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  • synthesis  (4)
  • 2,2′-Bipyridyl molybdenum difluoridedioxide  (1)
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  • 1
    Electronic Resource
    Electronic Resource
    Das cyclische Thioarsenat(III) (PPh4)2As2S6 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 979-981 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphenylphosphonium hexathiocyclodiarsenate(III) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Cyclic Thioarsenate(III) (PPh4)2As2S6The reaction of Na3AsS4 with tetraphenylphosphonium chloride in ethanol or dimethylformamide proceeds with an intramolecular redox reaction, yielding (PPh4)2As2S6. According to its X-ray crystal structure analysis (4071 reflections, R = 0.070) the anion consists of a six-membered ring of two As and four S atoms in the chair conformation. The As atoms occupy the ring positions 1 and 3, and each of them has an additional terminal S atom.
    Notes: Bei der Umsetzung von Na3AsS4 mit Tetraphenylphosphoniumchlorid in Ethanol oder Dimethylformamid tritt eine intramolekulare Redoxreaktion ein, bei der (PPh4)2As2S6 entsteht. Nach der Röntgenstrukturanalyse (4071 beobachtete Reflexe, R = 7,0%) besteht das Anion aus einem sechsgliedrigen Ring aus zwei As und vier S-Atomen in Sesselkonformation; die beiden As-Atome nehmen die Stellungen 1 und 3 ein und tragen jeweils noch ein terminales Schwefelatom.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210614
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  • 2
    Electronic Resource
    Electronic Resource
    Ein neues Syntheseverfahren für Vanadiumbronzen. Die Kristallstruktur von β—Ag0,33V2O5. Verfeinerung der Kristallstruktur von ∊—Cu0,76V2O5Professor Hartmut Bärnighausen zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 287-292 
    Details
    ISSN: 0044-2313
    Keywords: Silver vanadium bronze ; copper vanadium bronze ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Novel Means of Synthesis for Vanadium Bronzes. Crystal Structure of β—Ag0.33V2O5. Refinement of the Crystal Structure of ∊—Cu0.76V2O5Ag0.33V2O5 and Cu0.76V2O5 were obtained by heating equimolar mixtures of AgI + V2O5 (700°C) and CuI + V2O5 (525°C), respectively, in sealed quartz glass ampoules. In each case, one of the well-formed crystals served for an X-ray structure analysis. Ag0.33V2O5 has the structure known of the β phase of the vanadium bronzes, i. e. layers of edge-sharing, distorted VO6 octahedra are liked by certain common octahedron vertices, the Ag atoms randomly occupy two positions with occupation probabilities of 0.5. Cu0.76V2O5 has the previously determined structure of the ∊ phase, however, its space group is not Cm but C2/m.
    Notes: Ag0,33V2O2 und Cu0,76V2O5 wurden durch zweiwöchiges Erhitzen von äquimolaren Gemischen AgI + V2O5 (700°C) bzw. CuI + V2O (525°C) in einer Quarzglasampulle erhalten. Mit je einem der gut ausgebildeten Kristalle wurden eine Röntgenstrukturanalyse durchgeführt. Ag0,33V2O5 hat die für die β-Phase der Vanadiumbronzen bekannte Struktur, d. h. Schichten aus verzerrten, kantenverknüpften VO6-Oktaedern sind über bestimmte Oktaederecken verknüpft, die Ag-Atome nehmen statistisch zwei Atomlagen der Koordinationszahl 7 mit halber Besetzungswahrscheinlichkeit ein. Cu0,76V2O5 hat die früher bereits bestimmte Struktur der ∊-Phase, deren Raumgruppe jedoch nicht Cm sondern C2/m ist.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190211
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  • 3
    Electronic Resource
    Electronic Resource
    Neue Synthesewege für Thiohalogeno- und Cyclothioarsenate(III). Kristallstrukturen von PPh4[As2SBr6] · CH3CN und PPh4[SAsS5] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 82-88 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphenylphosphonium thiohalogenoarsenate(III) ; pentathiacyclothioarsenate(III) ; synthesis ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Novel Routes to the Synthesis of Thiohalogeno- and Cyclothioarsenates(III). Crystal Structures of PPh4[As2SBr6] · CH3CN and PPh4[SAsS5]By reactions of (PPh4)2[As2Cl8] and (PPh4)2[As2Br8] with Na2S4 in acetonitrile (PPh4)2[As2SCl6] · CH3CN and (PPh4)2[As2SBr6] · CH3CN were obtained, respectively. Using K2S5, PPh4[As2SCl5] and PPh4[SAsS5] were the products. The latter can also be obtained from PPh4[As2SCl5] and Na2S4, while PPh4[As3S3Br4] is formed from PPh4[As2SBr5] with K2S5. Two X-ray crystal structure determinations were performed. PPh4[As2SBr6] · CH3CN: triclinic, P1, Z = 2, a = 1200.4(7), b = 1507.3(6), c = 1594.4(8) pm, α = 81.59(2), β = 78.22(3), γ = 80.58(2)°, R = 0.096 for 2298 observed reflexions. The structure contains [As2SBr6]2- -ions in which the two Sb atoms are joined via one S and two Br atoms. PPh4[SAsS5]: triclinic, P1, Z = 2, a = 1133.9(4), b = 1142.5(4), c = 1186.9(5) pm, α = 102.77(4), β = 107.74(3), γ = 106.65(3)°, R = 0.043 für 2677 reflexions. In the [SAsS5]- -ion an AsS5 ring in the chair conformation is present.
