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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 589 (1990), S. 199-206 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Acetamidiniumhexafluorometallates of Silicon, Germanium, Tin, and TitaniumThe title compounds were crystallized from the aqueous solutions of their hexafluorometallate acids by adding acetamidinium fluoride. Their unit cells were determined and for [CH3C(NH2)2]2SiF6 the thermal decomposition was investigated thermoanalytically and its crystal structure was determined: s. g. C2/m, a = 9.886(4), b = 8.742(3), c = 7.650(3) Å, β = 127.02(2)°, layer structure, R = 0.04. The unit cell parameters of [CH3C(NH2)2]2GeF6 are a = 10.002(1), b = 8.870(2), c = 7.752(2) Å, β = 127.17(1)°, of [CH3C(NH2)2]2TiF6: a = 6.914(2), b = 6.709(1), c = 6.985(2) Å, α = 105.94(2)°, β = 111.95(4)°, γ = 94.30(2)°, of [CH3C(NH2)2]2SnF6: a = 6.980(2), b = 6.799(2), c = 7.018(3) Å, α = 105.40(3)°, β = 111.80(3)°, γ = 94.14(2)°.
    Notes: Die Titelverbindungen wurden aus den wäßrigen Lösungen der jeweiligen Hexafluorometallatsäuren nach Zugabe von Acetamidiniumfluorid auskristallisiert und ihre Gitterkonstanten bestimmt. Vom [CH3C(NH2)2]2SiF6 wurde der Abbau thermoanalytisch verfolgt und die Kristallstruktur bestimmt: R. Gr. C2/m, a = 9,886(4), b = 8,742(3), c = 7,650(3) Å, β = 127,02(2)°, Schichtstruktur, R = 0,04. Kristallographische Daten von [CH3C(NH2)2]2GeF6: a = 10,002(1), b = 8,870(2), c = 7,752(2) Å, β = 127,17(1)°, von [CH3C(NH2)2]2TiF6: a = 6,914(2), b = 6,709(1), c = 6,985(2) Å, α = 105,94(2)°, β = 111,95(4)°, γ = 94,30(2)°, von [CH3C(NH2)2]2SnF6: a = 6,980(2), b = 6,799(2), c = 7,018(3) Å, α = 105,40(3)°, β = 111,80(3)°, γ = 94,14(2)°.
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  • 2
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Diphenylfluorophosphane with Aldehydes. Crystal Structure of [α-(Difluorodiphenyl-λ5-phosphanyl)] Piperonyl DiphenylphosphiniteDiphenylfluorophosphane, Ph2PF, reacts with aldehydes forming phosphinito phosphoranes, Ph2F2P—CHR—O—PPh2. [α-(Difluorodiphenyl-λ5-phosphanyl)] piperonyl diphenyl-phosphinite, obtained by the reaction of Ph2PF with piperonal, crystallizes in the triclinic space group P1 with a = 969.3 pm, b = 2360 pm, c = 607,3 pm, α = 88.33°, β = 102.79°, γ = 92.40° and Z = 2.
    Notes: Diphenylfluorphosphan, Ph2PF, reagiert mit Aldehyden unter Bildung von Phosphinitophosphoranen, Ph2F2P—CHR—O—PPh2. Der mit Piperonal erhaltene Diphenyl-phosphinigsäure-[α-(difluorodiphenyl-λ5-phosphanyl)]piperonylestr kristallisiert in der triklinen Raumgruppe P1 mit a = 969,3 pm, b = 2360 pm, c = 607,3 pm, α = 88,33°, β = 102,79°, γ = 92,40° und Z = 2.
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  • 3
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thermal Behaviour of Cesiumchloroferrates(III). IV. The Crystal Structure of Cs3[FeCl5(H2O)]Cl and its Topotactic Formation from Cs2[FeCl5(H2O)] and CsClTricesium aquapentachloroferrate(III) chloride crystallizes from acid aqueous solutions of FeCl3 · 6 H2O and CsCl in the triclinic space group P11 with a = 714,1 pm, b = 1 070.9 pm, c = 950,4 pm, α = 105.65°, β = 109.51 °, γ = 89.08° and Z = 2. The compound is formed also from dicesium aquapentachloroferrate(III) and cesium chloride in a solid state reaction. The orientational relationships between the educt and product phases are elucidated, and a topotactic reaction mechanism is discussed.
