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Verbindungen in den Systemen Kalium(Rubidium)/Gold/Antimon: K3Au3Sb2, Rb3Au3Sb2 und K1,74Rb0,26RbAu3Sb2Professor Herbert Jacobs zum 60. Geburtstag gewidmet (1996)

Müller, Jürgen ; Zachwieja, Uwe

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 622 (1996), S. 635-639

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ISSN: 0044-2313

Keywords: Alkali metal gold antimon ; synthesis ; single-crystals ; crystal structure ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Compounds in the Systems Potassium(Rubidium)/Gold/Antimony: K3Au3Sb2, Rb3Au3Sb2, and K1,74Rb0,26RbAu3Sb2Brittle, silver coloured single crystals of K3Au3Sb2, Rb3Au3Sb2 and K1,74Rb0,26RbAu3Sb2 were obtainded by reaction of the alkali metal azides (KN3, RbN3) with gold and antimon powder at 550°C. The structures of the isotypic compounds (R3m, Z = 3) were determined by X-ray single-crystal diffractometer data: K3Au3Sb2, a = 6,198(2) Å, c = 21,520(5) Å, R/Rw (w = 1) = 0,046/0,058, Z(F02) ≥ 3σ(F02) = 175, Z(Var.) = 14; Rb3Au3Sb2, a = 6,443(3), c = 21,69(2), R/Rw (w = 1) = 0,059/0,082, Z(F02) ≥ 3σ(F02) = 258, Z(Var.) = 14; K1,74Rb0,26RbAu3Sb2, a = 6,288(2) Å, c = 21,617(5) Å, R/Rw (w = 1) = 0,049/0,069, Z(F02) ≥ 3σ(F02) = 390, Z(Var) = 14. The compounds crystallize with the K3Cu3P2-structure type. The Au—Sb partial structures consist of ∞2[AuSb2/3] layers with linear Sb—Au—Sb dumb-bells and SbAu3 pyramids. The layers are separated by two crystallographically independent alkali metal atoms along [001].

Notes: Spröde, silberfarbene Einkristalle von K3Au3Sb2, Rb3Au3Sb2 und K1,74Rb0,26RbAu3Sb2 wurden durch Reaktion der Alkalimetallazide (KN3, RbN3) mit Gold- und Antimonpulver bei 550°C erhalten. Die Strukturen der isotypen Verbindungen (R3m, Z = 3) wurden aus Einkristall-Röntgen-Diffraktometerdaten bestimmt: K3Au3Sb2, a = 6,198(2) Å, c = 21,520(5) Å, R/Rw (w = 1) = 0,046/0,058, Z(F02) ≥ 3σ(F02) = 175, Z(Var.) = 14; Rb3Au3Sb2, a = 6,443(3), c = 21,69(2), R/Rw (w = 1) = 0,059/0,082, Z(F02) ≥ 3σ(F02) = 258, Z(Var.) = 14; K1,74Rb0,26RbAu3Sb2, a = 6,288(2) Å, c = 21,617(5) Å, R/Rw (w = 1) = 0,049/0,069, Z(F02) ≥ 3σ(F02) = 390, Z(Var) = 14. Die Verbindungen kristallisieren im K3Cu3P2-Typ. Die Au—Sb-Teilstruktur besteht aus ∞2[AuSb2/3]-Schichten mit linearen Sb—Au—Sb-Hanteln und SbAu3-Pyramiden. Die Schichten werden längs [001] durch zwei kristallographisch unterschiedliche Alkalimetallatome separiert.

Additional Material: 4 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19966220411

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Isotype Strukturen einiger Hexaamminmetall(II)-halogenide von 3d-Metallen: [V(NH3)6]I2, [Cr(NH3)6]I2, [Mn(NH3)6]Cl2, [Fe(NH3)6]Cl2, [Fe(NH3)6]Br2, [Co(NH3)6]Br2 und [Ni(NH3)6]Cl2 (1996)

Eßmann, Ralf ; Kreiner, Guido ; Niemann, Anke ; [et al.]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 622 (1996), S. 1161-1166

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ISSN: 0044-2313

Keywords: Hexaammine metal(II) halides, [M(NH3)6]X2 ; single crystal structure determinations ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: The Structures of some Hexaammine Metal(II) Halides of 3 d Metals: [V(NH3)6]I2, [Cr(NH3)6]I2, [Mn(NH3)6]Cl2, [Fe(NH3)6]Cl2, [Fe(NH3)6]Br2, [Co(NH3)6]Br2 and [Ni(NH3)6]Cl2Crystals of yellow [V(NH3)6]I2 and green [Cr(NH3)6]I2 were obtained by the reaction of VI2 and CrI2 with liquid ammonia at room temperature. Colourless crystals of [Mn(NH3)6]Cl2 were obtained from Mn and NH4Cl in supercritical ammonia. Colourless transparent crystals of [Fe(NH3)6]Cl2 and [Fe(NH3)6]Br2 were obtained by the reaction of FeCl2 and FeBr2 with supercritical ammonia at 400°C. Under the same conditions orange crystals of [Co(NH3)6]Br2 were obtained from [Co2(NH2)3(NH3)6]Br3. Purple crystals of [Ni(NH3)6]Cl2 were obtained by the reaction of NiCl2 · 6H2O and NH4Cl with aqueous NH3 solution. The structures of the isotypic compounds (Fm3m, Z = 4) were determined from single crystal diffractometer data (see “Inhaltsübersicht”).All compounds crystallize in the K2[PtCl6] structure type. In these compounds the metal ions have high-spin configuration. The orientation of the dynamically disordered hydrogen atoms of the ammonia ligands is discussed.

