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  • 1
    ISSN: 0044-2313
    Keywords: Ternary halides ; synthesis ; crystal structures ; ionic conductivity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Halides of the A3MX6 Type. III [1, 2]. Synthesis, Structures, and Ionic Conductivity of the Halides Na3MX6 (X = Cl, Br)The bromides Na3MBr6 crystallize with the stuffed LiSbF6-type structure (type I; M = Sm—Gd) or with the structure of the mineral cryolite (type II; M = Gd—Lu). The structure types were refined from single crystal X-ray data (Na3SmBr6: trigonal, space group R3, a = 740.8(2) pm, c = 1 998.9(8) pm, Z = 3; Na3YBr6: monoclinic, space group P21/n, a = 721.3(4) pm, b = 769.9(2) pm, c = 1 074.8(4) pm, β = 90.60(4)°, Z = 2). Reversible phase transitions from one structure to the other occur. The phase transition temperatures were determined for the bromides as well as for the chlorides Na3MCl6 (M = Eu—Lu). The refinement of both structures for one compound was possible for Na3GdBr6 (I: trigonal, space group R3, a = 737.1(5) pm, c = 1 887(2) pm, Z = 3; II: monoclinic, space group P21/n, a = 725.2(1) pm, b = 774.1(3) pm, c = 1 080.1(3) pm, β = 90.76(3)°, Z = 2). All compounds exhibit ionic conductivity of the sodium ions which decreases with the change from type I to type II. The conductivity of the bromides is always higher when compared with the respective chlorides.
    Notes: Die Bromide Na3MBr6 kristallisieren im aufgefüllten LiSbF6-Typ (Typ I; M = Sm—Gd) oder im Kryolith-Typ (Typ II; M = Gd—Lu). Die Strukturen wurden anhand von Einkristalldaten verfeinert (Na3SmBr6: trigonal, Raumgruppe R3, a = 740,8(2) pm, c = 1 998,9(8) pm, Z = 3; Na3YBr6: monoklin, Raumgruppe P21/n, a = 721,3(4) pm, b = 769,9(2) pm, c = 1 074,8(4) pm, β = 90,60(4)°, Z = 2). Beide Strukturen sind reversibel ineinander umwandelbar. Die Umwandlungstemperaturen der Bromide wurden ebenso wie die der Chloride Na3MCl6 (M = Eu—Lu) bestimmt. An Na3GdBr6 wurden beide Strukturen an Einkristallen bestimmt (I: trigonal, Raumgruppe R3, a = 737,1(5) pm, c = 1 887(2) pm, Z = 3; II: monoklin, Raumgruppe P21/n, a = 725,2(1) pm, b = 774,1(3) pm, c = 1 080,1(3) pm, β = 90,76(3)°, Z = 2). Alle Verbindungen zeigen Natrium-Ionenleitfähigkeit, die beim Übergang vom Typ I in den Typ II stark abnimmt. Die Bromide zeigen, verglichen mit den Chloriden, jeweils eine bessere Leitfähigkeit.
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  • 2
    ISSN: 0044-2313
    Keywords: Reduced halides ; synthesis ; crystal structure ; europium ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NaEu2Cl6 and Na0.75Eu2Cl6: Mixed Valent Chlorides of Europium with SodiumThe reaction of Na2EuCl5 with Eu metal in sealed gold tubes yields blue single crystals of NaEu2Cl6. It crystallizes with the hexagonal crystal system (space group P63/m) with a = 755.74(8) pm, c = 429.81(5) pm, Z = 1; the structure is closely related to the UCl3-type. Green single crystals of Na0.75Eu2Cl6 were first obtained as a by-product in the synthesis of Na2EuCl5 in evacuated silica tubes and may be prepared by reduction of EuCl3 with sodium. Na0.75Eu2Cl6 crystallizes isotypic to NaEu2Cl6 with a = 753.69(11) pm and c = 416.3(2) pm.
