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  • Crystal structure  (6)
  • preparation  (4)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1466-1470 
    ISSN: 0044-2313
    Keywords: Synthesis ; Crystal structure ; Halides ; Clusters ; Lanthanides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Bromide with Trigonal-Bipyramidal [M5(C2)] Clusters: [Pr5(C2)]Br9The bromide [Pr5(C2)]Br9 is obtained via metallothermic reduction of PrBr3 with rubidium in the presence of praseodymium and carbon in a sealed niobium container at 730°C as dark red single crystals. [Pr5(C2)]Br9 crystallizes in the monoclinic crystal system [P21/n; Z = 4; a = 1 006.9(1); b = 1 886.1(1); c = 1 045.9(1) pm; β = 108.130(1)°; Rint = 0.059; R1 = 0.038; wR2 = 0.077]. One edge in the base of the trigonal bipyramid in [Pr5(C2)]Br9 is usually long (440 pm). It is not brigded by a Bri ligand. In addition to the eight Bri, the cluster is coordinated by 12 terminal ligands (Bra). Except for the known Bra-a-a and Bri-a connections, Bri-a-a brigdes are observed for the first time for trigonal-bipyramidal clusters.
    Notes: Das Bromid [Pr5(C2)]Br9 erhält man durch metallothermische Reduktion von PrBr3 mit Rubidium in Gegenwart von Praseodym und Kohlenstoff in einer verschweißten Niobampulle bei 730°C in Form dunkelroter Kristalle. [Pr5(C2)]Br9 kristallisiert im monoklinen Kristallsystem [P21/n; Z = 4; a = 1 006,9(1); b = 1 886,1(1); c = 1 045,9(1) pm; β = 108,130(1)°; Rint = 0,059; R1 = 0,038; wR2 = 0,077]. Eine Kante in der Basis der trigonalen Bipyramide in [Pr5(C2)]Br9 ist mit 440 pm ungewöhnlich lang und wird nicht von einem Bri-Liganden überbrückt. Zusätzlich zu den acht Bri werden die Cluster von 12 terminalen Liganden koordiniert (Bra). Neben den bekannten Bra-a-a- und Bri-a-Brücken treten hier erstmals bei trigonal-bipyramidalen Clustern Bri-a-a-Brücken auf.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 79-83 
    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.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 89-92 
    ISSN: 0044-2313
    Keywords: Calcium oxychloride ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: An Oxychloride of Calcium: Ca4OCl6Ca4OCl6 (hexagonal, P63mc, Z = 2), a = 905.8(3), c = 686.3(4) pm, (R = 0.031) crystallizes as colourless needles from reducing melts (CaCl2, Ca) that contain small amounts of „oxygen“. It contains „isolated“ tetrahedral units [Ca4O] and is isotypic with e.g., Ba4OCl6, Yb4OCl6 and K6HgS4. Ca4OCl6 does not form in the dehydration process of, for example, CaCl2 · 6 H2O.
    Notes: Ca4OCl6 (hexagonal, P63mc, Z = 2, a = 905.8(3)); c = 686.3(4) pm, (R = 0,031) kristallisiert in Form farbloser Nadeln aus „reduzierenden Schmelzen“ (CaCl2, Ca), die wenig „Sauerstoff“ enthalten. Es enthält „isolierte“ tetraedrische [Ca4O]-Einheiten und ist isotyp mit z. B. Ba4OCl6, Yb4OCl6 oder K6HgS4. Ca4OCl6 entsteht nicht beim Entwässern von z. B. CaCl2 · 6 H2O.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 614 (1992), S. 12-16 
    ISSN: 0044-2313
    Keywords: Europium(II) acetate ; Synthesis ; Crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: KEu(CH3COO)3, the First Ternary Europium(II) AcetateOn of EuCl2 with a melt of dry potassium acetate yields pale greenish-yellow single crystals (300°C, sealed glass ampoule, EuCl2 and K(CH3COO) in a molar ratio of 1 : 3). The crystal structure determination (orthorhombic, P212121 (no. 19), Z = 8, a = 1166.3(1) pm, b = 1288.4(2) pm, c = 1493.9(2) pm, R = 0.043, Rw = 0.032) revealed the composition KEu(CH3COO)3. The structure consists of one-dimensional chains built up by bridging acetate groups in the [100] and [001] directions in which potassium and europium alternate as central atoms. Eu2+ is surrounded by nine and eight and K+ by seven and six oxygen atoms, respectively. These chains are linked in the [010] direction so that a three-dimensional network is formed. The high coordination numbers of the acetate oxygen atoms of up to four are remarkable. Therefore, the acetate groups have highly bridging functions in addition to their chelating coordination of the cations.
