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  • crystal structures  (5)
  • Gallium compounds  (3)
  • 121Sb Mössbauer spectrum  (1)
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  • 1
    Electronic Resource
    Electronic Resource
    Difluorenylzink als Alkylierungsmittel zur Darstellung von Triorganometallanen der 13. Gruppe. Synthese und Kristallstruktur von [GaFl3(THF)] · Toluol (Fl = Fluorenyl) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 394-402 
    Details
    ISSN: 0044-2313
    Keywords: Zinc complexes ; organogallium compound ; indium complexes ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Difluorenyl Zinc as Alkylation Reagent in Formation of Triorgano Metallanes of Group 13. Synthesis and Crystal Structure of [GaFl3(THF)] · Toluol (Fl = Fluorenyl)Difluorenyl zinc (fluorenyl = Fl) gives with AlCl3 in THF the salt [AlCl2(THF)4][ZnCl3(THF)] (1) while the corresponding reaction with GaCl3 leads to the THF stabilized gallane [GaFl3(THF)] (2). As a result of the reactions of InCl3 and TlCl3 by the mentioned way above only the complex [InCl3(THF)3] (3) could be isolated. The mixture of solvents DME/THF gives the complex [InCl3(DME)(THF)] (4). For a comparison of the binding parameters with the zincate ion [ZnCl3(THF)]- the compound [ZnCl2(THF)2] (5) has been synthesized. 1-5 were characterized by NMR and IR techniques. 1, 2 · toluene, 3 and 5 could also be investigated by X-ray structure analysis. According this, 1 possesses a cation with a linear AlCl2 unit and a zincate ion, which is only sligthly pyramidalisized by the THF ligand. 2 contains also a distorted tetrahedral coordinated metal center. For 3 a meridional arrangement of the THF ligands was found. In 5 the absence of a negative charge leads to a shortening of the bond lengths in comparison to the zincate ion [ZnCl3(THF)]-.
    Notes: Difluorenylzink (Fluorenyl = Fl) ergibt mit AlCl3 in THF das Komplexsalz [AlCl2(THF)4][ZnCl3(THF)] (1), während die gleiche Reaktion mit GaCl3 zum THF-stabilisierten Gallan [GaFl3(THF)] (2) führt. Aus Umsetzungen mit InCl3 und TlCl3 konnte bisher nur der Komplex [InCl3(THF)3] (3) isoliert werden. Das Lösungsmittelgemisch THF/DME liefert den Komplex [InCl3(DME)(THF)] (4). Für einen Bindungslängenvergleich mit dem Zinkat-Ion [ZnCl3(THF)]- wurde der Komplex [ZnCl2(THF)2] (5) dargestellt. 1-5 wurden mittels NMR- und IR-Spektroskopie untersucht. Von 1, 2 · Toluol, 3 und 5 konnte eine Röntgenstrukturanalyse angefertigt werden. 1 besitzt danach ein Kation mit linearer AlCl2-Einheit und ein Zinkat-Ion, das durch den THF-Liganden nur wenig pyramidalisiert ist. In 2 liegt ebenfalls ein verzerrt tetraedrisch koordiniertes Metall-zentrum vor. Für 3 wurde eine meridionale Anordnung der THF-Liganden gefunden. In 5 wirkt sich die Abwesenheit einer Ladung im Vergleich zum Zinkat-Ion [ZnCl3THF]- deutlich bindungsverkürzend aus.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230163
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  • 2
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der Polyselenidokomplexe (PPh4)6[M(Se4)2]2[WSe4] · DMF mit M = Zink und QuecksilberHerrn Prof. Dr. Erhard Uhlemann zum 60. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 12-18 
    Details
    ISSN: 0044-2313
    Keywords: Mixed polyselenido complexes of zinc/tungsten, Mercury/tungsten ; crystal structures ; FIR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Polyselenido Complexes (PPh4)6[M(Se4)2]2[WSe4] · DMF with M = Zinc and MercuryThe title compounds have been prepared by the reactions of the acetates of zinc and mercury, respectively, with excess (PPh4)2 WSe4 in boiling dimethylformamide, forming black-red single crystals. According to the X-ray structure determinations both compounds crystallize isotypically in the space group 12/a with four formula units per unit cell. (PPh4)6[Zn(Se4)2]2[WSe4] · DMF: a = 2888.1(6), b = 1740.3(2), c = 2893.9(4) pm, β = 90.47(1)°. 3230 observed unique reflections, R = 0.009.(PPh4)6[Hg(Se4)2]2[WSe4] · DMF: a = 2891.8(5), b = 1738.0(4), c = 2920.1(5) pm, β = 90.29(2)°. 2978 observed unique reflections, R = 0.115%.The compounds consist of PPh4+ ions, spirocyclic octaseleno metallates [M(Se4)2]2-, tetrahedral WSe42-ions, and disordered DMF Molecules.
