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  • Chemistry  (29)
  • 121Sb Mössbauer spectrum  (1)
  • IR Spectra
  • 1990-1994  (29)
  • 1
    Electronic Resource
    Electronic Resource
    Die Kristallstruktur von In(CH2Ph)3Professor Ekkehard Fluck zum 60. Geburtstag am 27. Februar 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 592 (1991), S. 42-50 
    Details
    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.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915920105
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  • 2
    Electronic Resource
    Electronic Resource
    Sterisch abgeschirmte Nitridokomplexe von Molybdän und Wolfram Die Kristallstrukturen von [MoN(NPh2)3] und [W4N4(NPh2)6(OnC4H9)2]Professor Josef Goubeau in memoriam (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 593 (1991), S. 99-110 
    Details
    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.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915930110
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  • 3
    Electronic Resource
    Electronic Resource
    Fluorenylindate: Verbindungen mit schwachen In  -  C-Bindungen (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 11-15 
    Details
    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].
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260103
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  • 4
    Electronic Resource
    Electronic Resource
    Benzylgalliumverbindungen. Koordination von Benzylliganden in Cs[(PhCH2)2GaF2] (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 1579-1585 
    Details
    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.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260712
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  • 5
    Electronic Resource
    Electronic Resource
    Synthese und Charakterisierung von Gallium-Phosphor-Heterocubanen (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 67-71 
    Details
    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.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941270110
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  • 6
    Electronic Resource
    Electronic Resource
    [SbCl([15]Krone-5)](SbCl6)2 und [BiCI([18]Krone-6)(CH3CN)2](SbCl6)2: Salze mit Antimon(III)- und Bismut(III)-DikationenProfessor Wolfgang Beck zum 60. Geburtstag gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für die chemische Industrie 104 (1992), S. 354-356 
    Details
    ISSN: 0044-8249
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/ange.19921040336
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  • 7
    Electronic Resource
    Electronic Resource
    Synthesen und Kristallstrukturen der Polytellurido-Komplexe [K(15-Krone-5)2]2[MTe7] mit M = Zn und Hg (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 500-506 
    Details
    ISSN: 0044-2313
    Keywords: Polytellurido Complexes of Zinc and Mercury ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of the Polyellurido Complexes [K(15-Crown-5)2]2[MTe7] with M = Zn and HgThe title compounds were obtained in the presence of 15-crown 5 from solutions of zinc and mercury acetate, respectively, in DMF by addition of a solution of K2Te3 in DMF at 0°C (M = Zn) and -50°C (M = Hg). They form black crystal needles with metallic luster. Their crystal structures were determined by X-ray diffraction. The structures of [K(15-crown-5)2]2ZnTe7 and [K(15-crown-5)2]2HgTe7 show two-dimensional disorder as evidence by diffuse scattering. The averaged structures that were determined with the Bragg reflexions correspond to space group Pbcn and have very similar lattice parameters. Nevertheless, the structures differ. [HgTe7]2- ions consist of two condensed five membered rings. They are arranged to form strands in the c direction; within of one strand the ions have a definite orientation, but in different strands two different orientations occur randomly. A [ZnTe7]2- ion can be thought of consisting of a Zn2+ ion, a Te42- ion bonded in a chelate manner and a Te32- ion bonded with one terminal Te atom to the Zn2+. The [ZnTe7]2- ions are associated to strands in the c direction with two different strand orientations occuring randomly.
