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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 877-888 
    ISSN: 0044-2313
    Keywords: Barium ; Bis(trimethylsilyl)phosphanide ; Phosphanide ; Tin ; NMR ; X-ray Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Characterization of Hetero-bimetallic Bis(trimethylsilyl)phosphanides of Barium and TinThe reaction of barium bis[bis(trimethylsilyl)amide] with one equivalent of bis(trimethylsilyl)phosphane in 1,2-dimethoxyethane (dme) yields the heteroleptic dimeric (dme)barium bis(trimethylsilyl)amide bis(trimethylsilyl)phosphanide. This colorless compound crystallizes in the monoclinic space group P21/n with a = 1 259.1(3), b = 1 822.7(4), c = 1 516.1(3) pm, β = 110.54(3)° and Z = 4. The central moiety of the centrosymmetric molecule is the planar Ba2P2-cycle with Ba—P-bond lengths of 329 and 334 pm. In the presence of bis[bis(trimethylsilyl)amino]stannylene hetero-bimetallic bis(trimethylsilyl)phosphanides of tin(II) and barium are isolated. If the reaction of Ba[N(SiMe3)2]2 and Sn[N(SiMe3)2]2 in the molar ratio of 1:2 with six equivalents of HP(SiMe3)2 is performed in toluene, barium bis{tin(II)-tris[bis(trimethylsilyl)phosphanide]} can be isolated. This compound crystallizes in the orthorhombic space group P212121 with a = 1 265.1(1), b = 2 290.1(3), c = 2 731.9(3) pm and Z = 4. The anions {Sn[P(SiMe3)2]3}- bind as two-dentate ligands to the barium atom which shows the extraordinary low coordination number of four. The addition of tetrahydrofuran (thf) to the above mentioned reaction solution leads to the elimination of tris(trimethylsilyl)phosphane and the formation of thf complexes of barium bis{tin(II)-bis(trimethylsilyl)phosphanide-trimethylsilylphosphandiide}. The derivative crystallizes from toluene in the monoclinic space group P21/c with a = 1 301.9(2), b = 2 316.3(3), c = 3 968.7(5) pm, β = 99.29(1)° and Z = 8.
    Notes: Bei der Reaktion von Barium-bis[bis(trimethylsilyl)amid] mit einem Äquivalent Bis(trimethylsilyl)phosphan in 1,2-Dimethoxyethan (DME) wird heteroleptisches, dimeres (1,2-Dimethoxyethan-O,O′)barium-bis(trimethylsilyl)-amid-bis(trimethylsilyl)phosphanid isoliert. Diese farblose Verbindung kristallisiert in der monoklinen Raumgruppe P21/n mit a = 1 259,1(3), b = 1 822,7(4), c = 1 516,1(3) pm, β = 110,54(3)° und Z = 4. Das zentrale Strukturelement des zentrosymmetrischen Moleküls ist der planare Ba2P2-Cyclus mit Ba—P-Bindungslängen von 329 und 334 pm. In Gegenwart des Bis[bis(trimethylsilyl)amino]stannylens erhält man heterobimetallische Bis(trimethylsilyl phosphanide von Zinn(II) und Barium. Wird die Umsetzung von Ba[N(SiMe32]2 and Sn[N(SiMe3)2]2 im molaren Verhältnis 1:2 mit sechs Äquivalenten HP(SiMe3)2 durchgeführt, kann Barium-bis{zinn(II)-tris-[bis(trimethylsilyl)phosphanid]} isoliert werden. Diese Verbindung kristallisiert in der orthorhombischen Raumgruppe P212121 mit a = 1 265,1(1), b = 2 290,1(3), c = 2 731,9(3) pm und Z = 4. Die Anionen {Sn[P(SiMe3)2])3}- binden als zweizähnige Liganden an das Bariumatom, das dadurch die ungewöhnlich niedrige Koordinationszahl vier aufweist. Die Zugabe von THF zu der oben beschriebenen Reaktionslösung führt zur Eliminierung von Tris(trimethylsilyl)phosphan und der Bildung von Barium-bis{zinn(II)-bis(trimethylsilyl)phosphanid-trimethylsilylphosphandiid). Das Derivat kristallisiert aus Toluol in der monoklinen Raumgruppe P21/c mit a = 1 301,9(2), b = 2 316,3(3), c = 3 968,7(5) pm, β = 99,29(1)° und Z = 8.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1785-1796 
    ISSN: 0044-2313