    Notes: Bei der Umsetzung von EuCl2 mit einer Schmelze von trockenem Kaliumacetat im ungefähren Molverhältnis von 1 : 3 entstehen bei 300°C in einer abgeschmolzenen Glasampulle neben KCl blaß grünlichgelbe Kristalle. Die Röntgenstrukturanalyse (orthorhombisch, P212121 (Nr. 19), Z = 8, a = 1166,3(1) pm, b = 1288,4(2)pm, c = 1493,9(2)pm, R = 0,043, Rw = 0,032) ergab die Zusammensetzung KEu(CH3COO)3. Die Kristallstruktur wird von acetatverbrückten unendlichen Strängen in Richtung [100] und [001] bestimmt, in denen abwechselnd Kalium und Europium als Zentralteilchen aufeinanderfolgen. Dabei wird Eu2+ von 9 bzw. 8 Sauerstoffliganden, K+ aber nur von 7 bzw. 6 Sauerstoffatomen koordiniert. Durch zusätzliche Verknüpfungen der Stränge in Richtung [010] entsteht daraus ein dreidimensionales Netzwerk. Auffällig sind die ungewöhnlich großen Koordinationszahlen der Acetatsauerstoffatome von bis zu vier, so daß bei den Acetatgruppen neben der chelatisierenden Koordination zu den Kationen ihre Funktion als Brückenliganden im Vordergrund steht.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 141-144 
    ISSN: 0044-2313
    Keywords: Crystal structure ; Synthesis ; Thermolysis, Lanthanides ; Ternary ammonium nitrates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and Thermolysis of the (NH4)3[M2(NO3)9] (M = La—Gd)The ternary ammonium nitrates (NH4)3[M2(NO3)9] (M = La-Gd) are obtained as single crystals from a solution of the respective sesquioxides in a melt of NH4NO3 and sublimation of the excess NH4NO3. In the crystal structure of (NH4)3[Pr2(NO3)9] (cubic, P4332, Z = 4, a = 1 377.0(1) pm, R = 0.038, Rw = 0.023) Pr3+ is surrounded by six bidentate nitrate ligands of which three are bridging to neighbouring Pr3+ ions. This results in a branched folded chain, held together by the NH4+ ions which occupy cavities in the structure. (NH4)3[Pr2(NO3)9] is the first intermediate product of the thermal decomposition of (NH4)2[Pr(NO3)5(H2O)2] · 2H2O.
    Notes: Die ternären Ammoniumnitrate (NH4)3[M2(NO3)9] (M = La—Gd) erhält man in Form von Einkristallen durch Auflösen der entsprechenden Sesquioxide in einer Schmelze von NH4NO3 und Entfernen des Überschusses durch Sublimation. Die Strukturanalyse am Beispiel von (NH4)3[Pr2(NO3)9] (kubisch, P4332, Z = 4; a = 1377,0(1) pm; R = 0,038; Rw = 0,023) zeigt, daß Pr3+ von sechs zweizähnigen Nitratliganden umgeben ist, von denen drei jeweils zu einem weiteren Pr3+-Ion verbrücken. Dadurch entsteht eine verzweigte, gefaltete Kette. Sie wird durch NH4+-Ionen zusammengehalten, die sich in Hohlräumen befinden. (NH4)3[Pr2(NO3)9] stellt die erste Stufe beim thermischen Abbau von (NH4)2[Pr(NO3)9(H2O)2] · 2H2O dar.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 20-22 
    ISSN: 0044-2313
    Keywords: Crystal structure ; lanthanides ; adducts ; complex nitrates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cs4[La(NO3)6](NO3) · HNO3: The First Nitric Acid Adduct of a Ternary Alkali Lanthanide NitrateIn the crystal structure of Cs4[La(NO3)6](NO3). HNO3 (monoclinic, P21/c, Z = 2, a = 787.3(2); b = 1353.0(3); c = 1141.8(7) pm; β = 94,37(3)°) La3+ has a coordination number of twelve (six bidentate nitrate ligands). The structure may be viewed at as a layer structure: Layers of the composition [Cs(1)4La2(NO3)12]2-, and [Cs(2)4(NO3)2(HNO3)2]2+ are stacked alternatively in the [100] direction.