    Notes: Die Titelverbindungen entstehen aus Lösungen der Acetate von Zink bzw. Quecksilber in DMF bei Anwesenheit von 15-Krone-5 nach Zugabe einer Lösung von K2Te3 in DMF bei 0°C (M = Zn) bzw. -50°C (M = Hg). Die Verbindungen bilden schwarze, metallisch glänzende Kristallnadeln, die wir durch röntgenographische Strukturanalysen charakterisiert haben. Die Kristallstrukturen von [K(15-Krone-5)2]2[ZnTe7] und [K(15-Krone-5)2]2[HgTe7] sind zweidimensional fehlgeordnet, wie die entsprechende diffuse Streuung zeigt. Die Überlagerungsstrukturen, die mit Hilfe der Braggschen Reflexe bestimmt wurden, entsprechen bei beiden Verbindungen der Raumgruppe Pbcn bei sehr Ähnlichen Gitterparametern. Trotzdem unterscheiden sich die Strukturen. Die [HgTe7]2--Ionen bestehen aus zwei kondensierten Fünferringen. Sie sind zu Strängen längs c angeordnet, wobei sie innerhalb eines Stranges eine definierte Orientierung haben, aber von Strang zu Strang eine von zwei entgegengesetzten Orientierungen statistisch vorkommt. Ein [ZnTe7]2--Ion kann man sich aufgebaut denken aus einem Zn2+-Ion, einem chelatartig gebundenen Te42--Ion und einem Te32--Ion, das über ein terminales Te-Atom an das Zn2+ gebunden ist. Die [ZnTe7]2--Ionen sind zu Strängen längs c assoziiert, wobei statistisch zwei Strangorientierungen vorkommen.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190311
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  • 8
    Electronic Resource
    Electronic Resource
    Einbau von Metallfluoriden in Organoindiumfluoride (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 718-726 
    Details
    ISSN: 0044-2313
    Keywords: Organoindium fluorides ; organoindium fluoride cesium fluoride complexes ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Insertion of Metal Fluorides in Organoindium Fluorides.The reaction of i-Pr2InCl (1) with CsF in acetonitrile at room temperature yields [(i-Pr2InF)5(CsF · 2 MeCN)] ([2 · 2 MeCN]). {[(MesInF2)10MgF2] · 5 toluene} ({3 · 5 toluene}) can be isolated as a by-product in the reaction of Mes3In with BF3 · OEt2 in the presence of MgBrCl. [2 · 2 MeCN] and {3 · 5 toluene} were characterized by NMR spectroscopy as well as by X-ray structure determinations. [2 · 2 MeCN] forms infinite double chains of (i-Pr2InF)5-blocks and CsF-units. The coordination sphere of the cesium atom consists of three fluorine atoms and the nitrogen atoms of three acetonitrile molecules, which wrap the metal atom in a strongly distorted octahedral fashion. One of the acetonitrile molecules in [2 · 2 MeCN] has a μ2-bridging function. This results in the formation of four membered Cs2N2-rings.In {3 · 5 toluene}, ten molecules of MesInF2 are forming a cage in which a linear MgF2-unit is inserted.
    Notes: Die Reaktion von i-Pr2InCl (1) mit CsF in Acetonitril bei Raumtemperatur führt zu [(i-Pr2InF)5(CsF · 2 MeCN)] ([2 · 2 MeCN]).{[(MesInF2)10MgF2] · 5 Toluol} ({3 · 5 Toluol}) kann als Nebenprodukt bei der Umsetzung von Mes3In mit BF3 · OEt2 in der Gegenwart von MgBrCl erhalten werden. [2 · 2 MeCN] und {3 · 5 Toluol} wurden mittels NMR-Methoden sowie durch Röntgenstrukturanalysen charakterisiert. [2 · 2 MeCN] bildet unendliche Doppelstränge aus (i-Pr2InF)5-Blöcken und CsF-Einheiten. Die Koordinationssphäre des Cs-Atoms besteht aus drei F-Atomen und den N-Atomen von drei Acetonitril-Molekülen, was zu einer stark verzerrt oktaedrischen Umgebung des Metallatoms führt. Eines der Acetonitril-Moleküle in [2 · 2 MeCN] hat eine μ2-verbrückende Funktion, woraus sich die Ausbildung von Cs2N2-Vierringen ergibt.In {3 · 5 Toluol} wird ein Käfig aus zehn MesInF2-Einheiten geformt, in welchem eine lineare MgF2-Einheit eingelagert ist.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190414
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  • 9
    Electronic Resource
    Electronic Resource
    Darstellung und Charakterisierung von Organodilithiumphosphiden. Die Kristallstruktur von [Li(THF)(TMEDA)P(H)Mes] (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 885-888 
    Details
    ISSN: 0044-2313
    Keywords: Organodilithium phosphides ; organolithium phosphide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Characterization of Organodilithium Phosphides. The Crystal Structure of [Li(THF)(TMEDA)P(H)Mes]t-BuPH2 and MesPH2 can be reacted with two equivalents n-BuLi at R. T. in Et2O/n-hexane to yield the corresponding organodilithium phosphides t-BuPLi2 (1) and MesPLi2 (2). 1 and 2 can be isolated solvent-free as bright orange-yellow solids. 1 and 2 were characterized by NMR, IR, and RE spectra. When MesPH2 is treated with one equivalent of n-BuLi, MesP(H)Li is crystallizing as [Li(THF)(TMEDA)P(H)Mes] (3) from THF/TMEDA/n-pentane in the space group P21/n with a = 893.41(6), b = 1 734.7(1), c = 1 391.1(1) pm and β = 90.613(6)°.
