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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 1 (1995), S. 389-393 
    ISSN: 0947-6539
    Keywords: crystal structure ; differential thermal analysis ; nitrogen oxides ; phase transitions ; twinning ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mixtures of N2O3 and N2O4 have been prepared from measured volumes of NO and O2. Phase relationships in the system N2O3/N2O4, which depend on the composition of the samples and on the temperature, were studied by the Guinier technique and differential thermal analysis. Single crystals of phases A and B of N2O3 were grown in situ on a diffractometer and studied at temperatures between -107 and -170°C by X-ray diffraction. The structure analysis of A-N2O3 (tetragonal, space group I41/a, T = -170°C, a = 1625.57 (16), c = 880.49(13) pm, Z = 32, R1 = 0.051 for 1030 unique reflections) is hampered by twinning and additional disorder of one of two crystallographically independent molecules. B-N2O3 is nicely ordered with one molecule in the asymmetric unit (orthorhombic, space group P212121, T = -160°C, a = 506.86(4), b = 647.96(5), c = 863.26(6) pm, Z = 4, R1 = 0.023 for 1352 unique reflections). The most interesting features of the N2O3 molecule are its planarity and the extraordinarily long N—N bond (189.0(1) pm).
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0044-2313
    Keywords: Gadolinium Iodide Carbide Nitride ; Gadolinium Bromide Carbide Nitride ; Yttrium Iodide Carbide Nitride ; Lanthanum Iodide Carbide Nitride ; preparation ; X-ray single crystal structure investigation ; crystal structure ; condensed cluster ; chain of condensed octahedra and double tetrahedra ; C—C single bond ; Gd6(C2) octahedron ; Gd6N2 double tetrahedron ; Y10(C2)2 double octahedron ; Y6N2 double tetrahedron ; α-Gd4I6CN, β-Gd4I6CN, Y6I9C2N, α-Gd4Br6CN, α-La4I6CN ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Gd4I6CN: A Carbide Nitride with Chains of Gd6(C2) Octahedra and Gd6N2 Double TetrahedraThe compound α-Gd4I6CN is prepared by reaction of Gd, GdI3, C, and GdN (1:2:1:1 mole ratio) at 1 170 K in sealed Ta tubes. It is obtained as brown red, transparent needles which are air and moisture sensitive. The structure of α-Gd4I6CN contains Gd6 octahedra centered by C2 groups and double tetrahedra centered by N atoms. The units are alternatingly connected via common edges to form chains (Gd2Gd4/2C2) (Gd2/2Gd2/2N)2 parallel [001]. The linear chains are surrounded by I atoms above all free edges of the metal polyhedra and linked according to (Gd2Gd4/2C2) (Gd2Gd4/2N2)I4/2I8I2 in the a - b plane.We also found β-Gd4I6CN, which is formed in a monotropic transition from the α-form. In the structure the chains of Gd octahedra and tetrahedra as described for α-Gd4I6CN are more densely packed.The structure of Y6I9C2N is composed by chains of pairs of Y-octahedra and Y-tetrahedra, respectively. The octahedra are centered by C2 groups, the tetrahedra by N-atoms.We also synthesized the compounds Gd4Br6CN und La4I6CN by tempering at 1 220 K. They are isotypic with α-Gd4I6CN.