    Notes: Die Umsetzung von Na2EuCl5 mit Eu-Metall in Goldampullen führt zu blauen Einkristallen von NaEu2Cl6, einem Derivat des UCl3-Typs: Hexagonal, Raumgruppe P63/m, a = 755,74(8) pm, c = 429,81(5) pm, Z = 1. Grüne Einkristalle von Na0,75Eu2Cl6 wurden erstmals als Nebenprodukt bei der Synthese von Na2EuCl5 in evakuierten Quarzglasampullen erhalten, können jedoch auch durch gezielte Reduktion von EuCl3 mit Natrium gewonnen werden. Na0,75Eu2Cl6 ist isotyp mit NaEu2Cl6 mit a = 753,69(11) pm und c = 416,3(2) pm.
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  • 3
    ISSN: 0044-2313
    Keywords: Rare Earths ; Bromides ; Copper ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of (NH4)3Cu4Ho2Br13. Further Bromides of the (NH4)3Cu4M2Br13 Type (M = Dy—Lu, Y) and on Rb3Cu4Ho2Br13Single crystals of (NH4)3Cu4Ho2Br13 were obtained for the first time from the reaction of CuBr with HoBr3 which was contaminated with NH4Br: cubic, space group Pn3, Z = 2, a = 1101.71(5) pm. The crystal structure may be considered as a variant of the fluorite type according to [(HoBr6)4][(NH4)6(Cu4Br)2] ≡ Ca4F8. Pure products can be prepared from the binary halides in glass ampoules at 350°C. The bromides (NH4)3Cu4M2Br13 (M = Dy—Lu, Y) and Rb3Cu4Ho2Br13 are isotypic with (NH4)3Cu4Ho2Br13.
    Notes: Einkristalle von (NH4)3Cu4Ho2Br13 wurden erstmals bei der Reaktion von CuBr mit HoBr3, das mit NH4Br „verunreinigt“ war, erhalten: kubisch, Raumgruppe Pn3, Z = 2, a = 1101,71(5) pm. Die Kristallstruktur ist gemäß [(HoBr6)4][(NH4)6(Cu4Br)2] ≡ Ca4F8 als eine Variante des Flußspat-Typs aufzufassen. Reine Produkte können aus den binären Halogeniden bei 350°C in Glasampullen dargestellt werden. Die Bromide (NH4)3Cu4M2Br13 (M = Dy—Lu, Y) und Rb3Cu4Ho2Br13 sind mit (NH4)3Cu4Ho2Br13 isotyp.
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  • 4
    ISSN: 0044-2313
    Keywords: Lithium ; Rare Earth Halides ; Crystal Structures ; Ionic Motion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Halides of the A3MX6 Type. VI. Ternary Chlorides of the Rare-Earth Elements with Lithium, Li3MCl6 (M = Tb—Lu, Y, Sc): Synthesis, Crystal Structures, and Ionic MotionSingle crystal X-ray studies on the ternary chlorides Li3ErCl6, Li3YbCl6 and Li3ScCl6 show that they crystallize in three different structure types. Li3ErCl6 (trigonal, P3ml, Z = 3, a = 1117.7(2); c = 603.6(2) pm; the chlorides with M = Tb—Tm, Y are isotypic) and Li3YbCl6 (orthorhombic, Pnma, Z = 4, a = 1286.6(1); b = 1113.2(1); c = 602.95(8) pm; Li3LuCl6 is isotypic) have very similar structures that may be derived from hexagonal closest packings of chloride ions with the cations occupying octahedral holes in part statistically. Li3ScCl6 (monoclinic, C2/m, Z = 2, a = 639.8(1); b = 1104.0(2); c = 639,1(1) pm; β = 109.89(1)°) crystallizes isotypic with Na3GdI6 and Li3ErBr6, structures that may be derived from a cubic closes packings of anions. The ionic movement in Li3YCl6 and Li3YbCl6 has been investigated by impedance and 7Li-NMR spectroscopy.
