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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.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 201-206 
    ISSN: 0044-2313
    Keywords: Ternary oxides ; anionic gold ; Cs3AuO ; Rb3AuO ; K3AuO ; preparation ; single-crystal structure determination ; analysis of molar volumes ; electrical conductivity ; magnetic properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Oxides containing Anionic GoldThe preparation and crystal structure of the novel ternary oxides M3AuO (M = Cs, Rb, K) containing anionic gold is reported. Cs3AuO (a = 7.830(1) Å, c = 7.060(1) Å) crystallizes as a hexagonal, Rb3AuO (a = 5.501(1) Å) and K3AuO (a = 5.240(1) Å) as a cubic anti perovskite. Concerning to the ionic description (M+)3Au-O2- in Cs3AuO gold exists as an anion. In Rb3AuO and K3AuO the anionic character of gold decreases respectively. The analysis of bond length and molar volumes gives support to this view, as well as investigations of conductivity and magnetic properties do.
    Notes: Über die Darstellung und Kristallstrukturen der neuen ternären Oxide M3AuO (M = Cs, Rb, K) mit anionischem Gold wird berichtet. Cs3AuO (a = 7,830(1) Å, c = 7,060(1) Å) kristallisiert als hexagonaler, Rb3AuO (a = 5,501(1) Å) und K3AuO (a = 5,240(1) Å) als kubischer anti-Perowskit. Gemäß der Formulierung (M+)3Au-O2- liegt Gold in Cs3AuO als Anion vor. In den Verbindungen der leichteren Alkalimetalle nimmt der anionische Charakter von Gold sukzessiv ab. Die Analyse der Bindungslängen und Molvolumina belegt diese Sichtweise, ebenso die durchgeführten Leitfähigkeitsuntersuchungen und magnetischen Messungen.
    Additional Material: 3 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1901-1906 
    ISSN: 0044-2313
    Keywords: Tetrahydrogen mesoperiodate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li2H4I2O10, the First TetrahydrogendimesoperiodateLi2H4I2O10 has been obtained as an intermediate during the dehydration of LiH4IO6 · H2O to LiIO4, for the first time. According to the results of an X-ray structure determination (monoclinic, P21/n, a = 533.98(4), b = 471.85(4), c = 1431.48(10) pm, β = 91.614(7)°, Z = 2, 726 diffractometer data, R = 0.056), Li2H4I2O10 contains the previously unknown tetrahydrogendimesoperiodate ion H4I2O102-, consisting of two edge-shared IO6 octahedra. They are connected with LiO6 octahedra via common edges and vertices. The crystals are non-merohedrally twinned along (100).
    Notes: Li2H4I2O10 wurde als Zwischenstufe während der Entwässerung von LiH4IO6 · H2O zu LiIO4 erstmals erhalten. Nach der Röntgenstrukturanalyse (monoklin, P21/n, a = 533,98(4), b = 471,85(4), c = 1431,48(10) pm, β = 91,614(7)°, Z = 2, 726 unabhängige Reflexe, R = 0,056) liegt das bisher unbekannte Tetrahydrogendimesoperiodatanion H4I2O102- in Form zweier kantenverknüpfter IO6-Oktaeder vor, die ihrerseits mit LiO6-Oktaedern kanten- und eckenverknüpft sind. Die Kristalle sind systematisch verzwillingt. Es handelt sich um monokline Ebenenzwillinge nach (100).
    Additional Material: 4 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1803-1809 
    ISSN: 0044-2313
    Keywords: Hyponitrites ; cis-Na2N2O2 ; preparation ; properties ; crystal structure ; vibrational spectra ; 15N-MAS-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: To the Knowledge of cis-Sodium HyponitriteSurprisingly, cis-sodium hyponitrite can be prepared by reacting gaseous N2O and solid Na2O. For the first time, the structure of a simple salt of cis hyponitrous acid has been determinated unambigously. According to an abinitio structure determination based on powder data, cis-Na2N2O2 crystallizes monoclinic (P21/c, a = 5.107(1); b = 9.211(1); c = 6.159(1) Å; β = 97.91(1)°; Z = 4). Results of spectroscopic investigations (vibrational spectroscopy, 15N-MAS-NMR) agree with the symmetry of the cis-N2O22- anion as it has been proved by the crystal structure. Consider able differences regarding some chemical and physical properties have been observed for samples of cis-Na2N2O2 synthesized via different routes.