    Notes: Die Titelverbindungen entstehen in Form schwarz-roter Einkristalle beim Erhitzen der Acetate von Zink und Quecksilber mit überschüssigem (PPh4)2 WSe4 in Dimethylformamid-Lösungen. Nach den Röntgenstrukturanalysen kristallisieren die Verbindungen isotyp in der Raumgruppe I2/a mit vier Formeleinheiten pro Elementarzelle. (PPh4)6[Zn(Se4)2]2[WSe4]· DMF: a = 2888,1(6), b = 1740,3(2), c = 2893,9(4) pm, β = 90,47(1)°. 3230 beobachtete unabhängige Reflexe, R = 9,9%.(PPh4)6[Hg(Se4)2]2[WSe4] · DMF: a = 2891,8(5), b = 1738,0(4), c = 2920,1(5) pm, β = 90,29(2)°. 2978 beobachtete unabhängige Reflexe, R = 11,5%.Die Verbindungen bestehen aus PPh4 +-Ionen, spirocyclischen Octaselenometallaten [M(Se4)2]2-, tetraedrischen WSe42- Ionen und eingelagerten, fehlgeordneten DMf-Molekülen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090303
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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
    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
    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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  • 6
    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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  • 7
    Electronic Resource
    Electronic Resource
    Darstellung und Eigenschaften von OrganoindiumbromidenProfessor Karl-Heinz Thiele zum 65. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 346-358 
    Details
    ISSN: 0044-2313
    Keywords: Organoindium bromides ; solvate complexes ; trimagnesiumpentahalogen cation ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Properties of Organoindium Bromidesi-Pr3In gives with InBr3 (molar ratio 2:1, toluene, 50°C) i-Pr2InBr (1) and (molar ratio 1:2, toluene, 80°C) i-PrInBr2 (2). The corresponding reaction of (PhCH2)3In and InBr3 (2:1) gives (PhCH2)2InBr (3), while PhCH2InBr2 could be isolated only as ether adduct [PhCH2InBr2(OEt2)n] (4). With DME/MeCN and 2 and 4 with THF, respectively, yields the solvate complexes [InBr3(DME)(MeCN)] (5), [i-PrInBr2(THF)2] (6) and [PhCH2InBr2(THF)2] (7). The compounds 1-7 were investigated with NMR-, IR- and MS-techniques. Pyrolysis of the raw material of i-Pr3In, which contains “MgBrCl” and additional treatment with Et2O yields the salt [Mg3Cl4,65Br0,35(Et2O)6][i-PrInBr2,7Cl0,3] (8). The cation, a trinuclear magnesium complex, possesses local D3h-symmetric of the Mg3X5 backbone (X = Cl, Br).
    Notes: i-Pr3In ergibt mit InBr3 (Molverhältnis 2:1, Toluol, 50°C) i-Pr2InBr (1) und (Molverhältnis 1:2, Toluol, 80°C) i-PrInBr2 (2). (PhCH2)3In und InBr3 (2:1) ergeben entsprechend (PhCH2)2InBr (3), während PhCH2InBr2 nur als Etherat [PhCH2InBr2(OEt2)n] (4) erhalten wurde. Mit DME/MeCN bzw. 2 und 4 mit THF werden die Solvatkomplexe [InBr3(DME)(MeCN)] (5) bzw. [i-PrInBr2(THF)2] (6) und [PhCH2InBr2(THF)2] (7) erhalten. 1-7 wurden mittels NMR-und IR-Spektroskopie bzw. Massenspektrometrie untersucht. Pyrolyse des „MgBrCl“-enthaltenden Rohproduktes von i-Pr3In und nachträgliches Behandeln mit Et2O liefert das Salz [Mg3Cl4,65Br0,35(Et2O)6][i-PrInBr2,7Cl0,3] (8), welches ein dreikerniges, Magnesium-haltiges Kation mit lokaler D3h-Symmetrie des Mg3X5-Gerüstes (X = Cl, Br) enthält.