    Notes: Die ternären Chloride Li3ErCl6, Li3YbCl6 und Li3ScCl6 kristallisieren nach röntgenographischen Untersuchungen an Einkristallen in drei verschiedenen Strukturtypen. Li3ErCl6 (trigonal, P3ml, Z = 3, a = 1117,7(2); c = 603,6(2) pm; isotyp mit M = Tb—Tm, Y) und Li3YbCl6 (orthorhombisch, Pnma, Z = 4, a = 1286,6(1); b = 1113,2(1); c = 602,95(8) pm; Li3LuCl6 ist isotyp) haben sehr ähnliche Strukturen, die sich als hexagonal-dichteste Kugelpackungen von Chlorid-Ionen mit zum Teil statistischer Auffüllung der Oktaederlücken mit Kationen beschreiben lassen. Li3ScCl6 (monoklin, C2/m, Z = 2, a = 639,8(1); b = 1104,0(2); c = 639,1(1) pm; β = 109,89(1)°) kristallisiert isotyp mit Na3GdI6 und Li3ErBr6; die Anionen bilden hier eine kubisch-dichteste Kugelpackung. Die Ionenbewegung in Li3YCl6 und Li3YbCl6 wurde mittels Impedanzspektroskopie und 7Li-NMR-Spektroskopie untersucht.
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  • 5
    ISSN: 0044-2313
    Keywords: Rare Earth Halides ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Structural Variant to the NaErCl4/α-NiWO4 Type for Ternary Rare-Earth Halides NaMCl4: Synthesis and Crystal Structure of NaLuCl4Single crystals of NaLuCl4 (orthorhombic, Pbcn (Nr. 60), Z = 4, a = 618.6(1) pm, b = 1 592.2(2) pm, c = 657.0(1) pm) were grown for the first time from the binary components using the Bridgman technique. The crystal structure may be derived from a hexagonally closest packing of Cl- spheres with one half of all octahedral sites occupied by the cations Na+ and Lu3+, respectively. The close relation of the structure to that of NaErCl4 (α-NiWO4) is discussed. NaScCl4 was found to be isotypic to NaLuCl4.
    Notes: Einkristalle von NaLuCl4 (orthorhombisch, Pbcn (Nr. 60), Z = 4, a = 618,6(1) pm, b = 1 592,2(2) pm, c = 657,0(1) pm) wurden erstmals nach dem Bridgman-Verfahren aus den binären Komponenten gezüchtet. Die Kristallstruktur läßt sich von einer hexagonal-dichtesten Kugelpackung von Cl--Ionen ableiten, in der die Hälfte aller Oktaederlücken mit den Kationen Na+ bzw. Lu3+ besetzt ist. Die enge Verwandtschaft der Struktur mit jener von NaErCl4 (α-NiWO4) wird diskutiert. Mit NaScCl4 konnte ein zweiter Vertreter dieses Strukturtyps dargestellt werden.
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  • 6
    ISSN: 0044-2313
    Keywords: Ternary halides ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of the Ternary Rare Earth Chlorides Na2MCl5 (M = Sm, Eu, Gd)Single crystals of Na2EuCl5 were obtained from the melt of NaCl and EuCl3 in a 2:1.2 molar ratio by slow cooling. It crystallizes in the orthorhombic crystal system (space group Pnma) with the structure of K2PrCl5 with a = 1 204.0(3) pm, b = 833.9(3) pm, c = 768.2(3) pm, Z = 4. Pure powder samples of the compounds Na2MCl5 (M = Sm—Gd) are available by heating mixtures of the binary components below the melting point.