    Keywords: Organotin pyrrole derivatives ; NMR, vibrational spectra, X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trimethylstannyl- and Dimethylstannyl-substituted Pyrroles - Synthesis, Spectra, and StructuresMonomeric trimethylstannyl pyrroles, Me3Sn—R (Me = CH3 and R = —NC4H4, —NC4H2Me2-2,5, —NC4Me4-2,3,4,5, —C4H3NMe-1), are synthesized by metathesis reactions from Me3SnCl with 1(N)- and 2(C)-lithium pyrroles, respectively. An almost similar procedure gives monomeric dimethylstannylbis(pyrroles), Me2SnR2 (1 a - 3 a), from Me2SnCl2 and 1-Li-pyrrolides (1 : 2 molar ratio) in good yields. Lithiated 1,2,5-trimethylpyrrole and Me3SnCl forms the compound Me3Sn—CH2—C4H2Me(-5)NMe (8), the reaction of Me2SnCl2 with 2-lithium-1-methylpyrrole gives oligomeric [Me2Sn—C4H2NMe—]x, (6 a). The mass-, NMR, and vibrational spectra have been measured and discussed. The results of the X-ray structure determinations of Me3Sn—NC4H4 (1) and Me2Sn(—NC4Me4)2 (3 a) are compared with the structures of the known dimethylmetal pyrroles of Al, Ga, and In.
    Notes: Monomere Trimethylstannylpyrrole, Me3Sn—R (Me = CH3, R = —NC4H4, —NC4H2Me2-2,5, —NC4Me4-2,3,4,5, —C4H3NMe-1), werden durch Metathese aus Me3SnCl und 1(N)- bzw. 2(C)-lithiierten Pyrrolen synthetisiert. Analog hierzu werden aus Me2SnCl2 und Li—N Pyrroliden (Molverhältnis 1 : 2) die ebenfalls monomeren Dimethylstannylbis(pyrrole), Me2SnR2 (1a - 3a), in guten Ausbeuten erhalten. Einfach lithiiertes 1,2,5-Trimethylpyrrol bildet mit Me3SnCl die Verbindung Me3Sn—CH2—C4H2Me(-5)NMe (8); die Umsetzung von Me2SnCl2 mit 2C-lithiiertem 1-Methylpyrrol ergibt oligomeres [Me2Sn—C4H2NMe—]x (6 a). Die Massen-, Kernresonanz- und Schwingungsspektren werden aufgenommen und diskutiert. Die Ergebnisse der Röntgeneinkristallstrukturanalysen von Me3Sn—NC4H4 (1) und Me2Sn(—NC4Me4)2 (3 a) werden mit den Strukturdaten der bekannten Dimethylmetallpyrrole des Al, Ga und In Verglichen.
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  • 3
    ISSN: 0044-2313
    Keywords: 1,2-Bis(dimethylamino)-3,4,5-triphenyl-3,4,5-triphospha-1,2-diborolane ; 1,2-bis(dimethylamino)-3,4,5,6-tetra-tbutyl-3,4,5,6-tetraphospha-1,2-diborine ; preparation ; NMR ; molecular structures ; ab initio calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,2-Bis(dimethylamino)-3,4,5-triphenyl-3,4,5-triphospha-1,2-diborolane and 1,2-Bis(dimethylamino)-3,4,5,6-tetra-tbutyl-3,4,5,6-tetraphospha-1,2-diborine: Synthesis and Structure as well as Calculations on the Molecular StructureThe diphosphides K2[(C6H5)P—(C6H5)P—P(C6H5)], 4 or K2[(tBuP)—(tBuP)2—P(tBu)], 5, react with (ClBNMe2)2 to form the binary 5-membered ring system 1,2-bis(dimethylamino)-3,4,5-triphenyl-3,4,5-triphospha-1,2-diborolane (C6H5P)3(BNMe2)2, 2a, and the 6-membered ring system 1,2-bis(dimethylamino)-3,4,5,6-tetra-tbutyl-3,4,5,6-tetraphospha-1,2-diborine, (tBuP)4(BNMe2)2, 3a, respectively. 2a and 3a could be obtained in a pure form and characterized NMR spectroscopically and by X-ray structure analyses. The two ring systems are folded; 2a exists in the „envelope“- 3a in the „boat“-conformation. Ab initio computations for 3,4,5-triphospha-1,2-diborolane M5 show that the global minimum is characterized by one B—P double bond. The parent compound geometry M6 is characterized by transannular bonding in the PH—BH—BH—PH moiety which differs in character from those in the four- and five-membered rings (BH)2(PH)2 and (BH)2(PH)3 M5 d, respectively. Explicit calculation of the influence of amino substituents on boron improved agreement of the bond length between computed and X-ray data.