    Notes: Durch Gas-Festkörper-Reaktion von N2O und Na2O läßt sich überraschend cis-Natriumhyponitrit darstellen. Auf der Basis der so erhaltenen reinen, gut kristallisierten Präparate gelang erstmals die eindeutige strukturelle Charakterisierung eines einfachen Salzes der cis-Hyposalpetrigen Säure. Gemäß der voraussetzungsfrei anhand von Pulverdaten durchgeführten Strukturbestimmung kristallisiert cis-Na2N2O2 monoklin (P21/c, a = 5,107(1); b = 9,211(1); c = 6,159(1) Å; β = 97,91(1)°; Z = 4). Die Resultate der spektroskopischen Untersuchungen (Schwingungsspektroskopie, 15N-MAS-NMR) stehen im Einklang mit der durch die Kristallstrukturanalyse ermittelten Symmetrie des cis-N2O22--Anions. Präparate von cis-Na2N2O2, die auf verschiedenen Synthesewegen dargestellt wurden, zeigen auffallende Unterschiede in einigen chemischen und physikalischen Eigenschaften.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 6
    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.
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  • 7
    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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  • 8
    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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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 431-434 
    ISSN: 0044-2313
    Keywords: Ionic ozonides ; preparation ; P(CH3)4O3 ; As(CH3)4O3 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Knowledge of the New Ionic Ozonides P(CH3)4O3 and As(CH3)4O3P(CH3)4O3 and As(CH3)4O3 were prepared via ion exchange in liquid ammonia and characterized by X-ray-powder, IR, MS and DTA techniques. P(CH3)4O3 and As(CH3)4O3 are isotypic and have a wurtzite-like arrangement of ions with rotationally disordered O3-. (Powder data: P63mc; P(CH3)4O3: a = 687.8(2), c = 964.6(3) pm; As(CH3)4O3: a = 708.6(1), c = 991.0(3) pm). As(CH3)4O3 shows a displacive phase transition at -135°C. The low temperature phase is orthorhombic (a = 715.8(7), b = 1 209(1), c = 943.3(1) pm).
    Notes: P(CH3)4O3 und As(CH3)4O3 wurden mittels Ionenaustausch in fl. NH3 erstmals dargestellt und mit Röntgenpulvermethoden, IR-Spektroskopie, MS und DTA charakterisiert. P(CH3)4O3 und As(CH3)4O3 sind isotyp und bilden eine Ionenpackung im Wurtzit-Typ mit fehlgeordnetem O3-. (Röntgenpulverdaten: P63mc; P(CH3)4O3: a = 687,8(2), c = 964,6(3) pm; As(CH3)4O3: a = 708,6(1), c = 991,0(3) pm). As(CH3)4O3 zeigt bei - 135°C eine displazive Phasenumwandlung. Die Tieftemperaturphase hat orthorhombische Metrik (a = 715,8(7), b = 1 209(1), c = 943,3(1) pm).
    Additional Material: 2 Tab.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 484-487 
    ISSN: 0044-2313
    Keywords: Lithiummetaperiodate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Lithiummetaperiodate, LiIO4For the first time single crystals of LiIO4 were obtained. According to the results of an X-ray structure determination (monoclinic, P21/n; a = 525.5(3), b = 851.1(4), c = 796.9(5) pm, β = 104.21(3)°; Z = 4; 2 148 diffractometer data, R = 0.024) the coordination by oxygen is tetrahedral for iodine and strongly distorted trigonal bipyramidal for lithium. Two lithium-oxygen-polyhedra are connected via a common edge. LiIO4 crystallises isostructural to LiAlH4. The structure is discussed and compared to those of other metaperiodates and tetrahydridoaluminates.
    Notes: Erstmals wurden Einkristalle von LiIO4 erhalten. Nach der Röntgenstrukturanalyse (monoklin, P21/n; a = 525,5(3), b = 851,1(4), c = 796,9(5) pm, β = 104,21(3)°; Z = 4; 2 148 unabhängige Reflexe, R = 0,024) wird Iod tetraedrisch und Lithium stark verzerrt trigonal-bipyramidal von Sauerstoff koordiniert. Dabei sind jeweils zwei Lithium-Sauerstoff-Polyeder miteinander kantenverknüpft. Es besteht Isotypie zu LiAlH4. Die Struktur wird diskutiert und mit denen anderer Metaperiodate und Tetrahydridoaluminate verglichen.
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