    Notes: Einkristalle von Na2EuCl5 erhält man durch langsames Abkühlen einer Schmelze von EuCl3 und NaCl (molares Verhältnis 1,2:2). Na2EuCl5 kristallisiert orthorhombisch (Raumgruppe Pnma) im K2PrCl5-Typ mit a = 1 204,0(3) pm, b = 833,9(3) pm, c = 768,2(3) pm, Z = 4. Pulverproben der Verbindungen Na2MCl5 (M = Sm—Gd) gewinnt man durch Tempern von Gemengen der binären Komponenten.
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  • 7
    ISSN: 0044-2313
    Keywords: Ternary halides ; synthesis ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of the Ternary Rare Earth Chlorides NaMCl4 (M = Eu - Yb, Y)Single crystals of NaErCl4 were obtained from the melt of NaCl and ErCl3 (1:1 molar ratio) by slow cooling. It crystallizes in the monoclinic crystal system (space group P2/c) with the structure of α-NiWO4 with a = 632.24(9) pm, b = 759.78(9) pm, c = 674.2(1) pm, b̃ = 92.310(3)°, Z = 2. Two preparative routes to pure powder samples of the chlorides NaMCl4 are described. At room temperature, these are found to be isotypic with NaErCl4 (M = Tm - Yb; II) while the triclinic structure of NaGdCl4 is adopted with M = Gd - Ho, Y (I). Phase transitions from one structure to the other are observed for all compounds. The transition temperatures decrease with decreasing size of the ion M3+.
    Notes: Einkristalle von NaErCl4 erhält man durch langsames Abkühlen einer Schmelze von NaCl und ErCl3 (molares Verhältnis 1:1). NaErCl4-II kristallisiert monoklin (Raumgruppe P2/c) im α-NiWO4-Typ mit a = 632,24(9) pm, b = 759,78(9) pm, c = 674,2(1) pm, b̃ = 92,310(3)°, Z = 2. Zwei Wege zu reinen Pulverproben der Chloride NaMCl4 werden beschrieben. Bei Raumtemperatur sind diese für M = Tm - Yb isotyp zu NaErCl4 (II), mit M = Gd - Ho, Y kristallisieren sie in der triklinen Struktur von NaGdCl4 (I). Beide Modifikationen lassen sich reversibel ineinander umwandeln. Die Umwandlungstemperaturen werden mit abnehmendem Ionenradius von M3+ kleiner.
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  • 8
    ISSN: 0044-2313
    Keywords: Lithium ; Rare Earth Halides ; Crystal Structure ; Ionic Conductivity ; NMR Spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Halides of the A3MX6Type. VII. The Bromides Li3MBr6 (M=Sm—Lu, Y): Synthesis, Crystal Structure, and Ionic MobilityThe bromides Li3MBr6 (M=Sm—Lu, Y) are obtained from the binary components LiBr and MBr3. They crystallize with a substitution/addition variant of the AlCl3- type of structure as was established from single crystal X-ray diffraction data for Li3ErBr6 (monoclinic, C2/m, Z = 2, a = 689.0(3), b = 1191.6(9), c = 684.2(6) pm, β = 109.77(6)°) and by powder X-ray diffraction for the remaining bromides. They are isotypic with Na3GdI6 and Li3ScCl6, respectively. Impedance spectroscopy and 7Li-NMR spectroscopy show that the lithium ions are highly mobile.
    Notes: Die Bromide Li3MBr6 (M=Sm—Lu, Y) erhält man durch Umsetzung der binären Komponenten LiBr und MBr3. Sie kristallisieren in einer Substitutions-Additions-Varianten des AlCl3-Typs, was anhand von röntgenographischen Untersuchungen an einem Einkristall von Li3ErBr6 (monoklin, C2/m, Z = 2, a = 689,0(3); b = 1191,6(9); c = 684,2(6) pm, β = 109,77(6)°) sowie an Pulverproben der übrigen Bromide nachgewiesen wurde. Sie sind isotyp mit Na3GdI6 bzw. Li3ScCl6. Impedanzmessungen und 7Li-NMR-Messungen an Pulverproben zeigen eine hohe Mobilität der Li+-Ionen.
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