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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 592 (1991), S. 42-50 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of In(CH2Ph)3The reaction of InCl3 with PhCH2MgCl forms tribenzylindane 1, precipitating from toluene as pale yellow crystals. The crystal structure shows one dimensional chains of 1 in a zigzag arrangement. The synthesis and characterization of (PhCH2)2InCl 2 and PhCH2InCl2 3 is reported.
    Notes: Die Umsetzung von InCl3 mit PhCH2MgCl ergibt Tribenzylindan 1, welches in Form blaßgelber Kristalle aus Toluol isoliert werden kann. Die Kristallstruktur zeigt gewinkelte eindimensionale Ketten von 1. Über die Synthese und Charakterisierung von (PhCH2)2InCl 2 und PhCH2InCl2 3 wird berichtet.
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  • 2
    ISSN: 0044-2313
    Keywords: Molybdenum ; Tungsten ; Nitrido Complexes ; Syntheses ; 1H, 13C NMR ; IR Spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Stericly Shielded Nitrido Complexes of Molybdenum and Tungsten. The Crystal Structures of [MoN(NPh2)3] and [W4N4(NPh2)6(OnC4H9)2]The reactions of MoNCl3 and WNCl3, respectively, with lithium diphenylamide in tetrahydrofurane produce the monomeric nitrido complexes MN(NPh2)3 with CN = 4 at the metal atoms. In the presence of lithium-n-butyl LiNPh2 and WNCl3 also form the tetrameric nitrido complex [W4N4(NPh2)6(OnC4H9)2] which contains WV and WVI. The compounds are characterized by their i.r. spectra, by X-ray structural analysis, and, partially, by 1H and 13C n.m.r. spectroscopy.MoN(NPh2)3: Space group P1, Z = 2, 4060 observed independent reflexions, R = 0.031. Lattice dimensions at 20°C: a = 956.2(4) pm, b = 1 015.9(2) pm, c = 1 598.1(3) pm; α = 79.06(2)°, β = 85.67(3)°, γ = 82.57(3)°. The compound forms monomeric molecules with Mo≡N bond lengths of 163.4 pm and mean Mo—NPh2 distances of 199.2 pm.[W4N4(NPh2)6(OnC4H9)2]: Space group P21/n, Z = 2, 1903 observed independent reflexions, R=0.039. Lattice parameters at 19°C: a = 1582.2(3) pm, b = 1182.4(2) pm, c = 2053.3(4) pm; β = 103.77(2)°. The compound forms centrosymmetric molecules, in which the central W-W dumb-bell (bond length 253.5 pm) is linked by the nitrido ligands of two WN2(NPh2)2=units in a T shaped order of the N-atoms.
    Notes: Die Umsetzungen von MoNCl3 bzw. WNCl3 mit Lithium-Diphenylamid in Tetrahydrofuran führen zu den monomeren Nitridokomplexen MN(NPh2)3 mit KZ = 4 an den Metallatomen. Bei Anwesenheit von Lithium-n-butyl reagiert LiNPh2 mit WNCl3 auch zu dem tetrameren, Wolfram(V) und Wolfram(VI) enthaltenden Nitridokomplex [W4N4(NPh2)6(OnC4H9)2]. Die Verbindungen werden durch ihre IR-Spektren, zum Teil durch die 1H- und 13C-Kernresonanzspektren sowie durch Röntgenstrukturanalysen charakterisiert.MoN(NPh2)3: Raumgruppe P1, Z = 2, 4060 unabhängige beobachtete Reflexe, R = 3,1%. Gitterabmessungen bei 20°C: a = 956,2(4); b = 1015,9(2); c = 1598,1(3) pm; α = 79,06(2)°; β = 85,67(3)°; γ = 82,57(3)°. Die Verbindung bildet monomere Moleküle mit Bindungslängen Mo≡N 163,4 pm und Mo—NPh2 von im Mittel 199,2 pm.[W4N4(NPh2)6(OnC4H9)2]: Raumgruppe P21/n, Z = 2, 1903 beobachtete unabhängige Reflexe, R = 3,9%. Gitterabmessungen bei 19°C: a = 1 582,2(3); b = 1 182,4(2); c = 2 053,3(4) pm; β = 103,77(2)°. Die Verbindung bildet zentrosymmetrische Moleküle, deren zentrale W - W-Hantel (Bindungslänge 253,5 pm) über die Nitridoliganden zweier WN2(NPh2)2-Einheiten mit T-förmiger Anordnung der N-Atome verknüpft ist.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 121 (1988), S. 2071-2073 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The He(I) photoelectron (PE) spectra of the diphosphacyclobutadienes 2 and 3 have been recorded. The interpretation of the first PE bands is based on SCF-MO calculations (MNDO method). It is found that the first two bands correspond to π-MOs which are mainly localized in the four-membered ring. The first two bands are shifted towards higher energy in the PE spectrum of 3; we ascribe this to an electron transfer from the four-membered ring in 3 to the phenyl substituents.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 2283-2287 
