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  • 1
    ISSN: 0044-2313
    Keywords: Lanthanides ; crystal structure ; acetate halides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [La2Cl3(OAc)2(H2O)7]Cl: The First Lanthanide-Acetate-Halide-Hydrate with Chloride in Inner-Sphere Coordination[La2Cl3(OAc)2(H2O)7]Cl has been obtained as single crystals through the reaction of LaCl3 · 7H2O with diluted acetic acid or from La2O3 with acetyl chloride. In the crystal structure (triclinic, Z = 2, P1 (no. 2), a = 919.6(2), b = 950.7(2), c = 1178.9(2) pm, α = 82.52(1), β = 84.14(1), γ = 64.69(1)°, R = 0.021, Rw = 0.020), La3+ is surrounded by nine ligands (O, Cl). La1 has two chloride and seven oxygen ligands whereas La2 has one chloride and eight oxygen atoms as nearest neighbours. Four of the oxygen ligands of each lanthanum cation originate from a „tetradentate“ acetate anion, the others from crystal water molecules. The „tetradentate“ acetate groups are coordinated not only to one central La3+ as chelate ligands, but also to the „left“ and „right“ La3+ neighbours. Thereby, a one-dimensional infinite cationic chain, 1∞[La2Cl3(OAc)2(H2O)7]+, is formed that runs in the [011] direction. These chains are held together by „lonesome“ chloride ions which are surrounded by (4 + 1) water molecules and connected to the chains via hydrogen bonds.
    Notes: [La2Cl3(OAc)2(H2O)7]Cl wurde in einkristalliner Form durch Umsetzung von LaCl3 · 7H2O mit und in verdünnter Essigsäure oder von La2O3 mit Acetylchlorid erhalten. In der Kristallstruktur (triklin, Z = 2, P1 (Nr. 2); a = 919,6(2); b = 950,7(2); c = 1178,9(2) pm; α = 82,52(1), β = 84,14(1); γ = 64,69(1)°; R = 0,021; Rw = 0,020) ist La3+ von jeweils neun Liganden (O, Cl) umgeben. Dabei weist La1 zwei Chlorid- und sieben Sauerstoff-, La2 dagegen nur einen Chlorid-, jedoch acht Sauerstoff-Liganden als nächste Nachbarn auf. Je vier der Sauerstoff-Liganden in der Koordinationssphäre des Lanthans stammen von einer „vierzähnigen“ Acetatgruppe, die übrigen von Hydratwasser-Molekülen. Die Acetatgruppen koordinieren sowohl am zentralen (chelatisierend) als auch zu den „rechts“ und „links“ benachbarten La3+-Kationen. Hierdurch entstehen eindimensional unendliche, kationische Ketten 1∞[La2Cl3(OAc)2(H2O)7]+, die in Richtung [011] verlaufen. Diese Ketten werden durch „einsame“ Chlorid-Ionen zusammengehalten, die ihrerseits von (4 + 1) Hydratwasser-Molekülen umgeben sind, zu denen Wasserstoffbrücken-Bindungen ausgebildet werden.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1465-1473 
    ISSN: 0044-2313
    Keywords: Cesium Lutetium(III) Acetate ; Synthesis ; Crystal Structure ; Thermolysis ; Evolved Gas Aalysis (EGA) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Acetates of the Lanthanides with Cesium: Dimers in CsLu(CH3COO)4 and Trimers in Cs2[Lu3(CH3COO)10(OH)(H2O)]. Synthesis, Crystal Structures, ThermolysisSingle crystals of CsLu(CH3COO)4 and Cs2[Lu3(CH3COO)10(OH)(H2O)] were obtained from an aqueous solution of lutetium and cesium acetate in a 1:1 molar ratio. The crystal structures (CsLu(CH3COO)4: monoclinic, P21/n (no. 14), Z = 8, a = 1 293.1(2), b = 1 323.8(2), c = 1 622.5(3) pm, β = 92.01(2)°, Vm = 208.97(6) cm3/mol, R = 0.056, Rw = 0.034; Cs2[Lu3(CH3COO)10(OH)(H2O)]: monoclinic, C2/c (no.15), Z = 4, a = 2 138.5(6), b = 1 378.0(3), C = 1 482.9(4) pm, β = 106.15(2)°, Vm = 632.0(3) cm3/mol, R = 0.049, Rw = 0.036) were determined from four-circle-diffractometer data. The structures consist of dimers and trimers, respectively, that are built by bridging acetate groups. These units are fragments of the infinite chains of the Ho(CH3COO)3 type of structure. The isotypic compounds CsM(CH3COO)4 with M=Eu—Lu were synthesized and characterized by the X-ray Guinier technique. The thermal decomposition of CsLu(CH3COO)4 was examined with thermoanalytical methods (TG/DSC with coupled gas analysis) and the Guinier-Simon technique: it decomposes at 260°C in an endothermic reaction to Lu2O3 and Cs2CO3.
    Notes: Die Verbindungen CsLu(CH3COO)4 und Cs2[Lu3(CH3COO)10(OH)(H2O)] konnten aus wäßriger Lösung von Cs(CH3COO) und Lu(CH3COO)10 (OH)(H2O) dargestellt werden. Ihre Kristallstrukturen (CsLu(CH3COO)4: monoklin, P21/n (Nr. 14), Z = 8, a = 1293,1(2), b = 1323,8(2), c = 1 622,5(3) pm, β = 92,01(2)°, Vm = 208,97(6) cm3/mol, R = 0,056, Rw = 0,034; Cs2[Lu3(CH3COO)10(OH)(H2O)]: monoklin, C2/c (Nr. 15), Z = 4, a = 2138,5(6), b = 1378,0(3), C = 1 482,9(4) pm, β = 106,15(2)°, Vm = 632,0(3) cm3/mol, R = 0,049, Rw = 0,036) wurden anhand von Vierkreisdiffraktometerdaten bestimmt. In den Kristallstrukturen liegen zwei- bzw. dreikernige Baueinheiten vor, die durch verbrückende Acetatgruppen aufgebaut werden und Fragmente der unendlichen Ketten im Ho(CH3COO)3-Typ darstellen. Die isotypen Verbindungen CsM(CH3COO)4, M=Eu—Lu, wurden hergestellt und mittels Pulver-Röntgenmethoden charakterisiert. Das thermische Verhalten von CsLu(CH3COO)4 wurde mittels TG/DSC und simultaner Gasanalyse (EGA) einerseits und mit Hilfe der Guinier-Simon-Technik andererseits untersucht: Es zersetzt sich ab 260°C in Cs2CO3 und Lu2O3.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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