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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 461 (1980), S. 7-12 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Divalent Samarium: AISm2IIX5 (AI = K, Rb; X = Cl, Br, I)Ternary halides with divalent Samarium ASm2X5 were prepared and investigated by X-ray techniques. The paramagnetic susceptibility of Sm2+ has been measured with a Faraday balance and calculated theoretically.
    Notes: Ternäre Halogenide mit zweiwertigem Samarium ASm2X5 (A = K, Rb; X = Cl, Br, I) wurden dargestellt und röntgenographisch untersucht. Sie sind isotyp mit TlPb2Cl5. Die paramagnetische Suszeptibilität von Sm2+ wurde mit einer Faraday-Waage gemessen und theoretisch berechnet.
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  • 2
    ISSN: 0044-2313
    Keywords: Sodium Tetrachlorotitanate(II) ; Synthesis ; Crystal Structure ; Magnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure and Magnetism of Sodium Tetrachlorotitanate(II), Na2TiCl4Na2TiCl4 is obtained as single crystals by metallothermic reduction of TiCl3 with sodium (525°C, 90 d, Ta container). Pure powder samples may be prepared by synproportionation of TiCl3 with Ti in the presence of NaCl (950-520°C, 21 d). The structure refinement from four-circle diffractometer data confirms that Na2TiCl4 is isotypic with Sr2PbO4 (orthorhombic, space group Pbam (No. 55), Z = 2 a = 694.2(1), b = 1 198.9(2), c = 385.6(1) pm, R = 0.055, Rw = 0,038). Ti2+ is surrounded by a distorted octahedron of Cl-. The octahedra are connected via common edges to chains, ∞1[TiCl2/1Cl4/2]2-, that run in the [001] direction. Magnetic susceptibility data were recorded in the 2 to 300 K temperature range at various field strengths. The interpretation of the data was carried out with the aid of crystal-field calculations taking magnetic interactions into account. The non-Curie behaviour of the reciprocal magnetic susceptibility of Ti2+ in Na2TiCl4 is due to the influence of spin-obit coupling.
    Notes: Na2TiCl4 entsteht in Form von Einkristallen bei der metallothermischen Reduktion von TiCl3 mit Na (525°C, 90 d, Ta-Ampulle). Reine Pulverproben von türkis-grünem Na2TiCl4 sind durch Synproportionierung von TiCl3 mit Titan in Gegenwart von NaCl zugänglich (950-520°C, 21 d). Die Strukturverfeinerung aus Vierkreis-Diffraktometer-Daten bestätigt, daß Na2TiCl4 im Sr2PbO4-Typ kristallisiert (orthorhombisch, Raumgruppe Pbam (Nr. 55), Z = 2, a = 694,2(1), b = 1 198,9(2), c = 385,6(1) pm, R = 0,055, Rw = 0,038). Ti2+ ist in Form eines verzerrten Oktaeders von Cl- umgeben. Die Oktaeder sind über gemeinsame Kanten zu Ketten ∞1[TiCl2/1Cl4/2]2- verknüpft, die längs [001] angeordnet sind. Die magnetische Suszeptibilität wurde im Bereich von 2-300 K bei verschiedenen Feldstärken bestimmt. Die Interpretation der Meßdaten erfolgte über Kristallfeld-Rechnungen unter Berücksichtigung magnetischer Wechselwirkungen. Das Nicht-Curie-Verhalten der reziproken magnetischen Suszeptibilität von Ti2+ in Na2TiCl4 ist auf den Einfluß der Spin-Bahn-Kopplung zurückzuführen.