Notes: Durch Umsetzungen von VI2 und CrI2 mit flüssigem Ammoniak bei Raumtemperatur wurden gelbe Kristalle von [V(NH3)6]I2 bzw. grüne von [Cr(NH3)6]I2 erhalten. Farbloses [Mn(NH3)6]Cl2 wurde durch Umsetzung von Mn mit NH4Cl in überkritischem Ammoniak einkristallin dargestellt. Farblose und transparente Kristalle von [Fe(NH3)6]Cl2 und [Fe(NH3)6]Br2 konnten durch Umsetzung von FeCl2 bzw. FeBr2 in überkritischem Ammoniak bei 400°C erhalten werden. Wird unter den gleichen Bedingungen Tri-μ-amido-bis[triammincobalt(III)]-bromid mit Ammoniak umgesetzt, so entstehen u.a. orangefarbene Kristalle von [Co(NH3)6]Br2. Violette Einkristalle von [Ni(NH3)6]Cl2 wurden durch Umsetzung von NiCl2 · 6 H2O mit NH4Cl in wäßriger NH3-Lösung erhalten.Die Strukturen der isotypen Verbindungen [M(NH3)6]X2 (Fm3m, Z = 4) wurden aus Röntgen-Einkristall-Diffraktometerdaten bestimmt: Alle Verbindungen kristallisieren im K2[PtCl6]-Typ. Die Zentralatome liegen in den oktaedrischen Komplexen in high-spin Konfiguration vor. Die Orientierung der dynamisch fehlgeordneten Wasserstoffatome der Ammoniakliganden wird diskutiert.

Additional Material: 4 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19966220709

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NaAuGe, ein weiteres ternäres Aurid mit ethan-analogen Ge2Au6-Baueinheiten (1996)

Zachwieja, Uwe

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 622 (1996), S. 1173-1176

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ISSN: 0044-2313

Keywords: Sodium auride germanide ; synthesis ; single-crystals ; crystal structure ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: NaAuGe, a Further Ternary Auride with Ethane Analogous Ge2Au6 Building UnitsBlack, brittle single crystals of NaAuGe were obtained by the reaction of NaN3, gold sponge and germanium at 800°C. The structure was determined from X-ray single-crystal diffractometry data: space group Imm2, Z = 4, a = 4.422(1) Å, b = 7.238(2) Å, c = 7.531(2) Å, R1/wR2 = 0.0195/0.0482, N(Fo2) ≥ 2σ(Fo2) = 811 and N(var.) = 21.NaAuGe crystallizes in a new ternary variant of the KHg2 (CeCu2)structure type. Gold and germanium form puckered ∞2[AuGe3/3] layers with trigonal planar coordinated gold. The ∞2[AuGe3/3] nets are connected to a framework structure via Ge - Ge contacts along [010] which consist of ethane analogous Ge2Au6 building units. The sodium atoms are placed in channels of the Au - Ge framework structure which run along [100] and [010].

Notes: Schwarze, spröde Einkristalle von NaAuGe wurden durch Umsetzung von NaN3, Goldschwamm und Germanium bei 800°C erhalten. Die Struktur wurde aus Röntgen-Einkristall-Diffraktometerdaten bestimmt: Raumgruppe Imm2, Z = 4, a = 4,422(1) Å, b = 7,238(2) Å, c = 7,531(2) Å, R1/wR2 = 0,0195/0,0482, Z(Fo2) ≥ 2σ(Fo2) = 811 and Z(Var.) = 21.NaAuGe kristallisiert in einer neuen ternären Variante des KHg2 (CeCu2)-Typs. Gold und Germanium bilden stark gewellte ∞2[AuGe3/3]-Netze mit trigonal planar koordiniertem Gold. Die ∞2[AuGe3/3]-Netze werden über Ge - Ge-Kontakte die aus ethan-analogen Ge2Au6-Baueinheiten bestehen, entlang [010] zu einer Gerüststruktur verbunden. Natrium befindet sich in Kanälen der Au - Ge-Gerüststruktur, die längs [100] und [010] verlaufen.

Additional Material: 3 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19966220711

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