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  • 1
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur der “Fluorid-Ammoniakate“ Zr(NH3)F4 und Hf(NH3)F4 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 79-83 
    Details
    ISSN: 0044-2313
    Keywords: Crystal structure ; synthesis ; ammine complexes ; fluoride ; zirconium ; hafnium ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of the Fluoride-Ammine Complexes Zr(NH3)F4 and Hf(NH3)F4Colourless, easily cleavable single crystals of Zr(NH3)F4 and Hf(NH3)F4 without special shape are obtained by oxidation of zirconium and hafnium metal powder with NH4HF2 (molar ratio 1 : 2) in sealed Monel ampoules at reaction temperatures of 380-450°C. The two fluorideammine complexes crystallize isotypically in the triclinic space group P1 (no. 2) with a = 601.4(1)/597.8(8) pm [Zr(NH3F4)/Hf(NH3)F4], b = 802.8(2)/800.6(12) pm, c = 862.3(2)/860.8(8) pm, α = 106.39(1)/106.19(10)°, β = 104.25(1)/104.51(9)°, γ = 106.83(1)/106.69(11)°, Z = 4. Bicapped trigonal prisms [M(NH3)F7] are connected via edges and corners to form corrugated layers that are held together by hydrogen bonding.
    Notes: Farblose, leicht spaltbare Einkristalle von Zr(NH3)F4 und Hf(NH3)F4 ohne ausgeprägten Habitus erhält man durch Oxidation von Zirconium- bzw. Hafnium-Metallpulver mit NH4HF2 (molares Verhältnis 1:2) in verschweißten Monelampullen bei Reaktionstemperaturen von 380-450°C. Die beiden Ammoniakate kristallisieren isotyp in der triklinen Raumgruppe P1 (Nr. 2) mit a = 601,4(1)/597,8(8) pm [Zr(NH3)F4/Hf(NH3)F4], b = 802,8(2)/800,6(I2) pm, c = 862,3(2)/860,8(8) pm, α = 106,39(1)/106,19(10)°, β = 104,25(1)/104,51(9)°, γ = 106,83(1)/106,69(11)°, Z = 4. Es liegen zweifach bekappte trigonale Prismen [M(NH3)F7] (M = Zr, Hf) vor, die über gemeinsame Kanten und Ecken zu gewellten Schichten verknüpft sind, die ihrerseits über Wasserstoffbrückenbindungen zusammengehalten werden.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230114
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  • 2
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen von NH4[Si(NH3)F5] und [Si(NH3)2F4]Professor Roger Blachnik zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1646-1650 
    Details
    ISSN: 0044-2313
    Keywords: Synthesis ; crystal structures ; complex fluorides ; silicon ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of NH4[Si(NH3)F5] and [Si(NH3)2F4]Single crystals of NH4[Si(NH3)F5] and [Si(NH3)2F4] are obtained by reaction of silicon powder with NH4HF2 in sealed Monel ampoules at 400°C. NH4[Si(NH3)F5] crystallizes with the tetragonal space group P4/n (no. 85) with a = 614.91(7) pm, c = 721.01(8) pm, Z = 2. Characteristic for the structure is the anionic octahedron [Si(NH3)F5]-. Si(NH3)2F4 crystallizes with the monoclinic space group P21/c (no. 14) with a = 506.9(1) pm, b = 728.0(1) pm, c = 675.9(1), β = 93,21(2)°, Z = 2. Trans-[Si(NH3)2F4] molecules are characteristic for this structure.