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  • 3
    ISSN: 0044-2313
    Keywords: Na-β″-alumina ; lanthanide ion exchange ; crystal structure ; impedance spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structural Chemistry and Impedance Spectroscopy of Mg2+ stabilized Na+/Pr3+-β″-AluminasThe structure with the ionic distribution in the conduction planes of a Pr3+-exchanged Mg2+ stabilized Na+-β″-alumina crystal, composition determined by electron microprobe analysis to Na1.19Pr0.13Mg0.49Al10.49O17 (degree of exchange ξ = 25%, related to Na+ content), has been investigated by single crystal X-ray diffraction methods at room temperature (R3m, Z = 3, a = 561.8(2) pm, c = 3 361.5(11) pm). Pr3+ is slightly shifted in the ab-plane from the centrosymmetric 9 d (mO) into a 18 h site. Na+ occupies 18 h as well as 6 c (BR) positions. Ionic conductivity data of Mg2+ stabilized Na+/Pr3+-β″-Al2O3 crystals with varying degree of exchange determined by impedance spectroscopy are given in an Arrhenius diagram. With growing Pr3+ content the conductivity σ decreases with increasing activation energy.
    Notes: Die Struktur mit der Ionenverteilung in den Leitungsschichten eines Pr3+-ausgetauschten Mg2+-stabilisierten Na+-β″-Al2O3-Kristalls, analytisch durch Mikrosondemessungen bestimmte Zusammensetzung Na1,19Pr0,13Mg0,49Al10,49O17 (Austauschgrad ξ = 25%, bezogen auf Na+-Gehalt), wurde bei Raumtemperatur anhand röntgenographischer Einkristalldaten bestimmt (R3m, Z = 3, a = 561,8(2) pm, c = 3 361,5(11) pm). Pr3+ ist innerhalb der ab-Ebene geringfügig von der zentrosymmetrischen 9 d (mO) Lage in eine 18 h-Position ausgelenkt. Na+ besetzt sowohl die Punktlage 18 h als auch 6 c (BR). Impedanzspektroskopisch ermittelte Leitfähigkeitsdaten werden in Form eines Arrhenius-Diagramms für Mg2+-stabilisierte Na+/Pr3+-β″-Al2O3-Kristalle unterschiedlichen Austauschgrades vorgestellt. Mit zunehmendem Pr3+-Einbau fällt die Ionenleitfähigkeit σ, bei gleichzeitigem Anstieg der Aktivierungsenergie, ab.
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  • 4
    ISSN: 0044-2313
    Keywords: Octamethylammonium trichloride bis(diaquaterachloroneodymate hexachloroneodymate) ; preparation ; single crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of (CH3NH3)8[NdCl6][NdCl4(H20)2]2Cl3(CH3NH3)8[NdCl6][NdCl4 (H2O)2]2Cl3 is for the first time prepared and investigated by X-ray, single crystal work. It crystallizes in the monoclinic system (space group C2/m, Z = 2) with a = 9.358(5), b = 17.424(9), c = 15.360(8) Å, β = 108.30(4)°. The structure contains besides isolated Cl- ions distorted [NdCl6]3- octahedra and [NdCl4(H2O)2]- chains.
    Notes: (CH3NH3)8[NdCl6][NdCl4(H2O)2]2Cl3 wurde erstmals dargestellt und mit Röntgenmethoden an Einkristallen untersucht. Die Verbindung kristallisiert monoklin (Raumgruppe C2/m, Z = 2) mit den Gitterkonstanten: a = 9,358(5), b = 17,424(9), c = 15,360(8) Å, β = 108,30(4)°. In der Struktur liegen neben isolierten Cl--Ionen verzerrte [NdCl6]3--Oktaeder und [NdCl4(H2O)2]--Ketten vor.
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  • 5
    ISSN: 0044-2313
    Keywords: Ternary selenides of lanthanides ; preparation ; crystal structure ; electronic structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Ternary Selenides of Lanthanoides by Reduction of SesquiselenidesThe compounds MLn2Se3 (M = Na; Ln = La—Sm) and MLn8Se12 (M = Na, Ca; Ln = La—Sm) were prepared by reduction of the corresponding lanthanide sesquiselenides with sodium and calcium, respectively, for the first time. Further-more MLa8Se12 (M = Sr, Eu) could be obtained in an analogous way. All compounds were characterized by chemical analysis and X-ray powder diffraction. The electronic structures of these compounds were investigated by band structure calculations and magnetic measurements.
