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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1042-1046 
    ISSN: 0044-2313
    Keywords: Tribromoselenium (+) ; Triiodotellurium (+) ; Tetrabromoaluminate (-) ; Tetraiodoaluminate (-) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: SeBr3[AlBr4] and TeI3[AlI4] - two further Compounds in the SCl3[AlCl4] Structure TypeThe reaction of SeBr4 and AlBr3 in a closed glass ampoule at 150°C yields quantitatively SeBr3[AlBr4] in form of yellow moisture sensitive crystals. From Te, two equivalents of I2, and AlI3 one obtains TeI3[AlI4] in form of dark red, moisture sensitive crystals. Both compounds crystallize monoclinic in the space group Pc (SeBr3[AlBr4]: a = 670.7(7) pm, b = 663.9(5) pm, c = 1 428.6(2) pm, β = 101.21(9)°, TeI3[AlI4]: a = 731.9(1) pm, b = 730.8(1) pm, c = 1 565.5(3) pm, β = 102.01(2)°). They are isotypic and have the SCl3[AlCl4] structure type. The structures are built of tetrahedral AlX4- ions and of pyramidal EX3+ ions (E = S, Se, Te; X = Cl, Br, I). The chalcogen atoms are additionally coordinated by halogen atoms of surrounding AlX4- ions, corresponding to a strongly distorted octahedral coordination EX3+3.
    Notes: Durch Reaktion von SeBr4 mit AlBr3 in einer geschlossenen Ampulle bei 150°C entsteht SeBr3[AlBr4] in Form gelber, hydrolyseempfindlicher Kristalle in quantitativer Ausbeute. Aus Te, AlI3 und zwei Äquivalenten I2 entsteht unter gleichen Bedingungen TeI3[AlI4] in Form dunkelroter, ebenfalls hydrolyseempfindlicher Kristalle. Beide Verbindungen kristallisieren monoklin, Raumgruppe Pc (SeBr3[AlBr4]: a = 670,7(7) pm, b = 663,9(5) pm, c = 1 428,6(2) pm, β = 101,21(9)°, TeI3[AlI4]: a = 731,9(1) pm, b = 730,8(1) pm, c = 1 565,5(3) pm, β = 102,01(2)°). Sie sind isotyp zu SCl3[AlCl4]. Die Strukturen sind aus tetraedrischen AlX4--Ionen und aus pyramidalen EX3+-Ionen (E = S, Se, Te; X = Cl, Br, I) aufgebaut. Das Chalkogen ist dabei von Halogenatomen benachbarter AlX4--Ionen zusätzlich so koordiniert, daß es eine stark verzerrte oktaedrische EX3+3-Koordination aufweist.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 823-828 
    ISSN: 0044-2313
    Keywords: Tellurium ; niobium oxytrihalides ; hexatellurium(2+) ; tetrachlorooxoniobate (1-) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Prismatic Te62+ Ion in the Structure of Te6(NbOCl4)2Te6(NbOCl4)2 is obtained from Te, TeCl4 and NbOCl3 at 200°C. It crystallizes triclinic, space group P1 (a = 915,5(4) pm, b = 1655,3(6) pm, c = 3134,4(9) pm, α = 42,62(2)°, β = 117,12(6)°, γ = 138,24(8)°). The crystal structure analysis shows, that the structure is built of one-dimensional polymeric ∞1[NbOCl4-] chains in which the monomers are linked via linear O—Nb—O-bridges and from discrete Te62+ polycations that are also arranged in strands, but without significant interactions. The structure is closley related but not isotypic to the previously reported tungsten containing analogue Te6(WOCl4)2 (monoclinic, P21/c). A comparison of the two structures shows that rotations of the cationic strands relative to the anionic strands lead to different cation-anion interactions.