    Notes: In der Kristallstruktur von Cs4[La(NO3)6](NO3) · HNO3 (monoklin, P21/c, Z = 2, a = 787,3(2); b = 1353,0(3); c = 1141,8(7)pm; β = 94,37(3)°) hat La3+ die Koordinationszahl zwölf (sechs zweizähnige Nitratliganden). Sie kann als Schichtstruktur aufgefaßt werden: Zwischen Schichten der Zusammensetzung [Cs(1)4La2(NO3)12]2-, die längs [100] gestapelt sind, liegen Cs(2)+- und NO3--Ionen sowie HNO3-Moleküle, die ihrerseits Schichtpakete [Cs(2)4(NO3)2(HNO3)2]2+ bilden.
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  • 7
    ISSN: 0044-2313
    Keywords: Rhenium ; rubidium rhenium halide hydrates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O, a Mixed Halide-Hydrate with the Anionic Dimer {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2-[Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O crystallizes as dark redbrown single crystals from an hydrobromic-acid solution of ReCl3 and RbBr at 0°C. An important feature of the crystal structure (monoclinic, C2/c; a = 1494.61(8); b = 835.71(4); c = 3079.96(19) pm; β = 97.801(4)°; Vm = 573.9(4) cm3mol-1; R = 0.060; Rw = 0.038) is the connection of two anions [Re3(μ-Cl)3Br7(H2O)2]- via a water molecule to dimers, {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2-. These dimeric units are contained in slabs that are stacked in the [001] direction and held together by Rb+ cations and crystal water.
    Notes: [Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O kristallisiert in dunklen, rotbraunen Einkristallen aus bromwasserstoffsaurer Lösung von Rheniumtrichlorid und Rubidiumbromid bei 0°C. Ein wichtiges Merkmal der Kristallstruktur (monoklin; C2/c; a = 1494,61(8); b = 835,71(4); c = 3079,96(19) pm; β = 97,801(4)°; Vm = 573,9(4) cm3mol-1; R = 0,060; Rw = 0,038) ist die Verknüpfung zweier Anionen [Re3(μ-Cl)3Br7(H2O)2]- über ein Wassermolekül zu Dimeren {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2-. Diese dimeren Baugruppen sind zu Schichtpaketen zusammengefaßt, die längs [001] gestapelt und über die Rb+-Ionen in Gemeinsamkeit mit Kristallwasser verbunden sind.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 31-37 
    ISSN: 0044-2313
    Keywords: Alkali-iodoindates(III) ; indium ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of the Alkali-tetraiodoindates(III), AInI4 (A = Li, K, Rb, Cs)Single crystals of the yellow alkaliiodoindates(III), AInI4 (A = Li, K, Rb, Cs), are obtained from mixtures of the binary components by slow cooling of the melts. LiInI4 is isotypic with LiAlCl4: monoclinic, P21/c, Z = 4; a = 838.9(4); b = 751.2(3); c = 1526,7(8) pm; β = 92.67(4)°. KInI4 belongs to the ATIX4 type of structure (A = NH4, K, Rb; X = Br, I): cubic, F4 3c, Z = 24; a = 1990.8(1) pm. RbInI4 crystallizes with the β-GaBr2 type: trigonal, R3c, Z = 18; a = 2452.6(6); c = 978.6(4) pm. CsInI4 is isostructural with CsTII4: monoclinic, P21/c, Z = 4; a = 738.4(1); b = 1875.7(3); c = 853.6(2) pm; β = 105.75(2)°. In all structures almost regular tetrahedral polyhedra [InI4]- occur. The coordination numbers of the alkali cations cover the wide range from 6 (Li+) via 9 (Rb+) and 11 (Cs+) to 12 (K1+).
