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  • 1
    ISSN: 0044-8249
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 795-800 
    ISSN: 0044-2313
    Keywords: Tetraiodoferrate(III) ; Crystal Structure ; Raman Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Characterization, and Crystal Structures of Tetraiodoferrates(III)The extremely air and moisture sensitive tetraiodoferrates MFeI4 with M = K, Rb and Cs have been synthesized by reaction of Fe, MI and I2 at 300°C in closed quartz ampoules. The essentially more stable alkylammonium tetraiodoferrates NR4FeI4 with R = H, C2H5, n-C3H7, n-C4H9 and n-C5H11 can be obtained by reaction of Fe, NR4I and I2 in nitromethane. The Raman and UV/Vis-spectra of the black compounds show the existence of tetrahedral [FeI4]- ions in the structures. The crystal structure of the monoclinic CsFeI4 (CsTlI4 type, spgr P21/c; a = 7.281(1) Å; b = 17.960(3) Å; c = 8.248(2) Å; β = 107.35(15)°) is built up by tetrahedral [FeI4]- ions and CsI11 polyhedra. The crystal structure of the orthorhombic (n-C5H11)4NFeI4 (spgr Pnna; a = 20.143(4) Å; b = 12.683(3) Å; c = 12.577(3) Å) contains tetrahedral [(n-C5H11)4N]+ ions and [FeI4]- ions, respectively.
    Notes: Die extrem luft- und feuchtigkeitsempfindlichen Tetraiodoferrate MFeI4 mit M = K, Rb und Cs entstehen bei Umsetzung von Fe, MI und I2 bei 300°C in geschlossenen Quarzampullen. Die wesentlich stabileren Alkylammoniumtetraiodoferrate NR4FeI4 mit R = H, C2H5, n-C3H7, n-C4H9 und n-C5H11 sind durch Umsetzung von Eisenpulver mit NR4I und Iod in Nitromethan zu erhalten. Die Ramanspektren und UV/Vis-Spektren der schwarzen Verbindungen zeigen, daß in den Strukturen jeweils tetraedrische [FeI4]--Ionen vorliegen. Die Kristallstruktur des monoklinen CsFeI4 (CsTlI4-Typ, RG P21/c; a = 7,281(1) Å; b = 17,960(3) Å; c = 8,248(2) Å; β = 107,35(15)°) wird aus tetraedrischen [FeI4]--Ionen und CsI11-Polyedern aufgebaut. In der Kristallstruktur des orthorhombischen (n-C5H11)4NFeI4 (RG Pnna; a = 20,143(4) Å; b = 12,683(3) Å; c = 12,577(3) Å) sind tetraedrische [(n-C5H11)4N]+-Ionen und [FeI4]--Ionen enthalten.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 545 (1987), S. 148-156 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures and Phase Transformations of Cesium Trihalogenogermanates CsGeX3(X = Cl, Br, I)The compounds CsGeX3 (X = Cl, Br, I) have been obtained by reactions of Ge(OH)2 with CsX in aquaeous HX solutions. The thermal behavior has been studied by X-ray diffraction. Raman spectroscopy, and DTA/DSC. The compounds are dimorph. The low temperature modifications L-CsGeX3 show a rhomboedric deformed perovskite type structure. The high temperature phases H-CsGeX3 form the cubic perovskite type structure. The reversible phase transitions are interpreted as a result of position changes of the Ge atoms in the H-forms (Order-Disorder transitions). The transition temperatures increase in the sequence CsGeCl3 (155°C), CsGeBr3 (238°C), CsGeI3 (277°C).
    Notes: Das thermische Verhalten der Verbindungen CsGeX3 (X = Cl, Br, I), durch Umsetzungen von Ge(OH)2 mit CsX in wäßrigen HX-Lösungen erhalten, wurde unter Verwendung von Röntgenbeugung, Ramanspektroskopie und DTA/DSC untersucht. Die Verbindungen sind dimorph. Bei den Tieftemperaturmodifikationen L-CsGeX3 werden rhomboedrische Verzerrungsvarianten der Perowskitstruktur (Raumgruppe R3m), bei den Hochtemperaturformen H-CsGeX3 die kubische Perowskitstruktur gefunden. Die reversiblen Phasentransformationen werden als Ordnungs-Unordnungs-Übergänge infolge von Platzwechselvorgängen der Ge-Atome bei den H-Formen gedeutet. Die Umwandlungstemperaturen steigen in der Reihe CsGeCl3 (155°C), CsGeBr3 (238°C), CsGeI3 (277°C) an.