    Notes: Te6(NbOCl4)2 wird aus Te, TeCl4 und NbOCl3 bei 200°C erhalten. Es kristallisiert triklin, P1, a = 915,5(4) pm, b = 1655,3(6) pm, c = 3134,4(9) pm, α = 42,62(2)°, β = 117,12(6)°, γ = 138,24(8)°. Die Kristallstrukturanalyse zeigt, daß die Struktur aus eindimensional-polymeren, über O-Atome verknüpften ∞1[NbOCl4-]-Strängen und aus diskreten, strangartig angeordneten Te62+-Polykationen aufgebaut ist. Die Struktur ist eng verwandt, aber nicht isotyp mit derjenigen der analogen wolframhaltigen Verbindung Te6(WOCl4)2 (monoklin, P21/c). Ein Strukturvergleich zeigt, daß Verdrehungen der Kationenstränge relativ zu den Anionensträngen zu unterschiedlichen Kation-Anionwechselwirkungen führen.
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  • 3
    ISSN: 0044-2313
    Keywords: Cadmium(II) complex ; 1,2-bis(phenyltriazeno)benzene ligand ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Metal Complex with Neutral 1,2-Bis(phenyltriazeno)-benzene as Ligand: Synthesis and Crystal Structure of [Cd{PhN3(H)C6H4N3(H)Ph}{PhN3C6H4N3(H)Ph}2][Cd{PhN3(H)C6H4N3(H)Ph}{PhN3C6H4N3(H)Ph}2] is obtained in aqueous ammonia by the reaction of CdSO4 with an excess of 1,2-bis(phenyltriazeno)benzene. It forms orange red, air stable prismatic crystals with the monoclinic space group P21/c and a = 1217.7(2); b = 2161.8(6); c = 2008.3(5) pm; β = 100.07(6)º; Z = 4. The compound is composed of mononuclear complexes in which the Cd atom is coordinated by one chelating bis(phenyltriazeno)benzene and two monodentate 1-phenyltriazenido-2-phenyltriazeno benzene anions in a distorted tetrahedral arrangement. The Cd - N distances are in the range of 220.7 to 239.7 pm.
    Notes: [Cd{PhN3(H)C6H4N3(H)Ph}{PhN3C6H4N3(H)Ph}2] entsteht in ammoniakalischer Lösung aus CdSO4 und einem Überschuß an 1,2-Bis(phenyltriazeno)benzol in Form orangeroter, luftstabiler Kristalle. Es kristallisiert monoklin in der Raumgruppe P21/c mit a = 1217,7(2); b = 2161,8(6); c = 2008,3(5) pm; β = 100,07(6)º; Z = 4. Die Verbindung bildet einkernige Komplexe, in denen das Cd-Kation von einem chelatartig gebundenen Bis(phenyltriazeno)benzol und zwei einzähnig koordinierenden 1-Phenyltriazenido-2-phenyltriazenobenzol-Anionen verzerrt tetraedrisch umgeben ist. Die Cd - N-Abstände liegen im Bereich zwischen 220,7 und 239,7 pm.
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  • 4
    ISSN: 0044-2313
    Keywords: Tetrameric copper(II) complex ; μ2-oxo ligand ; 1-phenyltriazenido-2-phenyltriazeno benzene ligand ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Cu4[PhN3C6H4N3(H)Ph]4(μ2-O)2, a Tetranuclear Copper(II) Complex with 1-Phenyltriazenido-2-phenyltriazeno-benzene as LigandCu4[PhN3C6H4N3(H)Ph]4(μ-O)2 (1) results from the reaction of an aqueous solution of [Cu(NH3)4]2+ with 1,2-bis(phenyltriazeno)benzene in ether. 1 crystallizes in the orthorhombic space group Pba2 with the lattice parameters a = 1661.5(5), b = 1914.7(7), c = 1269.2(5) pm; Z = 2. In the tetrameric complex with the symmetry C2 the Cu2+ cations form a tetrahedron (Cu—Cu: 298.3(1)-337.1(1) pm). The μ2-oxo ligands occupy the twofold axis and bridge two opposite edges of the Cu4 tetrahedron (Cu—O: 190.0(3) and 192.5(4) pm). The 1-phenyltriazenido-2-phenyltriazeno benzene anions bridge two Cu2+ ions chelating one metal ion and coordinating monodentate the neighbouring one (Cu—N: 191.0(5)-204.1(4) pm).