    ISSN: 0009-2940
    Keywords: Indium, trialkyl derivatives ; Dialkylchloroindium ; Alkyldichloroindium ; Alkylindium dialkylamides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Properties of iPr2InCl, iPrInCl2, and (iPr2InHRtBu)2The reactions of triisopropylindium (1) with half an equivalent or two equivalents of indium (III) chloride leads to iPr2InCl (2) and iPrInCl2 (3), respectively. (iPr2InNHtBu)2 (4) can be synthesized from 2 and LiNHtBu. According to NMR, IR, and RE studies, 2-4 from dimers in solution and solid state. The X-ray analysis of 4 is reported.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 11-15 
    ISSN: 0009-2940
    Keywords: Indium compounds ; Indate, tetrafluorenyl ; Indate, chlorotrifluorenyl ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fluorenylindates: Compounds with Weak In  -  C BondsIn diethyl ether, fluorenyllithium reacts with indium(III) chloride to yield a lithium tetrafluorenylindate (1). Recrystallisation from THF gives [Li(THF)4][In(C13H9)4] (2). If the reaction is carried out in THF, the chlorotrifluorenylindate [Li(THF)4]-[ClIn(C13H9)3] (3) is isolated. According to crystal structure analyses 2 has long and weak In  -  C bonds [224.8(5) - 230.3(5) pm], while these distances in 3 are somewhat shorter [222.9 (5) - 226.7(4) pm].
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  • 6
    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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  • 7
    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).
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 1579-1585 
    ISSN: 0009-2940
    Keywords: Gallium compounds ; Gallane, tribenzyl- ; Gallane, dibenzyl(benzyloxy)- ; Gallate, dibenzyldifluoro- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Benzylgallium Compounds. Coordination of Benzyl Ligands in Cs[(PhCH2)2GaF2]Dissolving (PhCH2)3Ga (1) in THF yields the complex [(PhCH2)3Ga · THF] (2). Reaction of 1 with dry oxygen in toluene at -78°C leads to [(PhCH2)2GaOCH2Ph]2 (3), which is also formed from 1 and PhCH2OH. The salts K[(PhCH2)2GaF2] (5) and Cs[(PhCH2)2GaF2] (6) were obtained from (PhCH2)2GaCl (4) and KF or CsF, respectively, in acetonitrile. Crystal structures were determined for 2, 3, 6 and {[(PhCH2)2GaCl]2 · toluene} (7). Gallane 2 is a chiral monomeric complex in the solid state. The benzyl substituents create a propeller-shaped molecule with a counterclock-wise orientation of the ligands. 3 and 7 are crystallizing as centrosymmetrical dimers with Ga2X2 rings (X=O, Cl). 6 consists in infinite chains of {Cs[(PhCH2)2GaF2]}2 units with Cs-F contacts. In addition to the Cs-F interaction, the coordination of each Cs+ ion by two phenyl rings in a η6- fashion is observed.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 67-71 
    ISSN: 0009-2940
    Keywords: Gallium compounds ; Heterocubanes, gallium-phosphorus ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Characterization of Gallium-Phosphorus HeterocubanesThe reaction of iPrGaCl2 with tBuPLi2 in Et2O at -78°C gives the heterocubane [iPrGaP(tBu)]4 (1) by using the “dilution principle”. {(MesGa)3[GaP(H)tBu][P(tBu)]4} (2) was formed, when three equivalents of MesGaCl2 and one equivalent of GaCl3 in THF at -78°C were treated with 5 equivalents of tBuPLi2. Compounds 1 and 2 were characterized by NMR, IR, and MS techniques as well as by X-ray structure determination. The heterocubane molecules of 1 are disordered in the crystal; every atom site of the central cubical frame work is occupied by gallium and phosphorus atoms (occupation factor 0.5). The structure of 2 contains two crystallographically unique molecules, which are not disordered because of the additional P(H)tBu groups.
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  • 10
    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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