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  • 4
    ISSN: 0044-2313
    Keywords: Tetrabromoferrate(III) ; Preparation ; Characterization ; Raman spectra ; X-ray powder diagramms ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Characterization of Tetrabomoferrates(III) AFeBr4 with Monovalent Cations A = Cs, Rb, Tl, NH4, K, Na, Li, AgTetrabromoferrates(III) AFeBr4 of the monovalent cations A = Cs, Rb, Tl, NH4, Na, Ag, Li have been prepared in closed ampoules by reaction of the appropriate bromides with iron and an excessive amount of bromine. The dark red compounds were characterized by DTA, Raman spectroscopy and X-ray powder diffraction. Their crystal structures have been assigned to five structure types, containing FeBr4 anions. The coordination number runs from 12 (Cs+, Rb+) over 10 (NH4+) and 8 (K+), to 6 (Na+, Ag+, Li+). Lattice parameters for all compounds see “Inhaltsübersicht”. CsFeBr4 and RbFeBr4 crystallize orthorhombic in the BaSO4-type, NH4FeBr4 monoclinic in the KAlBr4-type, KFeBr4 orthorhombic in the GaGaCl4-type, NaFeBr4 monoclinic in the NaGaBr4-type, AgFeBr4 and LiFeBr4 monoclinic in the LiAlCl4-type, while the structure of TlFeBr4 is still unknown.
    Notes: Tetrabromoferrate(III) AFeBr4 mit einwertigen Kationen A = Cs, Rb, Tl, NH4, Na, Ag, Li wurden durch Umsetzungen der Bromide ABr und von Fe-Metal1 in Gegenwart eines Br2-Überschusses in geschlossenen Ampullen erhalten. Die dunkelroten Verbindungen wurden analytisch, thermisch, ramanspektroskopisch sowie durch Auswertung der Röntgenpulverdiagramme charakterisiert. Es wurden fünf Strukturen gefunden, jeweils mit tetraedrischen FeBr4-Anionen, aber unterschiedlicher Koordination der Kationen A. Die Koordinationszahlen fallen von 12 (Cs+, Rb+) über 10 (NH4+) und 8 (K+), bis zu 6 (Na+, Ag+, Li+). CsFeBr4 (a = 12,1905(2) Å, b = 7,510(19) Å, c = 9,8832(16) Å) und RbFeBr4 (a = 11,659(1) Å, b = 7,495(1) Å, c = 9,896(1) Å) kristallisieren im orthorhombischen BaSO4-Typ, NH4FeBr4 (a = 13,17(3) Å, b = 7,433(3) Å, c = 9,148(1) Å, β = 106,95(2)°) monoklin im KAlBr4-Typ, KFeBr4 (a = 7,688(1) Å, b = 10,373(2) Å, c = 10,206(2) Å) orthorhombisch im GaGaCl4-Typ, NaFeBr4 (a = 13,9261(3) Å, b = 7,470(2) Å, c = 7,4016(14) Å) orthorhombisch im NaGaBr4-Typ, AgFeBr4 (a = 7,538(2) Å, b = 6,869(1) Å, c = 13,852(2) Å, β= 92,73(2)°) und LiFeBr4 (a = 7,478(2) Å, b = 6,801(1) Å, c = 13,606(2) Å, β = 93,21(2)°) monoklin im LiAlCl4-Typ. Der Aufbau von TlFeBr4 konnte bisher nicht geklärt werden.
