, and CoThe ionic amido complexes [Na(12-crown-4)2][M[N-(SiMe3)2}3] with M = Mn (1), Fe (2) and Co (3) were prepared by the reaction of M[N(SiMe3)2]2 (M = Mn, Co) and Fe[N-(SiMe3)2]3, respectively, with sodium bis(trimethylsilyl)amide in toluene solution in the presence of 12-crown-4. 1-3 were characterized by IR spectroscopy and by crystal structure determinations. The complexes consist of cations [Na(12-crown-4)2]+ with a sandwich-like structure and anions [M{N(SiMe3)2}3]- in which the metal atoms are planarly coordinate by the three nitrogen atoms of the bis(trimethylsilyl)amido groups.
    Additional Material: 3 Ill.
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  • 5
    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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  • 6
    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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  • 7
    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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  • 8
    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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  • 9
    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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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 176-176 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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