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  • 1
    Electronic Resource
    Electronic Resource
    Metallorganische Verbindungen der Lanthanoide. LIII [1].(C5H5Gd)5(μ2-OCH3)4(μ3-OCH3)4(μ5-O) und [Na2(tC4H9OGd)4(μ3-OtC4H9)8(μ6-O)], zwei neue Alkoxigadoliniumcluster mit interstitiellem SauerstoffProfessor Karl-Heinz Thiele zum 60. Geburtstage am 9. März 1990 gewidmet (1990)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 581 (1990), S. 69-81 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organometallic Compounds of the Lanthanides. LIII. (C5H5Gd)5(μ2-OCH3)4(μ3-OCH3)4 (μ5-O) and [Na2(tC4H9OGd)4(μ3-OtC4H9)8(μ6-O)], two New Alkoxi Gadolinium Clusters with Interstitial OxygenGadolinium trichloride reacts in tetrahydrofurane with cyclopentadienyl sodium and two equivalents of sodium methoxide with formation of (C5H5Gd)5(μ2-OCH3)4(μ3-OCH3)4(μ5-O) (1), and with potassium tert-butoxide with formation of [Na2(tC4H9OGd)4(μ3-OtC4H9)8(μ6-O)] (2). The X-ray structure of 1 shows a tetragonal pyramide build up by five gadolinium atoms, containing an oxygen atom in the center of the base and eight bridging methoxo groups. The structure of 2 consists of an oxygen centered octahedron build up by two sodium and four gadolinium atoms, connected by eight bridging tert-butoxy groups and four terminal butoxides. The monoclinic crystals of 1, space group I2/a have the following crystallographic data: a = 2 276.9(5) pm, b = 2 063.1(6) pm, c = 3 152.2(3) pm, β = 90.7(1)°, Z = 12, Dcalcd 1.85 g · cm-3, R = 0.0519. 2 crystallizes tetragonal, space group I4/mmm with a = 1 728.5(4) pm, b = 1 031.0(3) pm, Z = 2, Dcalcd 1.69 g · cm-3, R = 0.0682.
    Notes: Gadoliniumtrichlorid bildet in Tetrahydrofuran mit Cyclopentadienylnatrium und zwei Äquivalenten Natriummethanolat (C5H5Gd)5(μ2-OCH3)4(μ3-OCH3)4(μ5-O) (1), mit Kalium-tert-butanolat kann dagegen [Na2(tC4H9OGd)4(μ3-OtC4H9)8(μ6-O)] (2) isoliert werden. Die Röntgenstrukturanalyse von 1 zeigt eine tetragonale Pyramide aus 5 Gadoliniumatomen mit einem Sauerstoffatom im Zentrum der Basisfläche sowie acht verbrückenden Methanolatgruppen, die von 2 einen aus zwei Natrium- und vier Gadoliniumatomen gebildeten, Sauerstoff-zentrierten Oktaeder mit vier endständigen und acht verbrückenden tert-Butanolat-Einheiten. Die monoklinen Kristalle von 1, Raumgruppe I2/a haben folgende Gitterkonstanten: a = 2 276,9(5) pm, b = 2 063,1(6) pm, c = 3 152,2(3) pm, β = 90,7(1)°, Z = 12, Dber. 1,85 g/cm3, R = 0,0519. 2 kristallisiert tetragonal, Raumgruppe I4/mmm mit a = 1 728,5(4) pm, c = 1 031,0(3) pm, Z = 2, Dber. 1,69 g/cm3, R = 0,0682.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19905810110
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  • 2
    Electronic Resource
    Electronic Resource
    γ-anti-Effekt an 1-Phosphabicyclo[3.3.1]nonan-Derivaten mit Substituenten am Phosphor. Synthese und Struktur von Pentacarbonyl(1-phosphabicyclo[3.3.1]nonan)chrom (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 127-134 
    Details
    ISSN: 0044-2313
    Keywords: γ-anti effect ; 1-phosphabicyclo 3.3.1 nonane derivatives ; pentacarbonylchromium complex ; structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: γ-Anti Effect in 1-Phosphabicyclo[3.3.1]nonane Derivatives with Substituents at Phosphorus. Synthesis and Structure of Pentacarbonyl(1-phosphabicyclo[3.3.1]nonane) ChromiumIn 1-phosphabicyclo[3.3.1]nonane derivatives of the composition C8H15P(X) the CC-conformation always dominates. Changes in the chemical shifts of the bridge-head carbon atom C(5) in the 13C-NMR spectrum are only originated by the electronic influence of the substituent X at the phosphorus centre. Based on a homogeneous interpretation of the electronic interactions and with regard to Pearsons's definition of electronegativity the electronegativities of substituents at the phosphorus atom X = Cr(CO)5, Fe(CO)4, and Ni(CO)3 are estimated. These groups are placed in antiperiplanar orientation to the carbon atom C(5).The molecular structure of (1-phosphabicyclo[3.3.1]-nonane) Cr(CO)5 3 was elucidated by X-ray diffraction analysis. The molecule features the 1-phosphabicyclononane ligand in the CC-conformation, which has a nearly undistorted Cr(CO)5 unit coordinated to the phosphorus atom (d Cr—P = 2.368(1) Å).
