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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 281-286 
    ISSN: 0044-2313
    Keywords: Tetraphosphorus hexaoxide disulfide and trisulfide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Improved Syntheses, Crystal Growth, and Crystal Structure Determination of P4O6S2 and P4O6S3Syntheses and single crystal growths of the title compounds are described. Both compounds crystallize in the space group P21/c (P4O6S2: a = 11.293(4); b = 6.457(3); c = 11.588(4) Å; β = 90.29(2)°, 2 450 diffractometer data, Rw = 0.035/P4O6S3: a = 15.611(5); b = 8,303(3); c = 9.697(4) Å; β = 127.12(2)°, 2 481 diffractometer data, Rw = 0.034). The structural data for the series P4O6Sn (n = 1 - 4) thus completed are compared to their oxide analogues P4O6On (n = 1 - 4). The changes in the geometry of the P4O6-cage in course of its successive oxidation are discussed.
    Notes: Darstellung und Einkristallzucht der Titelverbindungen werden beschrieben. Beide Verbindungen kristallisieren in der Raumgruppe P21/c (P4O6S2: a = 11,293(4); b = 6,457(3); c = 11,588(4) Å; β = 90,29(2)°, 2 450 Diffraktometerdaten, Rw = 0,035/P4O6S3: a = 15,611(5); b = 8,303(3); c = 9.697(4) Å; β = 127,12(2)°, 2 481 Diffraktometerdaten, Rw = 0,034). Durch die neu gelösten Strukturen werden die Daten für das System P4O6Sn (n = 1 - 4) komplettiert und können mit denen der analog aufgebauten Oxide P4O6On (n = 1 - 4) verglichen werden. Die Veränderungen der Molekülgeometrie des zentralen P4O6-Käfigs im Zuge der schrittweisen Oxidation werden diskutiert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1203-1208 
    ISSN: 0044-2313
    Keywords: β-Sodium thiocarbonate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Modified Synthesis and Crystal Structure Determination of β-Na2CS3.β-Na2CS3 has been synthesized via a novel route from Na2S and CS2, and its crystal structure has been determined using single crystal techniques (for crystallographic informations see “Inhaltsübersicht”). Structural relations between Li2CO3 and β-Na2CS3 are discussed. The ionic conductivities are 3 · 10-11S cm-1 and 1.3 · 10-2S cm-1 at 50°C and 250°C, respectively.
    Notes: In der Literatur als β-Na2CS3 beschriebenes Natriumthiocarbonat wurde auf einem neuen Wege aus Na2S und CS2 dargestellt und die Kristallstruktur aufgeklärt (C2/c; a = 1 003,6(1) pm, b = 633,7(1) pm, c = 855,5(1) pm, β = 108,05(1)°, Z = 4,1582 unabhängige Reflexe, R = 0,034). Strukturbeziehungen zu Li2CO3 werden diskutiert. Die Ionenleitfähigkeiten betragen 3 · 10-11S cm-1 und 1,3 · 10-2S cm-1 bei 50°C bzw. 250°C.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 805-808 
    ISSN: 0044-2313
    Keywords: Lithiumtetrahydrogenorthoperiodate monohydrate ; crystal structure ; tetrahydrogenorthoperiodate Ion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Existence of the Tetrahydrogenorthoperiodate Ion. The Crystal Structure of LiH4IO6 · H2OThe crystal structure of LiH4IO6 · H2O has been determined (P1; a = 564.74(12), b = 574.41(13), c = 970.4(6) pm, α = 101.37(2), β = 96.37(2), γ = 114.72(2)°; Z = 2; 5 731 independent reflections; R = 0.038). All hydrogen-atoms were localized from difference fourier map and refined without applying constraints. Thus the existence of the tetrahydrogenorthoperiodate-ion in the solid state is proved, unambigously. The crystal structure is discussed and compared to other alkaliorthoperiodates.
    Notes: Die Kristallstruktur von LiH4IO6 · H2O wurde bestimmt (P1; a = 564,74(12), b = 574,41(13), c = 970,4(6) pm, α = 101,37(2), β = 96,37(2), γ = 114,72(2)°; Z = 2; 5 731 unabhängige Reflexe, R = 0,038). Alle Wasserstofflagen konnten aufgefunden und frei verfeinert werden und beweisen erstmals die Existenz des Tetrahydrogenorthoperiodations im Festkörper. Die Kristallstruktur wird diskutiert und mit denjenigen anderer Alkaliorthoperiodate verglichen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 95-100 
    ISSN: 0044-2313
    Keywords: Subvalent ternary silver oxide ; [Ag6]4+ cluster ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ag5GeO4, the First Subvalent Ternary Silver OxideApplying high oxygen pressure the first subvalent ternary silver oxide Ag5GeO4 was obtained (for crystallographic data c.f. “Inhaltsübersicht”). Ag5GeO4 contains tetrahedral GeO44--ions besides [Ag6]4+ clusters, which have not been observed in ternary silver oxides, so far. The electrical and magnetical properties prove the localisation of two paired electrons in each silver octahedron. The thermal decomposition occurs in two steps at 432.7 °C and 524.5°C.