    Notes: Die Verbindungen MLn2Se3 (M = Na, Ln = La—Sm) und MLn8Se12 (M = Na, Ca; Ln = La—Sm) wurden durch Reduktion der entsprechenden Lanthanidsesquiselenide mit Natrium bzw. Calcium erstmals dargestellt. Weitere Selenide MLa8Se12 (M = Sr, Eu) konnten analog erhalten werden. Die dargestellten Verbindungen wurden analytisch und röntgenographisch charakterisiert. Zur Bestimmung der elektronischen Struktur dieser Verbindungen wurden Bandstrukturrechnungen und magnetische Messungen durchgeführt.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1744-1746 
    ISSN: 0044-2313
    Keywords: Terbium sesquiselenide ; chemical transport ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Tb2Se3Single crystals of Tb2Se3 could be prepared by chemical transport reaction with AlCl3. By starting from TbSe1.9 and terbium metal black needles of Tb2Se3 in the U2S3 type structure with the space group Pnma and a = 1113,0(1) pm, b = 402,4(1) pm and c = 1095,1(3) pm were obtained.
    Notes: Einkristalle von Tb2Se3 konnten durch chemischen Transport mit AlCl3 dargestellt werden. Ausgehend von pulverförmigem TbSe1,9 und Terbiummetall wurden schwarze, nadelförmige Einkristalle von Tb2Se3 im U2S3-Strukturtyp mit der Raumgruppe Pnma und a = 1113,0(1) pm, b = 402,4(1) pm und c = 1095,1(3) pm erhalten.
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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: Drei Bromide des Lanthans: LaBr2, La2Br5 und LaBr3Farbloses LaBr3 wurde durch Umsetzung von La2O3 mit NH4Br bzw. in einkristalliner Form durch chemischen Transport mit AlBr3 erhalten. Schwarze Einkristalle von LaBr2 und La2Br5 wachsen aus der Schmelze, die man bei der metallothermischen Reduktion von LaBr3 mit Lithium erhält (verschweißte Tantalampulle, 850°C). Die Kristallstrukturen der drei Lanthanbromide wurden verfeinert: LaBr2. 2H2-Typ, hexagonal (P63/mmc); a = 409,88(4) pm; c = 1 390,0(1) pm; R = Rw = 0,092; La2Br5. Pr2I5-Typ, monoklin (P21/m); a = 789,09(6) pm; b = 424,89(4) pm; c = 1342,3(1) pm β = 91,60(1)º; R = 0,067; Rw = 0,055; LaBr3. UCl3-Typ, hexagonal (P63/m) a = 797,13(4) pm; c = 452,16(4) pm; R = 0,036; Rw = 0,032.
    Notes: Colourless LaBr3 was obtained via the ammonium-bromide route and in singlecrystalline form by chemical vapour-phase transport with aluminium tribromide. Black single crystals of LaBr2 and La2Br5 have been grown from the melts that are obtained by lithium reduction of lanthanum tribromide in sealed tantalum ampoules at 850°C. The crystal structures of the three bromides of lanthanum were refined: LaBr2. 2H2-MoS2 type, hexagonal (P63/mmc), a = 409.88(4) pm, c = 1390.0(1) pm, R = Rw = 0.092; La2Br5. Pr2I5 type, monoclinic (P21/m), a = 789.09(6) pm, b = 424.89(4) pm, c = 1342.3(1) pm, β = 91.60(1)º, R = 0.067, Rw = 0.055; LaBr3. UCl3 type, hexagonal (P63/m), a = 797.13(4) pm, c = 452.16(4) pm, R = 0.036, Rw = 0.032.
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  • 8
    ISSN: 0044-2313
    Keywords: Lanthanoide bromoaluminates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) and Thermal Decomposition to LnBr3LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) was prepared in crystalline form for the first time. The crystal structures of LaAl3Br12, PrAl3Br12, and NdAl3Br12 were determined on single crystals by X-ray methods. The isotypic compounds crystallize with trigonal symmetry, space group P 3112, Z = 3. A structural comparison to lanthanoide chloroaluminates of equal composition is given and thermal decomposition of LnAl3Br12 (Ln = Nd) to the corresponding lanthanoide tribromide is described.