    Notes: Bei 1-Phosphabicyclo[3.3.1]nonan-Derivaten C8H15P(X) dominiert stets die CC-Konformation. Änderungen der chemischen Verschiebung des C(5)-Brückenkopfatoms im 13C-NMR-Spektrum werden alleine durch den elektronischen Einfluß des Substituenten X am Phosphoratom hervorgerufen. Auf der Grundlage einer einheitlichen Interpretation der elektronischen Wechselwirkungen und unter Anwendung des Elektronegativitätsbegriffs von Pearson konnte die Elektronegativität der in antiperiplanarer Position zu C(5) stehenden Phosphorsubstituenten X = Cr(CO)5, Fe(CO)4, Ni(CO)3 abgeschätzt werden.Die Molekülstruktur von (1-Phosphabicyclo[3.3.1]-nonan) Cr(CO)5 (3) wurde mittels Röntgenbeugung ermittelt. Das Molekül zeigt das Bild eines 1-Phosphabicyclo[3.3.1]nonans in der CC-Konformation, an dessen Phosphoratom eine nahezu unverzerrte Cr(CO)5 Einheit (d Cr—P = 2,368(1) Å) koordiniert ist.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926100121
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  • 3
    Electronic Resource
    Electronic Resource
    Organometallic Compounds of the Lanthanoides. LXVI. Synthesis and X-ray crystal structure of [O(CH2CH2C5H4)2Y(μ-OH]2 and (MeC5H4)3Ho(H2O), two unusual products of the hydrolysis of organolanthanoide compounds (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 131-138 
    Details
    ISSN: 0044-2313
    Keywords: Organolanthanoide compounds; ; yttrium ; holmium ; IR ; NMR spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metallorganische Verbindungen der Lanthanoide. LXVI. Synthese und Röntgenstrukturanalyse von [O(CH2CH2C5H4)2Y(μ-OH)]2 und (MeC5H4)3Ho(H2O), zwei ungewöhnlichen Produkten der Hydrolyse von Organolanthanoide-VerbindungenBei der partiellen Hydrolyse von [O(CH2CH2C5H4)2]Y(C5H4CH3) 1, [O(CH2CH2C5H4)2]Y(C5H5) 3, und [O(CH2CH2C5H4)2]Ho(C5H4CH3) 5 bilden sich [O(CH2CH2C5H4)2)Y(μ-OH)]2 2, (C5H5)3Y(OH2) 9 and (MeC5H4)3Ho(OH2) 11. Die neuen Verbindungen wurden durch Elementaranalysen, sowie IR- und NMR-spektroskopisch charakterisiert. Die Röntgenstrukturanalyse ergibt für 2 eine monokline Elementarzelle, Raumgruppe P21/n mit den Gitterkonstanten a = 1146,0(3), b = 1046,6(3), c = 1514,9(3) pm, β = 94,83(2)°. Die Molekülstruktur zeigt verbrückende Hydroxylgruppen, der mittlere Y—O-Abstand beträgt 223,8(3) pm. 11 kristallisiert kubisch in der Raumgruppe I43d mit a = 1847,9(3) pm mit z = 16 Formeleinheiten in der Elementarzelle. Die Moleküle besitzen C3-3 Symmetrie, die Koordination ist trigonal-pyramidal mit einem Wassermolekül und drei Methylcyclopentadienylliganden. Der Abstand Ho—O beträgt 231 pm.
    Notes: The partial hydrolysis of [O(CH2CH2C5H4)2]Y(C5H4CH3) 1, [O(CH2CH2C5H4)2]Y(C5H5)3, and [O(CH2CH2C5H4)2]Ho(C5H4CH3) 5 results in the formation of [O(CH2CH2CH2C5H4)2Y(μ-OH)2]2 2, (C5H5)3Y(OH2) 9 and (MeC5H4)3Ho(OH2) 11. The new compounds have been characterized by elemental analyses, IR and NMR spectra. The X-ray structural analyses shows 2 to be monoclinic, space group P21/n with a = 1146.0(3), b= 1046.6(3), c = 1514.9(3) pm, β = 94.83(2)°. The molecular structure shows bridging hydroxyl groups with a mean distance Y—O = 223.8(3) pm. 11 crystallizes in the cubic space group 143d with a = 1847.9(3)pm with Z = 16 molecules per unit cell. The molecules posses symmetry C3-3, the coordination is trigonal pyramidal with three methylcyclopentadienyl anions and one water molecule as ligands. The distance Ho—O is 231 pm.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090324
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  • 4
    Electronic Resource
    Electronic Resource
    Beiträge zur Chemie der Alkylverbindungen von Übergangsmetallen. 61. Darstellung und Kristallstruktur von Tetramethyltitan-1,2-bis(dimethylphosphino)ethan (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 523-526 
    Details
    ISSN: 0044-2313
    Keywords: Tetramethyltitanium-1,2-bis(dimethylphosphino)-ethane ; NMR data ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Transition Metal Alkyl Compounds. 61. Preparation and Crystal Structure of Tetramethyltitanium-1,2-bis(dimethylphosphino)ethaneThe title complex 1 was synthesized by addition of 1,2-bis(dimethylphosphino)ethane to a solution of tetramethyltitanium in diethylether. The complex was characterized by 1H, 13C and 31P NMR spectra and by X-ray crystal structure analysis. 1 consists of two independent molecules with distorted octahedral structure.
    Notes: Der Titelkomplex 1 wurde durch Addition von 1,2-Bis(dimethylphosphino)ethan an Tetramethyltitan in Diethylether erhalten. Der Komplex wurde 1H-, 13C- und 31P-NMR-spektroskopisch, sowie durch Röntgenkristallstruktur-analyse charakterisiert. 1 tritt in der Elementarzelle in zwei unabhängigen Molekülen mit verzerrt oktaedrischer Konstitution auf.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200322
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