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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 537-540 
    ISSN: 0044-2313
    Keywords: Antimony(V)-oxide chloride ; Synthesis ; IR Spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, IR Spectrum, and Crystal Structure of Sb12O18(OH)2Cl22 · 2CH2Cl2The title compound has been prepared by the reaction of Sb5O7Cl11 with dichloromethane at 20°C, forming colourless, moisture sensitive crystals. Sb12O18(OH)2Cl22 · 2CH2Cl2 crystallizes monoclinically in the space group P21/n with two formula units per unit cell. Structure solution with 2696 unique observed reflections, R = 0.042. Lattice dimensions at 19°C: a = 1350.2, b = 1466.7, c = 1392.9 pm, b̃ = 97.925°. The distorted octahedrally coordinated antimony atoms, bridged by oxygen atoms, exhibit a molecular array which may be seen as a fragment of the rutile type structure, isolated by terminal chloride ligands. The solvate molecule is associated by a hydrogen bridge OH···Cl.
    Notes: Die Titelverbindung entsteht in Form farbloser Kristalle bei der Reaktion von Sb5O7Cl11 mit Dichlormethan bei 20°C. Sb12O18(OH)2Cl22 · 2CH2Cl2 kristallisiert monoklin in der Raumgruppe P21/n mit zwei Formeleinheiten pro Elementarzelle. Strukturlösung mit 2696 unabhängigen beobachteten Reflexen, R = 0,042. Gitterkonstanten bei 19°C: a = 1350,2; b = 1466,7; c = 1392,9 pm, b̃ = 97,925°. Die verzerrt oktaedrisch koordinierten und über Sauerstoffatome verbrückten Antimonatome bilden ein molekulares Gerüst, das als ein durch terminale Chlorliganden isolierter Ausschnitt aus der Rutilstruktur angesehen werden kann. Das Solvatmolekül ist durch eine Wasserstoffbrücke OH…Cl assoziiert.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1573-1581 
    ISSN: 0044-2313
    Keywords: Weberite structure ; structure determination ; di-sodium iron vanadium hepta-fluoride ; di-sodium iron chromium hepta-fluoride ; di-sodium cobalt vanadium hepta-fluoride ; disodium cobalt chromium hepta-fluoride ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure Determinations of Four Monoclinic Weberites Na2MIIMIIIF7 (MII = Fe, Co; MIII = V, Cr)By solid state reaction of the binary fluorides single crystals of the following weberites were prepared and their monoclinic structure (space group C2/c, Z = 16) determined by X-ray methods: Na2FeVF7 (a = 1 271.0(3), b = 742.9(1), c = 2 471.6(5) pm, β = 100.03(3)°; R1 = 0.043 (1 545 Reflexe); Fe—F = 203.8, V—F = 193.0 pm); Na2FeCrF7 (a = 1 262.5(3), b = 739.1(1), c = 2 460.5(5) pm, β = 99.93(3)°; R1 = 0.029 (2 340); Fe—F = 203.6, Cr—F = 190.5 pm); Na2CoVF7 (a = 1 270.3(5), b = 739.1(3), c = 2 465.1(10) pm, β = 100.02(3)°; R1 = 0.028 (2 250); Co—F = 201.6, V—F = 193.6 pm); Na2CoCrF7 (a = 1 257.8(3), b = 733.5(1), c = 2 441.5(5) pm, β = 99.64(3)°; R1 = 0.030 (2 227); Co—F = 201.2, Cr—F = 190.2 pm). Concerning the above average distances within the distorted [MF6] octahedra and the shape of [NaF8] coordination details are given and discussed.
