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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 467 (1980), S. 187-196 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: X-Ray Studies on Titanium(III) Fluoro Compounds with Pyrochlore-related StructuresThe cubic compounds (a/pm) CsMIITiIIIF6, MII = Mg (1041.6), Ni (1043.9), Zn (1049.8), Co (1051.7), V (1052.6), Fe (1055.3), Mn (1064.9) and CsM0,5ITi1,5IIIF6, MI = K (1074.6), Rb (1080.6) were prepared. They crystallize in the modified pyrochlore structure of the RbNiCrF6 type, which is confirmed once more at single crystals of an oxide fluoride phase CsTi2X6 (X6 between O2F4 and O3F3): Space group Fd3m, a = 1028.8 pm, R = 2.6% (126 independent reflections). Further compounds CsM0,5ITi1,5IIIF6 according to their powder diagrams are orthorhombic (MI = NH4: a = 764.1, b = 767.5, c = 1087.5 pm) or monoclinic (Na: a = 737.0, b = 758.0, c = 1061.8 pm, β = 91.1°, Li: a = 1466, b = 1479, c = 1041 pm, β = 93.3°) with related, but not exactly know structures.
    Notes: Die kubischen verbindungen (a/pm) CsMIITiIIIF6, MII = Mg(1041,6), Ni(1043,9), Zn(1049,8), Co(1051,7), V(1052,6), Fe(1055,3), Mn(1064,9) und CsM0,5ITi1,5IIIF6, MI = K(1074,6), Rb(1080,6) wurden dargestellt. Sie kristallisieren in der modifizierten Pyrochlorstruktur des RbNiCrF6-Types, der an Einkristallen einer Oxidfluoridphase CsTi2X6 (X6 zwischen O2F4 und O3F3) erneut bestätigt wird: Raumgruppe Fd3m, a = 1028,8 pm, R = 2,6% (126 symmetrieunabhängige Reflexe). Weitere Verbindungen CsM0,5ITi1,5IIIF6 sind nach Pulveraufnahmen orthorhombisch (MI = NH4: a = 764,1, b = 767,5, c = 1087,5 pm) bzw. monoklin (Na: a = 737,0, b = 758,0, c = 1061,8 pm, β = 91,1°, Li: a = 1466, b = 1479, c = 1041 pm,β = 93,3°), mit verwandten, aber nicht genauer bekannten Strukturen.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 487 (1982), S. 75-84 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Relations of Distances and Coordination in the Layer Structures of the Ternary Fluorides K2MF4 and K3M2F7 (MII = Mg, Mn, Co=Zn)Results of X-ray single crystal structure refinements of the compounds K2MF4 (M = Mg, Mn, Co, Ni) and K3M2F7 (M = Mn, Co, Ni), all crystallizing in the tetragonal space group I4/mmm of the K2NiF4 and Sr3Ti2O7 type, resp., are reported. The distances obtained are discussed, including data of the compounds with M = Cu, Zn. The influence of the KF9 coordination is made responsible for the fact, that the octahedral MF6 dimensions are much the same as in the corresponding perovskites KMF3. The shortest K—F distance of this KF9 group, occuring in both layer structure types, decreases against lattice widening from 263.4 pm (K2MgF4) to 258.0 pm (K2MnF4). The charge ratio calculated from the KF9 coordination for the unlike bonded anions leads to a better balanced charge distribution in the K2MF4 type, as is obtained by applying Pauling's rules.
    Notes: Ergebnisse röntgenographischer Einkristallstrukturverfeinerungen an den im K2NiF4- bzw. Sr3Ti2O7-Typ kristallisierenden Verbindungen K2MF4 (M = Mg, Mn, Co, Ni) und K3M2F7 (M = Mn, Co, Ni), die alle der tetragonalen Raumgruppe I4/mmm angehören, werden mitgeteilt. Die resultierenden Abstandsdaten werden unter Einbeziehung der Verbindungen mit M = Cu, Zn diskutiert. Die weitgehend den zugehörigen Perowskiten KMF3 entsprechenden Abstandsverhältnisse in den MF6-Oktaedern werden dem Einfluß der KF9-Koordination zugeschrieben, deren kürzester Abstand K—F in beiden Schichtstrukturtypen entgegen der Gitteraufweitung von 263,4 pm (K2MgF4) auf 258,0 pm (K2MnF4) abnimmt. Das aus der KF9-Koordination berechnete Ladungsverhältnis der ungleich gebundenen Anionen führt zu einer ausgeglicheneren Ladungsbilanz für den K2MF4-Typ, als die Anwendung der Paulingschen Regeln.
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  • 7
    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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  • 8
    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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  • 9
    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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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 491 (1982), S. 137-144 
    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 a High Temperature Modification of Barium-Zinc-Iron(III) Fluoride BaZnFeF7A metastable high temperature form of BaZnFeF7 prepared at 750°C crystallizes monoclinically (a = 560.3(1), b = 997,1(3), c = 958.4(4) pm, β = 92.80(4)°, Z = 4) in the same space group P21/c as the low temperature form. The X-ray structure determination (RG = 5.2— for 2426 independent reflections) showed analogy in the coordination behaviour of Zn2+ and Fe3+ cations, which occupy in an ordered way groups of two edgesharing octahedra, at each of which one ligand remains unbridged (mean distances Zn—F = 204.7 pm, Fe—F = 194.6 pm). The linking of double octahedra via corners to form a threedimensional framework involves strongly bent fluorine bridges (average Zn—F—Fe = 126.5°). Related structures are discussed.
    Notes: Eine bei 750°C in Einkristallen dargestellte metastabile Hochtemperatur-form von BaZnFeF7 kristallisiert monoklin (a = 560,3(1), b = 997,1(3), c = 958,4(4) pm, β = 92,80(4)°, Z = 4) in derselben Raumgruppe P21/c, wie die Tieftemperaturform. Die röntgenographische Strukturbestimmung (RG = 5,2 -  für 2 426 unabhängige Reflexe) ergab koordinationschemisch analoges Verhalten für Zn2+- und Fe3+-Kationen, die geordnet kantenverknüpfte Gruppen von zwei Oktaedern besetzen, an denen je ein Ligand unverbrückt bleibt (mittlere Abstände Zn—F = 204,7 pm, Fe—F = 194,6 pm). Die Eckenverknüpfung der Doppeloktaeder zu einer Raumnetzstruktur verläuft über stark gewinkelte Fluorbrücken (Mittel Zn—F—Fe = 126,5°). Verwandte Strukturen werden diskutiert.
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