    Notes: Die Diphosphide K2[(C6H5)P—(C6H5)P—P (C6H5)], 4, bzw. K2[(tBuP)—(tBuP)2—P(tBu)], 5, reagieren mit (ClBNMe2)2 zu dem binären Fünfringsystem 1,2-Bis(dimethylamino)-3,4,5-triphenyl-3,4,5-triphospha-1,2-diborolan (C6H5P)3(BNMe2)2, 2a, bzw. dem Sechsringsystem 1,2-Bis(dimethylamino)-3,4,5,6-tetra-tbutyl-3,4,5,6-tetraphospha-1,2-diborin, (tBuP)4(BNMe2)2, 3a. 2a und 3a konnten in reiner Form isoliert, NMR-spektroskopisch und durch Röntgenstrukturanalysen charakterisiert werden. Beide Ringsysteme sind gefaltet; 2a zeigt eine „envelope“- 3a eine „Wannen“-Konformation.Ab initio Berechnungen an 3,4,5-Triphospha-1,2-diborolan M5 zeigen, daß im globalen Minimum eine B—P-Doppelbindung mit annähernd planarem σ3-Phosphor vorliegt. Die Geometrie der Stammverbindung des Sechsringes M6 weist „durch-den-Ring“-Bindung in der PH—BH—BH—PH-Baugruppe auf, welche sich von jenen im Vier- und Fünfring M5 d unterscheidet. Durch die explizite Berechnung des Einflusses von Aminosubstituenten an Bor auf die Geometrien des Fünf- und Sechsringes verbessert sich die Übereinstimmung der Bindungslängen mit den Daten der Röntgenstrukturanalyse.
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  • 4
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on Dialkyl Metal Phosphoric and Phosphinic Acid Derivatives of the Elements Aluminium, Gallium, Indium, and Thallium, III. The Vibrational Spectra of the Hypophosphites and Dimethyl ThiophosphinatesThe vibrational spectra (IR and RAMAN) of the dimethylmetal hypophosphites (CH3)2MOOPH2 and the dimethylmetal dimethylthiophosphinates (CH3)2MOSP(CH3)2 of the elements aluminium, gallium, and indium are assigned and discussed. A new spinning RAMAN cell is described.
    Notes: Die Schwingungsspektren (IR und RAMAN) der Dimethylmetall- hypophosphite, (CH3)2MOOPH2, und der Dimethylmetalldimethylthiophosphinate, (CH3)2MOSP(CH3)2, der Elemente Aluminium, Gallium und Indium werden zugeordnet und diskutiert. Außerdem wird eine neue, rotierende RAMAN-Probenhalterung beschrieben.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 429 (1977), S. 99-104 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of Dimeric DimethylaminodimethylindiumDimeric dimethylamino-dimethylindium was prepared by splitting off methane from the adduct Me3In—NHMe2 and characterized by its vibrational spectra. The structure - determined by X-ray analysis - has shown to have the monoclinic space group P21/c with a = 7.601, b = 7.336, c = 14.927 Å and β = 119.9°. Patterson, Fourier and Difference synthesis were used for determing the structure, which was refined by least square analysis to an R value of 0.068.
    Notes: Dimeres Dimethylamino-dimethylindium wurde durch Methanabspaltung aus dem Addukt Me3In—Me2NH dargestellt und schwingungsspektroskopisch charakterisiert. Die Röntgenstrukturanalyse führte zu der monoklinen Raumgruppe P21/c mit a = 7,601, b = 7,336, c = 14,927 Å und β = 119,9°. Die Struktur wurde aus Patterson-, Fourier- und Differenz-Fourier-Synthesen abgeleitet und nach der Methode der kleinsten Fehlerquadrate bis zu einem R-Wert von 0,068 verfeinert.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 551 (1987), S. 85-94 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bis(2,4,6-tri-t-butylphenyl) bicyclotetraphosphaneThe reaction of white phosphorus with 2,4,6-tri-t-butylphenyllithium and 1-bromo-2,4,6-tri-t-butylbenzene yields bis (2, 4, 6-tri-t-butylphenyl) bicyclotetraphosphane 1 and bis (2, 4, 6-tri-t-butylphenyl) diphosphene 2. 1 is characterized by its nmr and mass spectra. The crystal and molecular structure are described.