    Notes: Durch Festkörperreaktion der binären Fluoride wurden Einkristalle der folgenden Weberite dargestellt und röntgenographisch deren monokline Struktur bestimmt (Raumgruppe C2/c, Z = 16): Na2FeVF7 (a = 1 271,0(3), b = 742,9(1), c = 2 471,6(5) pm, β = 100,03(3)°; R1 = 0,043 (1 545 Reflexe); Fe—F = 203,8, V—F = 193,0 pm); Na2FeCrF7 (a = 1 262,5(3), b = 739,1(1), c = 2 460,5(5) pm, β = 99,93(3)°; R1 = 0,029 (2 340); Fe—F = 203,6, Cr—F = 190,5 pm); Na2CoVF7 (a = 1 270,3(5), b = 739,1(3), c = 2 465,1(10) pm, β = 100,02(3)°; R1 = 0,028 (2 250); Co—F = 201,6, V—F = 193,6 pm); Na2CoCrF7 (a = 1 257,8(3), b = 733,5(1), c = 2 441,5(5) pm, β = 99,64(3)°; R1 = 0,030 (2 227); Co—F = 201,2, Cr—F = 190,2 pm). Zu den genannten mittleren Abständen in den verzerrten [MF6]-Oktaedern und zur Form der [NaF8]-Koordination werden Einzelheiten mitgeteilt und diskutiert.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1614-1620 
    ISSN: 0044-2313
    Keywords: Structure determination ; vanadium weberites ; disodium metal(II) vanadium(III) heptafluorides ; sodium tetrafluoro-vanadate(III) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structures of the Vanadium Weberites Na2MIIVIIIF7 (MII = Mn, Ni, Cu) and of NaVF4At single crystals of the vanadium(III) compounds NaVF4 (a = 790.1, b = 531.7, c = 754.0 pm, β = 101.7°; P21/c, Z = 4), Na2NiVF7 (a = 726.0, b = 1031.9, c = 744.6 pm; Imma, Z = 4) and Na2CuVF7 (a = 717.6, b = 1043.5, c = 754.6 pm; Pmnb, Z = 4) X-ray structure determinations were performed, at Na2MnVF7 (a = 746.7, c = 1821.6 pm; P3221, Z = 6) a new refinement. NaVF4 crystallizes in the layer structure type of NaNbO2F2. The fluorides Na2MIIVF7 represent new orthorhombic (MII = Ni; Cu) resp. trigonal (MII = Mn) weberites. The average distances within the [VF6] octahedra of the four compounds are in good agreement with each other and with data of related fluorides (V—F: 193.3 pm). The differences between mean bond lengths of terminal and bridging F ligands are 5% in NaVF4, but less than 1% in the weberites. Details and data for comparison are discussed.
    Notes: An Einkristallen der Vanadium(III)-Verbindungen NaVF4 (a = 790,1, b = 531,7, c = 754,0 pm, β = 101,7°; P21/c, Z = 4), Na2NiVF7 (a = 726,0, b = 1031,9, c = 744,6 pm; Imma, Z = 4) und Na2CuVF7 (a = 717,6, b = 1043,5, c = 754,6 pm; Pmnb, Z = 4) wurden Röntgenstrukturbestimmungen durchgeführt, an Na2MnVF7 (a = 746,7, c = 1821,6 pm; P3221, Z = 6) eine neue Verfeinerung. NaVF4 kristallisiert in der Schichtstruktur des NaNbO2F2-Typs. Die Fluoride Na2MIIVF7 sind neue orthorhombische (MII = Ni; Cu) bzw. trigonale (MII = Mn) Weberit-Vertreter. Die mittleren Abstände in den [VF6]-Oktaedern der vier Verbindungen stimmen gut miteinander und mit Daten in verwandten Fluoriden überein (V—F: 193,3 pm). Die Unterschiede zwischen den mittleren Abständen terminaler und verbrückender F-Liganden betragen in NaVF4 5%, in den Weberiten aber weniger als 1%. Einzelheiten und Vergleichsdaten werden diskutiert.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 406 (1974), S. 38-44 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigation of Quaternary Fluorides LiMIIMIIIF6. Some Compounds of the BaLiCrF6 TypeSome monoclinically crystallizing compounds BaLiMIIIF6 (MIII = Al, Ga, Cr, V, Fe, Ti) are reported. Part of the lithium, which is tetrahedrally coordinated in the BaLiCrF6-type structures, could be replaced by Co(II) ions in solid solutions BaLiGaF6/KCoGaF6. The reflectance spectrum of tetrahedral CoF42- is given.