    Notes: α-Gd4I6CN wird durch Reaktion von Gd, GdI3, C und GdN (Molverhältnis 1:2:1:1) bei 1 170 K im verschlossenen Ta-Tiegel erhalten. Es bildet braunrot durchscheinende Nadeln, die gegen Luft und Feuchtigkeit empfindlich sind. Die Struktur von α-Gd4I6CN enthält durch C2-Einheiten zentrierte Gd6-Oktaeder und Doppel aus N zentrierten Tetraedern, Gd6N2. Abwechselnd sind Oktaeder und Tetraederdoppel über gemeinsame Kanten zu Ketten (Gd2Gd4/2C2) (Gd2/2Gd2/2N)2 verknüpft, die parallel [001] ausgerichtet sind. Diese eindimensionalen Einheiten sind über allen freien Kanten durch Iodatome koordiniert und untereinander nach dem Schema (Gd2Gd4/2C2) · (Gd2Gd4/2N2)I4/2I8I2 in der a - b-Ebene verknüpft.Daneben existiert noch ein β-Gd4I6CN, das sich monotrop aus der α-Form bei 1 300 K bildet. Dessen Struktur zeichnet sich durch eine dichtere Packung der für die α-Form beschriebenen Gd-Oktaeder-Tetraederketten aus.In der Struktur von Y6I9C2N sind die Ketten aus Doppeln sowohl C2-zentrierter Oktaeder als auch N-zentrierter Tetraeder der Y-Atome aufgebaut.Weiter erhielten wir die mit α-Gd4I6CN isotypen Verbindungen Gd4Br6CN und La4I6CN durch Tempern der Ausgangsverbindungen bei 1 220 K.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 649-654 
    ISSN: 0044-2313
    Keywords: Cerium Nitride Iodide ; preparation ; X-ray single crystal investigation ; crystal structure ; condensed cluster ; chain of condensed Ce tetrahedra around N ; Ce triangles around N ; magnetic properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure, and Magnetic Properties of Ce15N7I24The compound Ce15N7I24 is prepared by reaction of CeI3 and CeN (8:7 mole) at 1050 K in sealed Ta tubes. It is obtained as red, transparent needles which are air and moisture sensitive. The structure of Ce15N7I24 contains two crystallographically different types of N atoms. The one type of N is tetrahedrally coordinated by Ce atoms. The Ce4N tetrahedra are condensed via opposite edges to form chains. The other type of N has a triangular environment of Ce atoms. Ce15N7I24 is paramagnetic with an effective magnetic moment of 2,55 μB.
    Notes: Ce15N7I24 wird durch Reaktion von CeI3 und CeN (Molverhältnis 8:7) bei 1050 K im verschlossenen Ta-Tiegel erhalten. Es bildet rot durchscheinende Nadeln, die gegen Luft und Feuchtigkeit empfindlich sind. In der Struktur von Ce15N7I24 liegen zwei kristallchemisch unterschiedliche N-Atome vor. Die eine Sorte wird von den Ce-Atomen tetraedrisch koordiniert. Die Ce4N-Tetraeder sind über gemeinsame Kanten zu Ketten verknüpft. Die andere Sorte befindet sich im Mittelpunkt eines von Ce-Atomen aufgespannten Dreiecks. Die Ce3N-Dreiecke sind über I-Atome mit benachbarten Dreiecken und Tetraederketten verknüpft. Ce15N7I24 ist paramagnetisch mit einem effektiven magnetischen Moment von 2,55 μB.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1501-1507 
    ISSN: 0044-2313
    Keywords: Gadolinium carbide chloride ; gadolinium carbide bromide ; terbium carbide bromide ; crystal structure ; Gd—Gd bonds, electrical conductivity ; antiferromagnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Gadolinium Carbide Halides, Gd4C2X3 (X = Cl, Br)The compounds Gd4C2X3 (X = Cl, Br) and Tb4C2Br3 have been prepared by reaction of the metals (RE), REX3, and C in sealed Ta capsules at 1 100° and 1 300°C, respectively. Monophasic samples of Gd4C2Br3 and Tb4C2Br3 were obtained by reacting stoichiometric mixtures of the starting materials for five days. The needle shaped crystals are bronze-coloured and sensitive to air and moisture. Gd4C2X3 crystallizes in the space group Pnma (No. 62) with lattice constants a = 1 059.6(4), b = 368.4(1), c = 1 962.7(8) pm (Gd4C2Cl3), a = 1 084.4(1), b = 373.0(1), c = 2 036.1(1) pm (Gd4C2Br3). According to Guinier photographs, Tb4C2Br3 is isotypic (a = 1 074.3(2), b = 370.6(1), c = 2 019.4(1) pm).In the crystal structure C is octahedrally coordinated by Gd. The Gd6 octahedra are linked via common edges to form corrugated layers. The X-anions coordinate all free edges and corners of these layers and connect them via Xi—Xi contacts parallel [001].Gd4C2Br3 shows metallic conductivity. The magnetic susceptibility follows at high temperatures a Curie Weiss law with an effective moment of 7.95 μB. At temperatures below 50 K antiferromagnetic order is observed.