    Notes: Bei der Umsetzung von weißem Phosphor mit 2,4,6-Tri-t-butylphenyllithium und 1-Brom-2,4,6-tri-t-butylbenzol entstehen Bis(2,4,6-tri-t-butylphenyl)bicyclotetraphosphan 1 und Bis(2,4,6-tri-t-butylphenyl)diphosphen 2. 1 ist durch seine NMR-und Massenspektren charakterisiert. Die Kristall- und Molekülstruktur werden beschrieben.
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  • 7
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrogen Bridges. I. Molecular and Crystal Structure of Phosphonic Acid H3PO3 - X-ray and Neutron Diffraction Studies of the Hydrogen and Deuterium CompoundsThe structure of phosphonic acid H3PO3 has been redetermined by single crystal neutron diffraction (λ = 104.22 pm) at 15.0 ± 0.1 K yielding lattice parameters {Pna21; Z = 8; a = 716.6(3); b = 1201.3(5); c = 674.3(3) pm} and bond lengths {mean values from two crystallographically independent molecules: P—O 155; P=O 150; P—H 139; O—H 101 pm} of high reliability (R = 0.053). Each molecule is involved in four asymmetric hydrogen bonds (O…H 155 to 160pm; O—H…O 168 to 177°) with either hydroxyl group donating and the phosphoryl fragment acting as a twofold acceptor. Thus a complex, three-dimensional net, consisting of four- and eight-point circuits in a 1:2 ratio, is put up although the molecules are packed in a comparatively simple way to form an almost cubic closest arrangement.An X-ray crystal structure determination (R = 0.032) carried out at 173 ± 3 K for comparison revealed no significant differences and angles between phosphorus and oxygen atoms; an additional comparing neutron diffraction study at 15.0 ± 0.1 K (λ = 131.68 pm; isotropic atomic displacement parameters) of the hydrogen (r = 0.044) and deuterium compounds (R = 0.041) resulted in nearly identical structural models for the two isotopomers.
    Notes: Die Struktur der Phosphonsäure H3PO3 wurde mittels Neutronenbeugung (λ = 104,22 pm) an einem Einkristall bei 15,0 ± 0,1 K neu bestimmt, so daß Gitterparameter {Pna21; Z = 8; a = 716,6(3); b = 1201,3(5); c 674,3(3) pm} und Bindungslängen {Mittelwerte aus zwei kristallographisch unabhängigen Molekülen: P—O 155; P = O 150; P—H 139; O—H 101 pm} nun sehr genau (R = 0,053) bekannt sind. Jedes Molekül nimmt teil an vier unsymmetrischen Wasserstoff-Brückenbindungen (O…H 155 bis 160 pm; O—H…O 168 bis 177°), wobei die Hydroxyl-Gruppen als Donoren und die Phosphoryl-Fragmente als jeweils zweifache Akzeptoren auftreten. Insgesamt wird so ein komplexes, aus Maschen von vier und acht Knoten im Verhältnis 1:2 bestehendes Raumnetz aufgespannt, obwohl die Moleküle selbst verhältnismäßig übersichtlich im Sinne einer kubisch dichtesten Anordnung gepackt sind.Eine zum Vergleich bei 173 ± 3 K durchgeführte Röntgenstrukturanalyse (R = 0,032) ergab in den P—O-Abständen und O—P—O-Winkeln kaum nennenswerte Unterschiede; eine zusätzliche, vergleichende Neutronenbeugungsuntersuchung bei 15,0 ± 0,1 K (λ = 131,68 pm; isotrope atomare Auslenkungsparameter) an der Hydrogen- (R = 0,044) und an der Deuterium-Verbindung (R = 0,041) führte zu weitgehend übereinstimmenden Strukturmodellen für die Isotopomeren.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 625-631 
    ISSN: 0044-2313
    Keywords: Bis(dichloromethyl)mercury ; Dichloromethylmercuryalkyles ; synthesis ; NMR, vibrational spectra ; X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Spectroscopic and X-Ray Structural Investigations on Dichloromethyl Mercury CompoundsBis(dichloromethyl)mercury, Hg(CHCl2)2, and mixed alkyl compounds RHgCHCl2 (with R = CH3, C2H5) have been synthesized by known methods from CH2Cl2, lithium butanide and HgCl2, CH3HgCl or C2H5HgCl, respectively. The 1H-, 13C-NMR as well as the IR and Raman spectra of the liquid alkyls RHgCHCl2 and the high melting Hg(CHCl2)2 have been measured and assigned. According to the X-ray structure determination Hg(CHCl2)2 crystallizes in the monoclinic space group P21/c with 4 non-symmetric molecules per unit cell (R = 0.046).