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  • 5
    ISSN: 0044-2313
    Keywords: Iodoplatinates ; Preparation ; Crystal Structure ; Raman Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Characterization of Iodoplatinates MexNH4-xPtI4 (x = 2-4), Mixed Valence Octaiododiplatinates(II,IV) with Pt2I8 GroupsIodoplatinates APtI4 (A = MexNH4-x with x = 2-4) have been prepared by partial oxidation of the correspondent hexaiododiplatinates(II) A2Pt2I6 with I2 in methanolic solutions. X-ray structure analyses of the bronze-coloured needle-shaped crystals of the compounds showed rows of dinuclear anions Pt2I82-, built up by edgesharing planar PtI4 groups with PtII und octahedral PtI6 groups with PtIV. The different space requirement of the cations leads to the formation of three different structures. Within the anion stacks weak intermolecular PtIV—I … PtII interactions are detectable by Raman spectroscopy.
    Notes: Iodoplatinate APtI4 (A = MexNH4-x mit x = 2-4) wurden durch partielle Oxidation der entsprechenden Hexaiododiplatinate(II) A2Pt2I6 mit I2 in methanolischer Lösung erhalten. Röntgenstrukturanalysen der in Form bronzefarbener Nadeln kristallisierenden Verbindungen ergaben, daß gemischtvalente Octaiododiplatinate(II,IV) mit zweikernigen Anionen Pt2I82- vorliegen, bei denen jeweils eine planare PtI4- und eine oktaedrische PtI6-Gruppe über eine gemeinsame Kante verknüpft sind. Der unterschiedliche Platzbedarf der Kationen führt zur Ausbildung von drei verschiedenen Strukturen, bei denen die komplexen Baugruppen und die Kationen jeweils getrennt stapelförmig angeordnet sind. Mit Hilfe der Ramanspektroskopie sind schwache intermolekulare PtIV—I … PtII- Wechselwirkungen innerhalb der Anionenstapel feststellbar.
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  • 6
    ISSN: 0044-2313
    Keywords: Bis(octaaquocalcium)-tridecachlorohexamercurate-tridecachloropentamercurate ; 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 2CaCl2 · 11HgCl2 · 16H2O, a Cubic Mercury-rich Chloromercurate with Icosahedral Hg6Cl13 and Hg5Cl13 GroupsThe mercury-rich chloromercurate 2CaCl2 · 11HgCl2 · 16H2O has been obtained by crystallization from concentrated aqueous solutions of CaCl2 and HgCl2 at room temperature. In the cubic crystal structure (a = 18.170(3) Å, space group F23, Z = 4) a three-dimensional framework is formed by Hg6Cl13- and Hg5Cl133- anions with large cavities, in which the dodecahedral Ca(H2O)82+ cations are accomodated. 96 out of 104 Cl atoms in the cell form a lattice complex cP2[12i] with 8 Cl12 icosahedra, which are centered by Cl atoms. In four of these Hg atoms are situated on 6 edges thus forming Cl(HgCl2)6- anions, while the remaining four icosahedra hold 3 Hg atoms on edges and two on faces. Here the central Cl- anions are coordinated by 3 HgCl2 and 2 HgCl3 groups. The Hg5Cl13 and Ca(H2O)8 polyhedra are crystallographically disordered.
    Notes: Das quecksilberreiche Chloromercurat 2CaCl2 · 11HgCl2 · 16H2O ist durch Kristallisation aus konzentrierten wäßrigen Lösungen von CaCl2 und HgCl2 bei Raumtemperatur zu erhalten. In der kubischen Kristallstruktur (a = 18,170(3) Å, Raumgr. F23, Z = 4) bilden Hg6Cl13-- und Hg5Cl133--Anionen ein Gerüst mit großen Hohlräumen, in denen sich Ca(H2O)82+-Kationen mit dodekaedrischer Konformation befinden. Von den 104 Cl-Atomen in der Zelle bilden 96 einen Bauverband cP2[12i] mit acht Cl12-Ikosaedern, die jeweils durch ein Cl-Atom zentriert sind. Bei vier der Ikosaeder befinden sich 6 Hg-Atome auf Kanten, so daß Cl(HgCl2)6--Anionen resultieren. Bei den Hg5Cl133--Anionen besetzen jeweils 3 Hg-Atome Kanten und 2 Hg-Atome Flächen der Ikosaeder, so daß die zentralen Cl--Anionen von 3 HgCl2- und 2 HgCl3-Gruppen koordiniert sind. Die Hg5Cl13- und Ca(H2O)8-Baugruppen sind kristallographisch fehlgeordnet.