    Notes: Es wird über eine Reihe monoklin kristallisierender Verbindungen der Zusammensetzung BaLiMIIIF6 (MIII = Al, Ga, Cr, V, Fe, Ti) berichtet. Das in den Strukturen vom BaLiCrF6-Typ tetraedrisch koordiniert vorliegende Lithium ließ sich in Mischkristallen BaLiGaF6/KCoGaF6 partiell durch Co(II)-Ionen ersetzen. Das Reflexionsspektrum von tetraedrischem CoF42- wird mitgeteilt.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 387 (1972), S. 161-178 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The results of X-ray single crystal work on RbNiCrF6 (a = 10.21 Å) and of powder work on KNiCrF6 (a = 10.24 Å) and KNiCrF6 · H2O (a = 10.45 Å) are reported. All three compounds crystallize cubically in the space group Fd3m. They contain a network M2X6 of octahedra, analogous to that of the pyrochlores and with distances Ni-F = Cr-F = = 1.93 ± 0.02 Å which are equal within the error of determination. The structural relations between the three compounds, and compared with the pyrochlore structure are discussed, as well as the relations to the tetragonal bronze-type structure occuring as a high pressure phase of KNiCrF6.
    Notes: Die Ergebnisse einer Einkristallstrukturbestimmung an RbNiCrF6(a = 10,21 Å) und von Pulvermessungen an KNiCrF6 (a = 10,24 Å) und KNiCrF6 · H2O (a = 10,45 Å) werden mitgeteilt. Alle drei Verbindungen kristallisieren kubisch in der Raumgruppe Fd3m und enthalten ein den Pyrochloren analoges Oktaedernetz M2X6 mit innerhalb der Fehlergrenze gleichen Abständen Ni-F = Cr-F = 1,93 ± 0,02 Å. Die strukturellen Beziehungen der drei Verbindungen untereinander und zur Pyrochlorstruktur werden diskutiert, ebenso zur tetragonalen Bronzestruktur, die als Hochdruckphase von KNiCrF6 auftritt.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 406 (1974), S. 23-37 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of the Quaternary Fluoride BaLiCrF6The crystal structure of the monoclinic compound BaLiCrF6 was determined (a = 5.397, b = 10.355, c = 8.638 Å, β = 90.72°; SG P21/c, z = 4. R = 5.7% for all 1561 automatically recorded single crystal reflections hkl). The structure contains icosahedra of BaF12 (Ba-F = 2.890 Å) within a framework built up of isolated LiF4-tetrahedral (Li-F = 1.868 Å) and CrF6-octahedra (Cr-F = 1.903 Å) mutually linked by corners. All polyhedra are distorted. Structural relations and the variation of distances about the mean values given are discussed.
    Notes: Die Kristallstruktur der monoklinen Verbindung BaLiCrF6 wurde bestimmt (a = 5,397, b = 10,355, c = 8,638 Å, β = 90,72°; RG P21/c, z = 4. R = 5,7% für alle 1561 automatisch registrierten Einkristall-Reflexe hkl). Die Struktur enthält BaF12-Ikosaeder (Ba-F = 2,890 Å) innerhalb eines Raumnetzes, das aus isolierten LiF4-Tetraedern (Li-F = 1,868 Å) und CrF6-Oktaedern (Cr-F = 1,903 Å) besteht, die gegenseitig über Ecken miteinander verknüpft sind. Alle Polyeder sind verzerrt. Strukturbeziehungen sowie die Variation der Abstände um die angegebenen Mittelwerte werden diskutiert.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 409 (1974), S. 11-22 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Redetermination of the K2CuF4 StructureThe structure of K2CuF4 was redetermined by x-rays. An enlarged tetra-gonal unit cell of dimensions a = 5.858, c = 25.42 Å was found. The refinement in spacegroup D102d-I4c2 yielded R = 0.06. Contrary to former findings the JAHN-TELLER- distortion of the CuF6-octahedra corresponds to a tetragonal elongation with distances Cu-F = 1.92 Å (4 ×) and 2.22 Å(2×).