    Notes: Einkristalle der gelben Iodoindate(III) der Alkalimetalle, AInI4 (A = Li, K, Rb, Cs), erhält man aus Gemengen der binären Komponenten durch langsames Abkühlen der Schmelzen. LiInI4 ist isotyp mit LiAlCl4: monoklin, P21/c, Z = 4; a = 838,9(4); b = 751,2(3); c = 1526,7(8) pm; β = 92,67(4)°. KInI4 gehört zum ATIX4-Typ (A= NH4, K, Rb; X= Br, I): kubisch, F4 3c, Z = 24; a = 1990,8(1) pm. RbInI4 kristallisiert im β-Ga[GaBr4]-Typ: trigonal, R3c, Z = 18; a = 2452,6(6); c = 978,6(4) pm. CsInI4 ist isotyp mit CsTII4: monoklin, P21/c, Z = 4; a = 738,4(1); b = 1875,7(3); c = 853,6(2) pm; β = 105,75(2)°. Stets liegen annähernd tetraedrische Baugruppen [InI4]- vor. Die Koordinationszahlen der Alkali-Kationen überstreichen das Spektrum von 6 (Li+) über 9 Rb+, 11 (Cs+) bis 12 (K1+).
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  • 9
    ISSN: 0044-2313
    Keywords: Alkali uranium halides, A2UX5 (A = K, Rb; X = Cl, Br, I) ; preparation ; crystal structure ; magnetic susceptibility ; UV-Vis spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese, Kristallstruktur, Magnetismus und Absorptionsspektren von Halogeniden des Typs A2UX5 (A = K, Rb; X = Cl, Br, I)Die ternären Uran(III)-halogenide A2UX5 (A = K, Rb; X = Cl, Br, I) wurden aus den binären Komponenten AX und UX3 in verschweißten Tantalampullen gewonnen. Nach Guinier-Aufnahmen (Raumtemperatur) kristallisieren sie sämtlich im K2PrCl5/Y2HfS5-Typ. Einkristall-Strukturverfeinerungen wurden für K2UI5 und Rb2UCl5 unternommen. Magnetische Suszeptibilitätsmessungen erfolgten mit einem SQUID-Magnetometer von Raumtemperatur bis zur Temperatur des flüssigen Heliums: Eindimensionale (innerhalb einer Kette) und dreidimensionale antiferromagnetische Ordnung wird bei tiefen Temperaturen, abhängig vom Abstand U3+—U3+, beobachtet. Absorptionsspektren wurden zwischen 4000 und 28000 cm-1 aufgenommen. Sie zeigen die für U3+ charakteristischen Übergänge und, abhängig vom Halogenid, sehr starke f - d Übergänge oberhalb 14000 bzw. 15000 cm-1.
    Notes: The ternary uranium(III) halides A2UX5 (A = K, Rb; X = Cl, Br, I) have been prepared from the binary components AX and UX3 in sealed tantalum containers. According to their Guinier X-ray powder patterns, they all crystallize with the K2PrCl5/Y2HfS5 type of structure. Lattice constants for ambient temperature are reported. Single-crystal structure refinemens were undertaken for K2UI5 and Rb2UCl5. Magnetic susceptibility data were recorded with a SQUID magnetometer from liquid helium to room temperature. One-dimensional (intrachain) and three-dimensional antiferromagnetic ordering occur at low temperatures dependent upon the U3+—U3+ distance. Absorption spectra were recorded between 4 000 and 28 000 cm-1. They show f - f transitions typical for U3+ and, depending on the halide, very strong f - d transitions above 14 000 to 15 000 cm-1, respectively.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1493-1495 
    ISSN: 0044-2313
    Keywords: Synthesis ; Crystal structure ; Crown ether ; Lanthanides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [La2I2(OH)2(dibenzo-18-crown-6)2]I(I3), a Cationic Dimeric in-cavity Complex with Iodide and Triiodide as AnionsSingle crystals of [La2I2(OH)2(dibenzo-18-crown-6)2]I(I3) are obtained from the reaction of LaI3 and dibenzo-18-crown-6 in acetonitrile. The crystal structure monoclinic, C2/m, Z = 4, T = 293 [100] K, a = 2179(3) [2162.3(3)], b = 1070.3(3) [1069.6(1)], c = 1118.2(3) [1110.6(1)] pm, β = 93.1(1) [92.83(1)]°, R1 = 0.0601 [0.0411], wR2 = 0.1449 [0.1014] contains hydroxide-bridged cationic dimers and iodide as well as triiodide as anions.
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