    Notes: Durch Anwendung von Sauerstoffüberdruck gelang die Darstellung des ersten bezüglich Silber zweifelsfrei subvalenten Silberoxids, Ag5GeO4 (P21/n,a = 637,66(2) pm, b = 991,78(4) pm, c = 923,44(3)pm,β = 91,379(3)°, Z = 4, 2495 symmetrieunabhängige Reflexe, R = 0,061, Rw = 0,054). Ag5GeO4 enthält tetraedrische Orthogermanat-Ionen GeO44- und für ternäre Silberoxide neuartige [Ag6]4+-Cluster, neben Ag+ . Die elektrischen und magnetischen Eigenschaften belegen die Lokalisierung von jeweils zwei Elektronen in den Ag6--Einheiten. Der thermische Abbau erfolgt in zwei Stufen bei 432,7 °C und 524,5 °C.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 53-57 
    ISSN: 0044-2313
    Keywords: Dilithium trihydrogen orthoperiodate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li2H3IO6, a New Variant of the Molybdenite StructureLi2H3IO6 crystallizes in P61 (a = 529.70(8), c = 2 759.6(5) pm; Z = 6). The crystals are twinned by merohedry, described by m ‖ [001] and 2 ⊥ [001]. According to the results of an X-ray structure determination (2 778 diffractometer data, Rw = 0.047), Li2H3IO6 exhibits a layer structure, with oxygen forming a distorted variant of the sulfur partial structure in molybdenite (MoS2), however, with iodine and lithium in the more (Li) or less (I) distorted octahedral holes. The Li2IO6 packages are connected via strong hydrogen bonds along the edges of distorted trigonal prisms.
    Notes: Li2H3IO6 kristallisiert in der Raumgruppe P61 (a = 529,70(8), c = 2 759,6(5) pm; Z = 6). Die Kristalle sind merohedrisch verviellingt, beschrieben durch m ‖ [001] und 2 ⊥ [001]. Nach der Röntgenstrukturanalyse (2 778 unabhängige Reflexe, Rw = 0,047) liegt eine Schichtstruktur vor, in der die Sauerstoffatome eine verzerrte Variante der Schwefelteilstruktur von Molybdänit (MoS2) ausbilden, die Kationen besetzen die mehr (Li) oder weniger (I) verzerrten Oktaederlücken. Die Li2IO6-Schichtpakete werden entlang der Kanten der verzerrten trigonalen Prismen durch Wasserstoffbrückenbindungen miteinander verknüpft.
    Additional Material: 3 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 48-52 
    ISSN: 0044-2313
    Keywords: Alkali bismuth gold oxide ; preparation ; 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 NaBi2AuO5NaBi2AuO5 was obtained by hydrothermal reaction of ‘Bi2O5’, Au2O3 · 2H2O and saturated aqueous NaOH solution at temperatures from 300 to 600°C and oxygen pressure from 3 × 108 to 6 × 108 Pa for the first time. The crystal structure (P4b2; a = 1 220.02(6) pm; b = 386.68(3) pm; Z = 4; Rw = 0.022) consists of bisphenoidic distorted AuO4 groups, which are stacked in c-direction. They are connected by square pyramidal BiO5 units. Sodium is occupying holes within the Au/Bi/O framework thus formed.
    Notes: NaBi2AuO5 wurde durch Hydrothermalreaktion aus ‘Bi2O5’, Au2O3 · 2H2O und ges. wäßriger NaOH bei Temperaturen von 300 bis 600°C und Sauerstoffdrucken von 3 · 108 bis 6 · 108 Pa erstmals dargestellt. Nach den Ergebnissen der Röntgenstrukturanalyse (P4b2, a = 1 220,02(6); b = 386,68(3) pm; Z = 4; Rw = 0,022) liegen bisphenoidisch verzerrte AuO4-Gruppen vor, die in c-Richtung gestapelt sind. Die Verknüpfung erfolgt über quadratisch pyramidale BiO5-Baueinheiten. In dieser Raumnetzstruktur besetzt Natrium die vorhandenen Lücken.