    Notes: Die röntgenographische Neubestimmung ergab für die K2CuF4- Struktur eine Vergrößerung der tetragonalen Elementarzelle auf die Gitterabmessungen a = 5,858, c = 25,42 Å. In der Raumgruppe D102d-I4c2 ließ sich die Struktur bis R = 0,06 verfeinern. Im Gegensatz zu früheren Befunden erweist sich die JAHN-TELLER-Verzerrung CuF6-Oktaeder jetzt auch hier als gestreckt. Im Rahmen der Bestimmungsgenauigkeit sind alle Oktaeder tragonal mit Abständen Cu-F = 1,92 Å (4×) und 2,22 Å (2×).
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1048-1054 
    ISSN: 0044-2313
    Keywords: Structure determination ; [FeO5] square pyramide ; asymmetric [PbO6] coordination ; lone pair effect ; perovskite relation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Lead Strontium Ferrate(III): The Crystal Structure of the Phase Pb4Sr2Fe6O15At orthorhombic single crystals of Pb4Sr2Fe6O15 (a = 568.73(8), b = 392.03(4), c = 2107.5(3) pm; Z = 4/3, space group Pnma) a X-ray structure determination has been performed (R1 = 0,036 for 488 „observed“ resp. wR2 = 0,073 for all 643 independent reflexions). It revealed a framework of polyhedra related to perovskite, in which chains of edgesharing pyramids [FeO5] (average Fe1—O: 197 pm; Fe1—Fe1: 305.5 pm) are linked via apices with corner-sharing [FeO6] octahedra (Fe2—O: 201 pm). 12-fold, strongly distorted cuboctahedrally coordinated „perovskite positions“ show mixed occupancy by 2/3 Sr + 1/3 Pb (= Sr2; Sr2—O: 287 pm). More spacy channels, running parallel to the chains of pyramids along [010] of the structure, contain lead atoms only. The double occupancy of the corresponding cages results in short distances Pb1—Pb1 (355.9 pm) and Pb1—Fe2 (314.4 pm), as well as in a very asymmetric [PbO6] coordination (Pb1—O: 253 pm), in the opposite hemisphere of which the lone electron pair s2 is supposed to be located. Details are communicated and structural relations discussed.
    Notes: An orthorhombischen Einkristallen von Pb4Sr2Fe6O15 (a = 568,73(8), b = 392,03(4), c = 2107,5(3) pm; Z = 4/3, Raumgruppe Pnma) wurde eine Röntgenstrukturbestimmung durchgeführt (R1 = 0,036 für 488 „beobachtete“ bzw. wR2 = 0,073 für alle 643 unabhängigen Reflexe). Diese ergab ein perowskitverwandtes Polyedergerüst, in dem Ketten kantenverknüpfter [FeO5]-Pyramiden (Mittelwert Fe1—O: 197 pm; Fe1—Fe1: 305,5 pm) mit ihrerseits eckenverknüpften [FeO6]-Oktaedern (Fe2—O: 201 pm) über Ecken verbunden sind. Zwölffach, stark verzerrt kuboktaedrisch koordinierte „Perowskit-Positionen“ sind gemischt besetzt mit 2/3 Sr + 1/3 Pb (= Sr2; Sr2—O: 287 pm). Dagegen befinden sich in größeren Kanälen, die sich parallel zu den Pyramidenketten längs [010] durch die Struktur ziehen, nur Bleiatome. Die doppelte Besetzung der zugehörigen Hohlräume führt zu kurzen Abständen Pb1—Pb1 (355,9 pm) und Pb1—Fe2 (314,4 pm), und zu einer ganz einseitigen [PbO6]-Koordination (Pb1—O: 253 pm). in deren Gegenhemisphäre das s2-Elektronenpaar zu vermuten ist. Einzelheiten werden mitgeteilt und Strukturverwandtschaften diskutiert.
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