    Additional Material: 11 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210303
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  • 8
    Electronic Resource
    Electronic Resource
    Reaktionen von Diorganogallium(indium)fluoriden. Die Kristallstruktur von Mes2InFProfessor Dirk Reinen zum 65. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 597-606 
    Details
    ISSN: 0044-2313
    Keywords: Diorganogallium fluorides ; Diorganoindium fluorides ; reactions ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Diorganogallium(indium) Fluorides. The Crystal Structure of Mes2InFMes2GaF (1) reacts with t-BuNH2 at 20°C to the amine adduct [Mes2Ga(F)(t-BuNH2)] (2). Treatment of 1 with H2S gives after a redox reaction γ-S8-Sulfur (Muthmanns' Sulfur) (3) as the only isolated product. When i-Pr2InF (4) is reacted with [SnCl2(dioxane)] in toluene at 70°C one yields after workup [i-PrInCl2(dioxane)] (5), which is formed after ligand exchange and reaction with dioxane.2 and 5 were investigated by NMR-, IR- and MS-techniques. In addition, 2 · 2,5 THF, 3, 5 and Mes2InF were characterized by an X-ray structure determination. According to that 2 · 2,5 THF contains dimeres, associated by hydrogen brigdes, while 5 possesses a polymeric structure with bridging dioxane molecules. 3 forms eightmembered rings with C2-symmetry. Me2InF is a trimer in the solid state with an In3F3-backbone.
    Notes: Mes2GaF (1) reagiert mit t-BuNH2 bei 20°C zum Aminaddukt [Mes2Ga(F)(t-BuNH2)] (2). Bei Einwirkung von H2S auf 1 tritt eine Redoxreaktion ein, deren einziges isoliertes Produkt der γ-S8-Schwefel (Muthmannsche Schwefel) (3) ist. Wird i-Pr2InF (4) mit [SnCl2(Dioxan)] in Toluol bei 70°C umgesetzt erhält man nach Aufarbeitung das durch Ligandenaustausch und Adduktformierung gebildete [i-PrInCl2(Dioxan)] (5).2 und 5 wurden mittels NMR- und IR-Spektroskopie sowie Massenspektrometrie untersucht. Zusätzlich wurden 2 · 2,5 THF, 3, 5 und Mes2InF durch eine Röntgenstrukturanalyse charakterisiert. 2 · 2,5 THF liegt danach als über Wasserstoffbrückenbindungen assoziiertes Dimer vor, während 5 eine polymere Struktur mit verbrückenden Dioxanmolekülen besitzt. 3 bildet achtgliedrige Ringe mit zweizähliger Lagesymmetrie. Mes2InF formt Trimere mit einem In3F3-Sechsring-Gerüst.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210417
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  • 9
    Electronic Resource
    Electronic Resource
    Synthese und Eigenschaften von Trimesitylthallium. Ein Vergleich der Trimesitylelement-Verbindungen der 13. GruppeProfessor Armin Berndt zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 309-315 
    Details
    ISSN: 0044-2313
    Keywords: Organoindium compound ; organothallium compound ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Properties of Trimesitylthallium. A Comparison of the Trimesitylelement Compounds of Group 13The reaction of T1C13 with MesMgBr (Mes = 2,4,6-Me3C6H2) in THF at 0°C gives trimesitylthallium, TlMes3 (2). 2 has been characterized with NMR, IR and MS techniques as well as by an X-ray structure determination. 2 crystallizes isostructural to InMes3 (1a). The molecules of 2 are coordinated by the three mesityl substituents in a planar fashion. A new modification of InMes3 (1b) could be obtained by recrystallization of InMes3 from toluene/n-pentane in the space group C2/c. The literature known modification 1a and the new metallane 2 crystallize in the space group P21/n. The molecules in 1b possess C2-symmetry. The trimesitylelement compounds EMes3 (E = B, A1, Ga, In, T1) have been compared with each other.
    Notes: Die Reaktion von TlCl3 mit MesMgBr (Mes = 2,4,6-Me3C6H2) in THE bei 0°C liefert Trimesitylthallium, TlMes3 (2). 2 wurde mittels NMR- und IR-Spektroskopie bzw. Massenspektrometrie untersucht. Die Röntgenstrukturanalyse ergab ein isostrukturell zu InMes3 (1 a) kristallisierendes Molekül, dessen Tl-Zentrum planar von den drei Mesitylsubstituenten umgeben ist. Durch Kristallisation aus Toluol/n-Pentan konnte eine neue Modifikation des In-Mes3 (1 b) erhalten werden, die im Gegensatz zu 1 a und 2 (P21/n) in der Raumgruppe C2/c kristallisiert, wobei die Moleküle von 1 b C2-Symmetrie besitzen. Die Trimesitylelement-Verbindungen EMes3 (E = B, Al, Ga, In, Tl) werden miteinander verglichen.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230150
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