    Additional Material: 4 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 163-173 
    ISSN: 0044-2313
    Keywords: Rubidiumsesquioxide ; Rb4O6 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reinvestigation of Rubidiumsesquioxide, Rb4O6Rb4O6 was prepared as a pure substance by solid state reaction between Rb2O2 and RbO2; it proves to be thermodynamically stable. The suggested structure was confirmed and refined by X-ray powder and single crystal methods (I43d; a = 932,42(4) pm; Rb4(O2-)2(O22-); Z = 4). Rb4O6 melts at 461°C followed by exothermic decomposition. The fact that O2- and O22- cannot be distinguished is discussed.
    Notes: Rb4O6 wurde durch Festkörperreaktion zwischen Rb2O2 und RbO2 erstmals röntgenrein dargestellt; es ist thermodynamisch stabil. Der bestehende Strukturvorschlag konnte durch röntgenographische Pulver- und Einkristalluntersuchungen bestätigt und verfeinert werden (I43d; a = 932,42(4) pm, Rb4(O2-)2(O22-), Z = 4). Rb4O6 schmilzt bei 461°C mit anschließender exothermer Zersetzung. Das Problem der Ununterscheidbarkeit von O2- und O22- wird diskutiert.
    Additional Material: 3 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1633-1638 
    ISSN: 0044-2313
    Keywords: Cesium cyclooctaphosphate octahydrate ; preparation ; 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 Cs8P8O24 · 8H2OCs8P8O24 · 8H2O was obtained from Na8P8O24 · 6H2O by cation exchange. Crystal growth was achieved by applying gel techniques (agar agar). The crystal structure (P1; a = 766.6(8); b = 1 156.9(9); c = 1 163.4(9) pm; α = 100,2(1)°; β = 106.5(2)°; γ = 92.2(1)°; Z = 1; 4 099 unique diffractometer data; R = 0.051; R(w) = 0.037) contains cyclo-octaphosphate anions with point symmetry C2h. The cesium atoms are coordinated irregularily by eight and ten oxygen atoms, respectively. The threedimensional linkage of the P8O248--rings is established via bonds to cesium atoms and hydrogen bonds Provided by H2O molecules.
    Notes: Cs8P8O24 · 8H2O wurde durch Kationenaustausch aus dem entsprechenden Natriumsalz gewonnen. Die Kristallzüchtung erfolgte diffusionskontrolliert (Agar-Agar-Gel). Die Kristallstruktur (P1; a = 766,6(8); b = 1 156,9(9); c = 1 163,4(9) pm; α = 100,2(1)°; β = 106,5(2)°; γ = 92,2(1)°; Z = 1; 4 099 unabhängige Reflexe; R = 0,051; R(w) = 0,037) enthält cyclo-Octaphosphatanionen mit der Punktsymmetrie C2h. Caesium ist unspezifisch mit 8 bzw. 10 Sauerstoffatomen koordiniert. Die dreidimensionale Verknüpfung der Ringe erfolgt über Koordination an Caesium und über Wasserstoffbrückenbindungen ausgehend vom Kristallwasser.
    Additional Material: 4 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1409-1412 
    ISSN: 0044-2313
    Keywords: Polyphosphate ; lithium aluminium polyphosphate ; 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 Determination of LiAl[(P2O6)2]Single crystals of previously unknown LiAl[(P2O6)2] have been obtained by reaction of Li2CO3, Al2O3 and H3PO4 (1:1:16) at 350°C. The title compound crystallizes in Pbcn (a = 1 244.54(1), b = 823.40(1), c = 892.46(1) pm; Z = 4). The least-squares refinement (with anisotropic temperature factors) was performed using 766 observed reflections yielding R = 0.029 and R(w) = 0.075. Four anion chains are running parallel to the shortest axis in the unit cell, the period of identity amounting to four. Aluminium is surrounded by an almost regular octahedron, lithium by a distorted tetrahedron of oxygen.
    Notes: Durch Umsetzung von Li2CO3, Al2O3 und H3PO4 im molaren Verhältnis 1:1:16 bei 350°C bildet sich vorher unbekanntes LiAl[(P2O6)2] einkristallin. LiAl[(P2O6)2] kristallisiert orthorhombisch in Pbcn mit a = 1 244,54(1), b = 823,40(1), c = 892,46(1) pm; Z = 4. Die Verfeinerung (mit anisotropen Temperaturfaktoren) erfolgte mit 766 beobachteten Reflexen bis zu R = 0,029 und R(w) = 0,075. Vier Phosphatketten verlaufen in der Elementarzelle mit einer Periodizität von vier parallel zu b. Aluminium ist oktaedrisch, Lithium verzerrt tetraedrisch von Sauerstoff umgeben.
    Additional Material: 3 Ill.
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