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  • Crystal Structures  (6)
  • Gallium compounds  (3)
  • syntheses  (3)
  • Diorganogallium fluorides  (2)
  • X-ray structures  (2)
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  • 1
    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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  • 2
    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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  • 3
    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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  • 4
    Electronic Resource
    Electronic Resource
    Cäsium-Fluor-Vierringe als Strukturmotiv in Cäsium-Triorganofluorometallaten der Gruppe 13Herrn Prof. Dr. Ekkehard Fluck zum 65. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 355-359 
    Details
    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.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290317
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  • 5
    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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  • 6
    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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  • 7
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Komplexe des 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphetsFrau Professor Marianne Baudler zum 75. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 942-950 
    Details
    ISSN: 0044-2313
    Keywords: 1λ5,3λ5-diphosphete ; iron, chromium, tungsten complexes ; nmr, mass, ir spectra ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Complexes of 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-Diphosphete1,1,3,3-Tetrakis(dimethylamino)-1λ5,3aλ5-diphosphete, 1, reacts with W(CO)6 to yield the isomeric complexes {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)tungsten 4 and {1,1,3,3-tetrakis(dimethylamino)-1,4-dihydro-1λ5,3λ5-[1,3]diphosphetium}(pentacarbonyl)tungsten 5. With Cr(CO)6 the complex {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)chromium 6 is formed. From the reaction products of Fe3(CO)12 and Fe2(CO)9 with 1 the complex {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)iron 7 could be isolated. Properties, nmr, ir and mass spectra of the new compounds are reported. 6 and 7 were characterized by X-ray structure determinations.
    Notes: 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet, 1, reagiert mit W(CO)6 zu den isomeren Komplexen {1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet}(pentacarbonyl)wolfram 4 und {1,1,3,3-Tetrakis(dimethylamino)-1,4-dihydro-1λ5,3λ5-[1,3]diphosphetium}(pentacarbonyl)wolfram 5, mit Cr(CO)6 zu dem Komplex {1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet}(pentacarbonyl)chrom 6. Aus den Reaktionsprodukten von Fe3(CO)12 und Fe2(CO)9 mit 1 konnte der Komplex {1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet}(pentacarbonyl)eisen 7 isoliert werden. Eigenschaften, NMR-, IR- und Massenspektren der neuen Verbindungen werden mitgeteilt. 6 und 7 wurden zusätzlich durch Kristallstrukturanalysen charakterisiert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220605
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  • 8
    Electronic Resource
    Electronic Resource
    Diorganogalliumfluoride. Die Kristallstruktur des Mischkristalls [B(CH2Ph)3]0,92[Ga(CH2Ph)3]0,08 · NCMe (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 123-129 
    Details
    ISSN: 0044-2313
    Keywords: Diorganogallium fluorides ; tribenzylbor-tribenzylgallium-acetonitril mixed crystal ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Diorganogallium Fluorides. The Crystal Structure of the Mixed Crystal [B(CH2Ph)3]0.92[Ga(CH2Ph)3]0.08 · NCMeThe reaction of GaR3 with BF3 · OEt2 in diethylether leads to the diorganogallium fluorides R2GaF [R = i-Pr (1), CH2Ph (2), Mes (3)]. Compound 1 is also available by the reaction of i-Pr2GaBr (6) with KF at -20°C in acetonitrile. The by-product B(CH2Ph)3, formed together with 2 during the first reaction, crystallizes with ca. 8% Ga(CH2Ph)3 in acetonitrile as [B(CH2Ph)3]0.92[Ga(CH2Ph)3]0.08 · NCMe (4) in the space group P21/n with a = 1050.32(7) pm, b = 1159.5(2) pm, c = 1591.6(1) pm and β = 96.931(6)°.
    Notes: Die Reaktion von GaR3 mit BF3 · OEt2 in Diethylether führt zu den Diorganogalliumfluoriden R2GaF [R = i-Pr (1), CH2Ph (2), Mes (3)]. 1 kann eben-so über die Umsetzung von i-Pr2GaBr (6) mit KF bei -20°C in Acetonitril dargestellt werden. Das bei der Synthese von 2 nach dem ersten Weg anfallende B(CH2Ph)3 kristallisiert mit ca. 8% Ga(CH2Ph)3 aus Acetonitril in Form von [B(CH2Ph)3]0,92[Ga(CH2Ph)3]0,08 · NCMe (4) in der Raumgruppe P21/n mit a = 1050,32(7) pm, b = 1159,5(2) pm, c = 1591,6(1) pm und β = 96,931(6)°.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926120121
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  • 9
    Electronic Resource
    Electronic Resource
    [Sb(12-Krone-4)2(CH3CN)][SbCl6]3 und [Bi(12-Krone-4)2(CH3CN)][SbCl6]3, die ersten Trikationen von Antimon(III) und Bismut(III)Professor Hartmut Bärnighausen zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 271-276 
    Details
    ISSN: 0044-2313
    Keywords: Crown ether complexes of Sb3+ and Bi3+ ; synthesis ; IR spectra ; 121Sb Mössbauer spectrum ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Sb(12-Crown-4)2(CH3CN)][SbCl6]3 and [Bi(12-Crown-4)2(CH3CN)][SbCl6]3, first Trications of Antimony(III) and Bismuth(III)The crown ether complexes [M(12-crown-4)2(CH3CN)][SbCl6]3 with M = Sb and Bi are formed by the reaction of antimony trichloride and bismuth trichloride, respectively, with antimony pentachloride in acetonitrile solution in the presence of 12-crown-4. They form colourless, moisture sensitive crystals, which were characterized by X-ray structure determinations and by IR spectroscopy. The complex with M = Sb was also characterized by 121Sb Mössbauer spectroscopy.Both complexes crystallize isotypically in the orthorhombic space group Pbcn with four formula units per unit cell.M = Sb: 3 483 observed unique reflections, R = 0.038. M = Bi: 2 958 observed unique reflections, R = 0.036. The compounds consist of SbCl6- ions and trications [M(12-crown-4)2(CH3CN)]3+, in which the M3+ ions are ninefold coordinated by the eight oxygen atoms of the crown ether molecules and by the nitrogen atom of the acetonitrile molecule. The lone pair of the M3+ ions has no steric effect.