    Notes: Durch Reaktionen von (PPh4)2[As2Cl8] und (PPh4)2[As2Br8] mit Na2S4 in Acetonitril wurden (PPh4)2[As2SCl6] · CH3CN bzw. (PPh4)2[As2SBr6] · CH3CN hergestellt. Mit K2S5 entstanden PPh4[As2SCl5] bzw. PPh4[SAsS5]. Letzteres ist auch aus PPh4[As2SCl5] und Na2S4 zugänglich, während PPh4[As3S3Br4] aus PPh4[As2SBr5] mit K2S5 entsteht. Zwei Kristallstrukturen wurden durch Röntgenbeugung bestimmt.PPh4[As2SBr6] · CH3CN: triklin, P1, Z = 2, a = 1200,4(7), b = 1507,3(6), c = 1594,4(8) pm, α = 81,59(2), β = 78,22(3), γ = 80,58(2)°. R = 9,6% für 2298 beobachtete Reflexe. Die Struktur enthält [As2SBr6]2- - Ionen, in denen die beiden Sb-Atome über ein S- und zwei Br-Atome miteinander verbunden sind. PPh4[SAsS5]: triklin, P1, Z = 2, a = 1133,9(4), b = 1142,5(4), c = 1186,9(5) pm, α = 102,77(4), β = 107,74(3), γ = 106,65(3)°, R = 4,3% für 2677 Reflexe. Im [SAsS5]- -Ion ist ein AsS5-Ring in Sesselkonformation vorhanden.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090316
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  • 4
    Electronic Resource
    Electronic Resource
    Die Kristallstruktur von [MoO2F2(2,2′-Bipyridyl)] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 117-120 
    Details
    ISSN: 0044-2313
    Keywords: 2,2′-Bipyridyl molybdenum difluoridedioxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of [MoO2F2(2,2′-bipyridyl)]The title compound crystallizes in the space group P21/n with a = 869.6(1), b = 1390.1(3), c = 959.0(1) pm, β = 110.967(5)°, Z = 4; structure determination with 1718 observed independent reflections, R = 0.031. The compound consists of molecules having two cis oxo ligands and a bipyridyl chelate in the MoO2 plane.
    Notes: Die Titelverbindung kristallisiert in der Raumgruppe P21/n mit a = 869,6(1); b = 1390,1(3); c = 959,0(1) pm; β = 110,967(5)°, Z = 4; Strukturbestimmung mit 1718 beobachteten unabhängigen Reflexen, R = 3,1%. Die Verbindung besitzt eine Molekülstruktur mit cis-ständigen Oxoliganden und dem Bipyridylchelat in der MoO2-Ebene.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926100119
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  • 5
    Electronic Resource
    Electronic Resource
    Tetraphenylphosphonium-Heptathiacyclo-thioarsenat(III), PPh4[SAsS7]Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 211-215 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphenylphosphonium heptathiacyclo thioarsenate(III) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetraphenylphosphonium Heptathiacyclo Thioarsenate(III), PPh4[SAsS7]From PPh4[As2SCl5] und K2S5 the title compound was obtained in acetonitrile among other products. According to an X-ray crystal structure analysis, it crystallizes in the orthorhombic space group Pna21 with a = 1 826.1(3), b = 1 312.0(2), c = 1 215.9(2) pm, Z = 4. The structure consists of PPh4+ and [SAsS7]- ions, AsS7 rings in the crown conformation as in S8 being present.
    Notes: Aus PPh4[As2SCl5] und K2S5 wurde in Acetonitril unter anderem die Titelverbindung erhalten. Nach der Röntgenstrukturanalyse mit 1474 beobachteten Reflexen (R = 7,1%, wR = 2,7%) kristallisiert sie rhombisch in der Raumgruppe Pna21; a = 1 826,1(3), b = 1 312,0(2), c = 1 215,9(2) pm, Z = 4. Die Struktur besteht aus PPh4+-und [SasS7]-Ionen, wobei AsS7-Ringe in der Kronenform wie beim S8 vorliegen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915950120
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