    Notes: Die Bromide LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) wurden erstmals in kristalliner Form dargestellt und die Kristallstrukturen von LaAl3Br12, PrAl3Br12 anhand von röntgenographischen Einkristalluntersuchungen bestimmt. Alle kristallisieren in der trigonalen Raumgruppe P 3112, Z = 3. Ein struktureller Vergleich mit Lanthanoidchloroaluminaten der gleichen Zusammensetzung und der thermische Abbau von LnAl3Br12 (Ln = Nd) zum entsprechenden Lanthanoidtribromid werden beschrieben.
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  • 9
    ISSN: 0044-2313
    Keywords: Lanthanides ; sulfide and selenide disilicates ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: M4X3[Si2O7]-Type Lanthanide Chalcogenide Disilicates (M = Ce—Er; X = S, Se)Attempts to produce single crystals of MSe2 (or MSe2-X) by vapour phase transport with iodine or the oxidation of MCl2 (or MClH) with sulfur in the presence of NaCl in sealed evacuated quartz containers often yielded well-grown single crystals with the composition M4X3[Si2O7] (M = pr, Sm, Gd, X = Se, and M = Nd, Er, X = S) as by-products. The crystal structures (tetragonal, 141/amd (no. 141)), Z = 8, contain two crystallographically independent M3+ Cations that are interconnected by chalcogenide (X2-) and disilicate anions ([Si2O7]6-). (M1)3+ is surrounded by eight (five X2- and three terminal O2- of the disilicate group), (M2)3+ by nine (three X2- and six terminal O2- of the [Si2O7]6- anion) chalcogenide anions. The disilicate anion itself exhibits the eclipsed conformation with non-linear Si—O—Si bridges (angles: 128 - 133°).
    Notes: Bei Versuchen zum chemischen Transport von MSe2 (bzw. MSe2-x) mit I2 bzw. bei der Oxidation von MCl2 bzw. MClHx mit S in Gegenwart von NaCl in evakuierten, geschlossenen Quarz-Ampullen wurden jeweils gut ausgebildete Einkristalle der Zusammensetzung M4X3[Si2O7] (M = Pr, Sm, Gd, X = Se bzw. M = Nd, Er, X = S) als Nebenprodukte erhalten. In den Kristallstrukturen (tetragonal, I41/amd (Nr. 141)), Z = 8; liegen zwei kristallographisch unterschiedliche M3+-Kationen vor, die über Chalkogenid- (X2-) und Disilicat-Anionen ([Si2O7]6-) verknüpft sind. Dabei ist (M1)3+ von insgesamt acht (fünf X2- und drei terminale O2- der Disilicat-Gruppe), (M2)3+ von neun (drei X2- und sechs terminale 02- des [Si2O7]6--Anions) Chalkogenid-Anionen umgeben. Das Disilicat-Anion selbst weist die ekliptische Konformation mit nicht gestrecktem Si—O—Si-Winkel (128 - 133°) auf.
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  • 10
    ISSN: 0044-2313
    Keywords: preparation ; crystal structure ; complex chlorides of lanthanides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of (4-Picolinium)[LnCl4(H2O)3] (Ln = La, Ce, Pr, Nd)The complex water containing chlorides (4-Picolinium)[LnCl4(H2O)3] (Ln = La, Ce, Pr, Nd) were prepared for the first time, and the crystal structures of (4-Picolinium)[LnCl4(H2O)3] (Ln = La, Pr) were determined on single crystals by X-ray methods. The isotypic compounds crystallize with triclinic symmetry, space group P1, Z = 2. Surprisingly there exist the dimeric complex anions [Ln2Cl8(H2O)6]2- (Ln = La, Pr).
    Notes: Die komplexen wasserhaltigen Chloride (4-Picolinium)[LnCl4(H2O)3] (Ln = La, Ce, Pr, Nd) wurden erstmals dargestellt und die Kristallstrukturen von (4-Picolinium)[LnCl4(H2O)3] (Ln = La, Pr) anhand von Einkristalluntersuchungen röntgenographisch bestimmt. Die isotypen Verbindungen kristallisieren in der triklinen Raumgruppe P1, Z = 2. überraschend liegen die dimeren komplexen Anionen [Ln2Cl8(H2O)6]2- (Ln = La, Pr) vor.
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