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  • 7
    ISSN: 0044-8249
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 8
    ISSN: 0044-2313
    Keywords: Palladium ; Se6 ; Chalcogen Complex ; Crystal Structure ; Vibrational Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: PdCl2Se6 and PdBr2Se6, New Chalcogenrich Complexes of Palladium(II) Halides with Se6 Groups as LigandsPdCl2Se6 und PdBr2Se6, chalcogenrich complexes of palladium halides with Se6 groups as ligands have been prepared by reactions of Pd metal with melts of selenium and SeX4 (X = Cl, Br) at 180°C in closed silica ampoules. The new compounds have been characterized by vibrational spectra and thermal analysis. The X-ray analysis of PdCl2Se6 showed a polymeric structure, built up by chains of linear PdX2 groups connected by Se6 groups in a chair conformation.
    Notes: PdCl2Se6 und PdBr2Se6, zwei chalkogenreiche Komplexe von Palladium(II)-Halogeniden mit Se6-Gruppen als Liganden, wurden durch Umsetzung von Pd-Metall in Schmelzen aus Selen und SeX4 (X = Cl, Br) bei 180°C in geschlossenen Quarzglasampullen erhalten. Die neuen Verbindungen wurden schwingungsspektroskopisch und thermoanalytisch charakterisiert. Die Röntgenstrukturanalyse von PdCl2Se6 ergab eine polymere Struktur, in der hantelförmige PdX2-Gruppen über Se6-Gruppen mit Sesselkonformation zu Ketten verknüpft sind.
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  • 9
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Heptabromodigermanates(II) A3Ge2Br7 (A = Rb, NH4)  -  Syntheses, Characterization, and Crystal StructuresHeptabromodigermanates(II) A3Ge2Br7 (A = Rb, NH4) have been obtained by crystallization from aqueous ABr—GeBr2—HBr solutions. The compounds can be characterized as double salts ABr · 2 AGeBr3, because the crystal structures (monoclinic, space group P21/c, Z = 4) consist of pyramidal GeBr3 groups.
    Notes: Heptabromodigermanates(II) A3Ge2Br7 (A = Rb, NH4) wurden durch Kristallisation aus wäßrigen ABr—GeBr2—HBr—Lösungen erhalten. Die Verbindungen sind als Doppelsalze ABr · 2 AGeBr3 zu formulieren, denn in den Kristallstrukturen (monoklin, Raumgruppe P21/c; Z = 4) sind pyramidale GeBr3-Gruppen enthalten.
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  • 10
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Mixed-valence Iodoplatinate(II, IV) (NH3Me)4Pt3I11 with PtI6, PtI4, and Pt2I6 Anions in the Crystal StructureThe mixed-valence iodoplatinate(II, IV) (NH3Me)4Pt3I11 has been obtained from aqueous solutions by reactions of H2PtCl6 with N2H4 · 2 HCl and NH3MeI. The monoclinic crystal structure contains planar Pt2I62- anions side by side with PtI62- and PtI42- anions, which are connected by asymmetric iodide bridges to ∞1[PtI4I2/2]-chains.
    Notes: Schwarze Kristalle des gemischtvalenten Iodoplatinats(II, IV) (NH3Me)4Pt3I11 wurden aus wäßrigen Lösungen durch Reaktion von H2PtCl6 mit N2H4 · 2 HCl und NH3MeI erhalten. Am Aufbau der monoklinen Kristallstruktur (RG C2/m; a = 1 531,35(27) pm; b = 2 033,3(4) pm; c = 1 178,51(12) pm; β = 115,33(13)°; Z = 4) sind neben planaren Pt2I62--Anionen auch PtI62-- und PtI42--Anionen beteiligt, welche über asymmetrische Iodbrücken zu ∞1[PtI4I2/2]-Ketten verknüpft sind.
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