    Notes: Bis(dichlormethyl)quecksilber, Hg(CHCl2)2, und die gemischten Alkylverbindungen RHgCHCl2 (mit R = CH3, C2H5) werden nach bekannten Vorschriften aus CH2Cl2, Lithiumbutanid und HgCl2 bzw. CH3HgCl oder C2H5HgCl synthetisiert. Die 1H- und 13C-NMR- sowie die IR- und Ramanspektren der flüssigen Alkyle RHgCHCl2 und des hochschmelzenden Hg(CHCl2)2 werden registriert und ausgewertet. Nach der Röntgenstrukturanalyse kristallisiert Hg(CHCl2)2 in der monoklinen Raumgruppe P21/c mit 4 azentrischen Molekülen in der Elementarzelle (R = 0,046).
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  • 9
    ISSN: 0009-2940
    Keywords: Silicon compounds ; Hydrogen-hydrogen contacts ; Radicals ; ENDOR spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organosilyl exchange reactions of the extremely electronrich and formally “antiaromatic” 1,4-bis(trimethylsilyl)-substituted 1,4-dihydropyrazine 1 with Ph3SiCl or Me5Si2Cl yielded the new compounds 2 and 3 with triarylsilyl and disilanyl substituents. At δ = 4.53 in CDCl3 compound 3 shows a particularly high-field shifted 1H-NMR resonance for the 1,4-dihydropyrazine protons. In contrast to the planar ring arrangement of 1,4-bis(triisopropylsilyl)-1,4-dihydropyrazine 4, the crystal structure determination of the 2,5-dimethylated analogue 5 as obtained by reductive silylation exhibits a pronounced boat conformation of the heterocycle due to steric repulsion between the substituents, the closest H…H (CH3/ CH) contact being 211 pm. Despite the sizeable structural differences between 4 and 5 both compounds are reversibly oxidized at very negative potentials, at -0.90 and -0.85 V vs. Fc+/0, respectively, It appears that the electrochemical behavior of this class of compounds is determined ***primarly by the configuration at the nitrogen centers and less by the ring conformation. Compound 4 reacts with C60 under EPR-detectable electron exchange to afford 4+* and C-*60. The radical cation 4+* generated separately via oxidation with iodine was characterized by low-temperature UV/Vis and ENDOR spectroscopy. An ENDOR spectrum revealing silylalkyl coupling was also obtained for the related radical cation of reversibly oxidizable 1,1′ -bis(tert-butyldimethylsilyl)-1,1′,4,4′ -bipyridylidene (8).
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 391 (1972), S. 97-106 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dialkyl gallium and dialkyl indium oxalatesThe trialkyls of gallium and indium react with oxalic acid in a 2:1 molar ratio. The products have the formula (RaM)2O4C2 with M = Ga, In and R = CH3 C2H5. The vibrational spectra (IR and RAMAN) point to nonplanar structures of D2 symmetry. Mass spectroscopic investigations are used for further determination of the structures.
    Notes: Die Trialkyle des Galliums und Indiums reagieren mit wasser-freier Oxalsäure im Verhältnis 2:1. Man erhält Produkte der Zusammensetzung (R2M)2O4C2 mit M = Ga, In und R = CH3, C2H5. Die Schwingungsspektren (IR und Raman) deuten auf nicht planare Strukturen der Symmetrie D2 hin. Massenspektroskopische Untersuchungen werden zur weiteren Strukturaufklärung herangezogen.
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