    Notes: Die Kronenetherkomplexe [M(12-Krone-4)2(CH3CN)][SbCl6]3 mit M = Sb und Bi entstehen durch Reaktion von Antimontrichlorid bzw. Bismuttrichlorid mit Antimonpentachlorid in Acetonitrillösung in Gegenwart von 12-Krone-4. Sie bilden farblose, feuchtigkeitsempfindliche Kristalle, die wir durch kristallographische Strukturanalysen und durch die IR-Spektren charakterisiert haben. Von dem Komplex mit M = Sb wurde ein 121Sb-Mößbauer-Spektrum aufgenommen.Beide Komplexe kristallisieren isotyp in der orthorhombischen Raumgruppe Pbcn mit vier Formeleinheiten pro Elementarzelle. M = Sb: 3 483 beobachtete unabhängige Reflexe, R = 0,038. M = Bi: 2 958 beobachtete unabhängige Reflexe, R = 0,036. Die Verbindungen enthalten neben den SbCl6--Ionen Trikationen [M(12-Krone-4)2(CH3CN)]3+, in denen die M3+-Ionen durch die acht O-Atome der beiden Kronenethermoleküle und durch das N-Atom des Acetonitrilmoleküls neunfach koordiniert sind. Das freie Elektronenpaar an den M3+-Ionen bleibt ohne sterische Wirksamkeit.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190208
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  • 10
    Electronic Resource
    Electronic Resource
    Mesityltrifluorogallate. Die Kristallstrukturen von Cs[MesGaF3] und K[MesInBr3] (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1897-1904 
    Details
    ISSN: 0044-2313
    Keywords: Mesityltrifluoro gallates ; mesitylbromo indates ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mesityltrifluoro Gallates. The Crystal Structures of Cs[MesGaF3] and K[MesInBr3]Mes3Ga reacts with GaBr3 in the ratio 1:2 in a commutation reaction to MesGaBr2 (1). 1 can be reacted with KF and CsF in MeCN to K[MesGaF3] (2) and Cs[MesGaF3] (3), respectively. K[MesInBr3] (4) was isolated when MesInBr2 was treated with KF in MeCN. The use of 15-crown-5 was leading to [K(15-crown-5)2][Mes2InBr2] (5) in a substituent exchange reaction. 1-5 were characterized by NMR-, IR- and MS-techniques. The solid state structures of 3 and 4 could be established by X-ray structure determinations. According to these determinations, a layer-type arrangement of the molecules is both structures in common. In the center of the layers, ionic interactions were formed, while the separation of the layers is caused by the bulky mesityl substituents.
    Notes: Mes3Ga reagiert mit GaBr3 im Verhält-nis 1:2 in einer Kommutierungsreaktion zu MesGaBr2 (1). 1 kann mit KF bzw. CsF in MeCN zu K[MesGaF3] (2) bzw. Cs[MesGaF3] (3) umgesetzt werden. Dagegen konnte bei der Reaktion von MesInBr2 mit KF in MeCN nur K[MesInBr3] (4) isoliert werden. Der Einsatz von 15-Krone-5 führt nach einer Substituentenaustauschreaktion zu [K(15-Krone-5)2][Mes2InBr2] (5). 1-5 wurden mittels NMR- und IR-Spektroskopie sowie Massenspektrometrie charakterisiert. Die Festkörperstrukturen von 3 und 4 konnten mit Röntgenstrukturanalysen aufgeklärt werden.Danach ist beiden Verbindungen ein schichtartiger Aufbau gemeinsam, wobei im Zentrum der Schichten die interionischen Wechselwirkungen ausgebildet werden. Die Separation der Schichten folgt aus der abschirmenden Wirkung der Mesitylgruppen an der Oberfläche der Schichten.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936191113
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