    Notes: Tricaesiumaquapentachloroferrat(III)-chlorid kristallisiert aus salzsauren wäßrigen Lösungen von FeCl3 · 6 H2O und CsCl in der triklinen Raumgruppe P11 mit a = 714,1 pm, b = 1 070,9 pm, c = 950,4 pm, α = 105,65°, β = 109,51°, γ = 89,08° und Z = 2. Die Verbindung kann auch aus Dicaesiumaquapentachloroferrat(III) und Caesiumchlorid in einer Feststoffreaktion gebildet werden. Die Orientierungsbeziehungen zwischen Edukt- und Produktphase werden erläutert und ein topotaktischer Reaktionsmechanismus diskutiert.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 588 (1990), S. 139-146 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Structure of a New Modification of Phosphorus Sulfide P4S9A new modification of P4S9 is formed by the reaction of phosphorus pentasulfide with isopropanol in a molar ratio 1:4. The pure substance can be isolated by repeated fractional crystallization from CS2. This modification crystallizes in the monoclinic space group P21/n with a = 855.5 pm, b = 1263.7 pm, c = 1245.3 pm, β = 104.94°, Z = 4. Normally the P4S9 I crystallizes from its melts, only by shorttime heating the cubic modification (P4S9 II) is yielded.
    Notes: Bei der Reaktion von Phosphor(V)-sulfid mit Isopropanol im Molverhältnis 1:4 bildet sich eine neue Modifikation des P4S9. Die reine Substanz läßt sich durch mehrfache fraktionierte Kristallisation aus CS2 isolieren. Diese Modifikation kristallisiert in der monoklinen Raumgruppe P21/n mit a = 855,5 pm, b = 1263, 7 pm, c = 1245,3 pm, β = 104,94°, Z = 4. Nach kurzzeitigem Aufschmelzen kristallisiert die kubische Modifikation (P4S9 II), während längeres Schmelzen zur Kristallisation des P4S9 I führt.
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  • 5
    ISSN: 0044-2313
    Keywords: I. r. and 31P n. m. r. spectroscopy ; bis(phosphane) sulphur dioxide nickel(0) complexes ; X-ray structure of Ni(PCy3)2(SO2) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sulphur Dioxide as Ligand and Synthon. X. The Coordination Geometry of SO2 in Bis(phosphane)-Sulphur Dioxide-Nickel(0) Complexes. Structure of Ni(PCy3)2(SO2)The SO2 coordination geometry in Ni(PR3)2(SO2) complexes with steric parameters of the coligands Θ ≫ 141° was investigated by means of IR and 31P-NMR spectroscopy. The X-ray structure of Ni(PCy3)2(SO2) is described. The hitherto discussed n2-S.O-SO2 coordination mode for this type of complexes couldn't be confirmed.
    Notes: Zur Ermittlung der SO2-Koordinationsgeometrie in Ni(PR3)2(SO2)-Komplexen deren Coliganden Kegelöffnungswinkel von Θ ≫ 141° aufweisen, wurden die IR-und 31P-NMR-Spektroskopie herangezogen. Die Einkristallröntgenstrukturanalyse von Ni(PCy3)2(SO2) wird beschrieben. Eine für diesen Komplextyp bislang diskutierte n2-S.O-Koordination des Schwefeldioxids ließ sich nicht bestätigen.
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  • 6
    ISSN: 0044-2313
    Keywords: Guanidinium hexafluorometallates ; guanidinium pentafluorooxoniobate ; guanidinium tetrafluorodioxowolframate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Guanidinium Hexafluorometallates of Titanium, Silicon, Germanium, and Tin. Guanidinium Pentafluorooxoniobate and Guanidinium TetrafluorodioxowolframateThe title compounds were crystallized from the aqueous solutions of their fluorometallate respectively oxofluorometallate acids by adding of guanidinium fluoride solution. Their unit cells were determined and for [C(NH2)3]2 TiF6 its crystal structure was determined: s. g. Cm, a = 12.869 Å, b = 7.378 Å, c = 6.243 Å, β = 114.45°, layer structure, R = 0.0257. The unit cell parameters of [C(NH2)3]2 SiF6: a = 12.612 Å, b = 7.272 Å, c = 6.171 Å, β = 114.30°, of [C(NH2)3]2 GeF6: a = 12.773 Å, b = 7.343 Å, c = 6.202 Å, β = 114.38°, of [C(NH2)3]2 SnF6 : a = 12.972 Å, b = 7.439 Å, c = 6.356 Å, β = 114.14°, of [C(NH2)3]2 NbOF5:a = 12.987 Å, b = 7.425 Å, c = 6.326 Å, β = 114,25°, of [C(NH2)3]2 WO2F4:a = 12.941 Å, b = 7.396 Å, c = 6.256 Å, β = 114.33°.