    Notes: t-BuPH2 und MesPH2 werden bei Zimmertemperatur in Et2O/n-Hexan mit zwei äquivalenten n-BuLi zu den entsprechenden Organodilithiumphosphiden t-BuPLi2 (1) und MesPLi2 (2) umgesetzt. 1 und 2 können lösungsmittelfrei als leuchtend orange-gelbe Festkörper isoliert werden. 1 und 2 wurden mittels NMR-, IR- und RE-Spektren charakterisiert. Wird MesPH2 mit nur einem äquivalent n-BuLi behandelt, kristallisiert MesP(H)Li in Form von [Li(THF)(TMEDA)P(H)Mes] (3) aus THF/TMEDA/n-Pentan in der Raumgruppe P21/n mit a = 893,41(6), b = 1 734,7(1), c = 1 391,1(1) pm und β = 90,613(6)°.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190513
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  • 10
    Electronic Resource
    Electronic Resource
    Diorganoindium-Kationen. Die Kristallstruktur von [Mes2In][BF4] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 847-850 
    Details
    ISSN: 0044-2313
    Keywords: Diorganoindium cations ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Diorganoindium Cations. The Crystal Structure of [Mes2In][BF4](PhCH3)2In and Mes3In react with BF3 · OEt2 in a ratio of 3:4 at 80°C in toluene to the corresponding salts [R2In][BF4] [R = PhCH2 (1), Mes (2)]. The same results could be obtained, when the diorganoindium fluorides (PhCH2)2InF and Mes2InF were treated with BF3 · OEt2 at 80°C in toluene. 1 und 2 were characterized by NMR-, IR- und MS-techniques. The arrangement of the ions in 2 could be established by an X-ray structure determination. The cations and anions of 2 are forming infinite chains. The metal centers are coordinated by two BF4--ions, so that every In atom possesses a distorted octahedral coordination sphere.
    Notes: (PhCH2)3In und Mes3In reagieren mit BF3 · OEt2 im Verhältnis 3:4 bei 80°C in Toluol zu den entsprechenden Salzen [R2In][BF4] [R = PhCH2 (1), Mes (2)]. Zum selben Ergebnis gelangt man, wenn die Diorganoindiumfluoride (PhCH2)2InF und Mes2InF mit BF3 · OEt2 bei 80°C in Toluol behandelt werden. 1 und 2 wurden mittels NMR- und IR-Spektroskopie sowie Massenspektrometrie charakterisiert. Die Anordnung der Ionen in 2 konnte durch eine Röntgenstrukturanalyse aufgeklärt werden. 2 bildet danach unendliche Ketten aus Kationen und Anionen, wobei durch eine chelatartige Anordnung zweier BF4--Ionen an jedes Metallzentrum eine verzerrt oktaedrische Koordinationssphäre der Indiumatome resultiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200516
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