    Notes: Einkristalle von NH4[Si(NH3)F5] und Si(NH3)2F4 erhält man durch Umsetzung von pulverförmigem Silicium mit NH4HF2 in verschlossenen Monelampullen bei 400°C. NH4[Si(NH3)F5] kristallisiert tetragonal in der Raumgruppe P4/n (Nr. 85) mit a = 614,91(7) pm, c = 721,01(8) pm; Z = 2. Charakteristische Baueinheit ist der anionische Oktaeder [Si(NH3)F5]-. Si(NH3)2F4 kristallisiert monoklin in der Raumgruppe P21/c (Nr. 14) mit a = 506,9(1) pm, b = 728,0(1) pm, c = 675,9(1), β = 93,21(2)°, Z = 2. Es liegt eine Molekülstruktur mit trans-[Si(NH3)2F4]-Oktaedern vor.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966221005
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  • 3
    Electronic Resource
    Electronic Resource
    Kristallstruktur von (NH4)3SnF7: Ein Doppelsalz gemäß (NH4)3[SnF6]F und kein (NH4)4SnF8 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1347-1348 
    Details
    ISSN: 0044-2313
    Keywords: Ammonium Tin Fluorid ; Crystal Structure ; Fluorides ; Tin ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Crystal Structure of (NH4)3SnF7: A Double Salt According to (NH4)3[SnF6]F and not (NH4)4SnF8(NH4)3SnF7 is obtained as colourless single crystals from the reaction of NH4HF2 with tin powder at 300°C. The crystal structure (cubic, Pm3m, Z = 1, a = 602.5(1) pm at 293 K; a = 598.0(1) pm at 100 K) contains [SnF6]2- octahedra and lonesome F- ions surrounded by NH4+ cations only; it may be considered as a derivative of the Cu3Au-type of structure according to Cu3[Au]□ ≡(NH4)3[SnF6]F. The F- ions of the [SnF6]2- octahedra with their Sn4+ centre in the origin of the unit cell at m3m are disordered in different ways at 293 and 100 K, respectively.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230903
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  • 4
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur von NH4DyF4. Über weitere Fluoride NH4MF4 (M = La—Tb) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1393-1398 
    Details
    ISSN: 0044-2313
    Keywords: Rare Earth Fluorides ; Crystal Structure ; Ammonium Fluorides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of NH4DyF4. Further Fluorides NH4MF4 (M = La—Tb)
    Notes: Die Fluoride NH4MF4 (M = La—Dy) entstehen bei der Umsetzung der Metalle M mit N2H6F2 bei Temperaturen zwischen 80 und 350°C in verschweißten Monelampullen. Es werden in Abhängigkeit vom Selten-Erd-Element und von der Reaktionstemperatur drei Strukturen beobachtet: Die Kristallstruktur der Form I wurde anhand von Einkristallen von NH4DyF4 aufgeklärt [orthorhombisch, Pbcm (Nr. 57), Z = 4; a = 852,10(7) pm, b = 722,54(8) pm, c = 626,28(12) pm]; die bei niedrigen Temperaturen hergestellten Fluoride NH4MF4 (M = Ce—Tb) sind isotyp. Bei höheren Temperaturen treten die Formen II [für M = La—Nd; orthorhombisch (?), Z = 8] bzw. III [M = Eu—Tb, geordnete Überstruktur zum CaF2-Typ, analog TlGdF4, tetragonal, P4/m (?), Z = 16] auf.The fluorides NH4MF4 (M = La—Dy) are obtained through the reaction of the metals M with N2H6F2 at temperatures between 80 and 350°C in sealed Monel ampoules. Dependent upon the rare-earth element M and the reaction temperature three crystal structures are observed: The crystal structure of modification I was determined from single crystal data of NH4DyF4 [orthorhombic, Pbcm (no. 57), Z = 4; a = 852.10(7) pm, b = 722.54(8) pm, c = 626.28(12) pm]; the fluorides NH4MF4 (M = Ce—Tb) obtained at fairly low temperatures are isotypic. At higher temperatures the modifications II [for M = La—Nd; orthorhombic (?), Z = 8] and III [M = Eu—Tb, ordered superstructure of the CaF2 type, analogous to TlGdF4, tetragonal, P4/m (?), Z = 16] are observed.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230913
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