    Notes: Die Titelverbindungen wurden aus den wässrigen Lösungen der jeweiligen Fluorometallat-bzw. oxofluorometallatsäuren nach Zugabe von Guanidiniumfluoridlösung als kristalline Verbindungen erhalten und ihre Gitterkonstanten bestimmt. Vom [C(NH2)3]2 Tif6 wurde die Kristallstruktur bestimmt: R.Gr. Cm, a = 12,869 Å, b = 7,378 Å, c = 6,243 Å, β = 114,45°, Schichtstruktur, R = 0,0257. Kristallographische Daten von [C(NH2)3]2 SiF6:a = 12,612 Å, b = 7,272 Å, c = 6,171 Å, β = 114,30°, von [C(NH2)3]2 GeF6:a = 12,773 Å, b = 7,343 Å, c = 6,202 Å, β = 114,38°, von [C(NH2)3]2 SnF6:a = 12,972 Å, b = 7,439 Å, c = 6,356 Å, β = 114,14°, von [C(NH2)3]2 NbOF5:a = 12,987 Å, b = 7,425 Å, c = 6,326 Å, β = 114,25°, von [C(NH2)3]2 WO2F4:a = 12,941 Å, b = 7,396 Å, c = 6,256 Å, β = 114,33°.
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  • 7
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Phosphorus Compounds with Adamantane Structure. XIV. Crystal Structure of a 3, 5-Diphenyl-1, 2, 4-dithiazolium Salt with the Cage-like Anion [P4NS9]The compound 3, 5-Diphenyl-1, 2, 4-dithiazolium 1, 3, 5, 7-pentathioxo-10-aza-2, 4, 6, 8, 9-pentathia-1α5,3λ5,5λ5,7λ5-tetraphosphatricyclo[3.3.1.13,7]decanide has been prepared by the reaction of P4S10 with benzonitrile. It crystallizes in the triclinic space group P1 with a = 9.914 Å, b = 15.025 Å, c = 9.186 Å, α = 100.48°, β = 99.90°, γ = 90.66°, and Z = 2. The anion has the structure of a P4S10-like cage, in which one P—S—P group is replaced by the P—N—P group.
    Notes: 3, 5-Diphenyl-1, 2, 4-dithiazolium-1, 3, 5, 7-tetrathioxo-10-aza-2, 4, 6, 8, 9-pentathia-1λ5,3λ5,5λ5,7λ5-tetraphospha-tricyclo[3.3.1.13,7]decanid entsteht bei der Reaktion von P4S10 mit Benzonitril. Die Verbindung kristallisiert in der triklinen Raumgruppe P1 mit a = 9, 914 Å b = 15,025 Å, c = 9,186 Å, α = 100,48°, β = 99,90° γ = 90,66° und Z = 2. Das Anion hat die Struktur eines P4S10-ähnlichen Käfigs, in dem eine PSP-durch eine PNP-Gruppe ersetzt ist.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 527 (1985), S. 99-104 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristallstruktur des Calciumpolyphosphates [Ca2(PO3)4]xβ-Calciumpolyphosphat kristallisiert in der monoklinen Raumgruppe P21/c mit den Gitterkonstanten a = 6,999, b = 7,717, c = 16,944 Å, β = 90,44°. Die Full-Matrix-Verfeinerung mit Einheitsgewicht führte zu R = 0,022. Auf die Periode der Anionenkette kommen 4 Tetraeder, Kettenrichtung ist x. Die Kationen-Polyeder bilden Doppelketten, ebenfalls parallel x, in denen die Polyeder über gemeinsame Flächen und Kanten verknüpft sind.
    Notes: β-Calciumpolyphosphate crystallizes in the monoclinic space group P21/c, unit cell a = 6.999, b = 7.717, c = 16.944 Å, β = 90.44°. Full matrix refinement with unit weight lead to R = 0.022. The period of the anion chain amounts to 4 tetrahedra, chain direction is x. The cation polyhedra form double chains, also parallel x, in which the polyhedra are linked by common faces and edges.
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