    Notes: Die Verbindungen Gd4C2X3 (X = Cl, Br) und Tb4C2Br3 werden durch fünftägiges Tempern von Metall, Trihalogenid und C in verschweißten Ta-Kapseln bei Temperaturen zwischen 1 100° und 1 300°C dargestellt. Die Kristalle bilden bronzefarbene Nadeln und sind gegen Luft und Feuchtigkeit mäßig empfindlich. Es liegt die Raumgruppe Pnma (Nr. 62) vor mit den Gitterkonstanten a = 1 059,6(4), b = 368,4(1), c = 1 962,7(8) pm (Gd4C2Cl3), a = 1 084,4(1), b = 373,0(1), c = 2 036,1(1) pm (Gd4C2Br3). Nach Guinier-Aufnahmen ist Tb4C2Br3 isotyp (a = 1 074,3(2), b = 370,6(1), c = 2 019,4(1) pm).In der Kristallstruktur ist C oktaedrisch von Gd koordiniert. Die Gd6-Oktaeder sind über gemeinsame Kanten kondensiert und bilden gewellte Schichten. Die X-Anionen koordinieren alle freien Ecken und Kanten dieser Schichten und verknüpfen sie parallel [001] über Xi—Xi-Kontakte.Gd4C2Br3 zeigt metallisches Verhalten. Die Hochtemperatursuszeptibilität befolgt ein Curie-Weiss-Gesetz mit einem magnetischen Moment von 7,95 μB. Bei Temperaturen unterhalb 50 K findet man langreichweitige antiferromagnetische Ordnung.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 49-63 
    ISSN: 0044-2313
    Keywords: Oxomolybdates ; cluster ; crystal structure ; HRTEM ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of PbMo5O8; a reduced Oxomolybdate with Mo10O28 Double OctahedraThe crystal structure of the new phase PbMo5O8 contains oligometric Mo clusters which consist of two edge-sharing Mo6 octahedra connected according to Mo10O6iO4/2i-iO16/2i-a. The compound is isotypic with LaMo5O8. Isolated, divalent Pb atoms are located in the “channels” of the monoclinic structure (a = 999.3(2) pm, b = 924.7(1) pm, c = 753.6(2) pm, β = 109.39(2)°, P21/a. Compared to the compound In 11Mo40O62 the Mo—O distances (average 206 pm) and the Mo—Mo distances within the octahedral units (average 275 pm) are slightly decreased by 1 and 4 pm, respectively. The very short Mo—Mo distances (278 pm) between the cluster units which are not observed in In11Mo40O62 (320 pm) are due to excess electrons in these inter-cluster bonds which would otherwise occupy antibonding cluster states.
    Notes: Mit der neuen Phase PbMo5O8 wurde ein weiteres Beispiel für oligomere Mo-Cluster aus zwei kantenverknüpften Mo6-Oktaedern gefunden, die nach Mo10O6iO4/2i-iO16sol;2i-a verknüpft sind. Die Verbindung ist isotyp zu LaMo5O8. In den „Kanälen“ der monoklinen Struktur a = 999,3(2) pm, b = 924,7(1) pm, c = 753,6(2) pm, β = 109,39(2)°, P21/a) findet man isolierte, zweiwertige Pb-Atome. Gegenüber der Verbindung In11Mo40O62 sind die Mo—O-Abstände mit durchschnittlich 206 pm nur gering um 1 pm und die Mo—Mo-Abstände innerhalb der oktaedrischen Baueinheiten mit durchschnittlich 275 pm ebenfalls nur schwach um 4 pm verkürzt. Allerdings findet man mit 278 pm sehr kurze Mo—Mo-Abstände zwischen den Clustereinheiten, die so nicht bei In11Mo40O62 (320 pm) beobachtet werden können. An diesen inter-Cluster-Bindungen sind überschüssige Elektronen beteiligt, die andernfalls antibindende Clusterzustände besetzen würden.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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