    Notes: Cu4[PhN3C6H4N3(H)Ph]4(μ-O)2 (1) entsteht bei der Umsetzung einer wäßrigen Lösung von [Cu(NH3)4]2+ mit 1,2-Bis(phenyltriazeno)benzol in Ether. 1 kristallisiert orthorhombisch in der Raumgruppe Pba2 mit den Gitterkonstanten a = 1661,5(5); b = 1914,7(7); c = 1269,2(5) pm; Z = 2. Im tetrameren Komplex mit der Symmetrie C2 bilden die Cu2+-Ionen ein Tetraeder (Cu—Cu: 298,3(1)-337,1(1) pm). Die μ2-Oxoliganden liegen auf der C2-Achse und überbrücken zwei gegenüberliegende Tetraederkanten (Cu—O: 190,0(3) und 192,5(4) pm). Die 1-Phenyltriazenido-2-phenyltriazeno-benzol-Anionen verbrücken benachbarte Cu2+-Ionen, die sie einerseits chelatisierend und andererseits einzähnig koordinieren (Cu—N: 191,0(5)-204,1(4) pm).
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1971-1975 
    ISSN: 0044-2313
    Keywords: Tellurium ; niobium oxytrihalides ; poly(heptatellurium(2+)) ; tetrachlorooxoniobate (1-) ; tetrabromooxoniobate (1-) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tellurium Cations stabilized by Niobium Oxytrihalides: Synthesis and Crystal Structure of Te7NbOBr5 and Te7NbOCl5The reaction of Te2Br with NbOBr3 in a sealed evacuated glass ampoule at 225°C yields Te7NbOBr5 in form of bright black needles. Te7NbOCl5 is obtained from tellurium, TeCl4 and NbOCl3 at 220°C. Both compounds crystallize orthorhombic in the space group Pcca (Te7NbOBr5: a = 2 651,9(4) pm, b = 836.6(1) pm, c = 794.6(1) pm; Te7NbOCl5: a = 2 597.7(5) pm, b = 805.1(1) pm, c = 791.2(1) pm). The crystal structure determinations show that Te7NbOBr5 and Te7NbOCl5 are built of one-dimensional polymeric tellurium cations, one-dimensional associated pyramidal NbOX4 groups (X = Cl, Br) and isolated halide anions. Magnetic properties of Te7NbOX5 were determined and confirm the expected diamagnetism. Te7NbOX5 can thus be formulated as ∞1[Te72+] ∞1[NbOX4-] (X-). The charge distribution in the structure type Te7MOX5 (M = W, Nb; X = Cl, Br) became clear by synthesis and characterisation of the two niobium containing compounds.
    Notes: Durch Reaktion von Te2Br mit NbOBr3 in einer evakuierten Glasampulle bei 225°C entsteht Te7NbOBr5 in Form von schwarzglänzenden, stäbchenförmigen Kristallen. Te7NbOCl5 wird aus Te, TeCl4 und NbOCl3 bei 220°C erhalten. Beide Verbindungen kristallisieren im orthorhombischen Kristallsystem in der Raumgruppe Pcca (Te7NbOBr5: a = 2 651,9(4) pm, b = 836,6(1) pm, c = 794,6(1) pm; Te7NbOCl5: a = 2 597,7(5) pm, b = 805,1(1) pm, c = 791,2(1) pm). Die Kristallstrukturanalysen zeigen, daß Te7NbOBr5 und Te7NbOCl5 aus eindimensionalen polymeren Tellur-Kationen, eindimensionalen Strängen von pyramidalen, über O-Atome assoziierten NbOX4-Einheiten und aus isolierten Halogenidionen aufgebaut sind. Magnetische Messungen bestätigen den erwarteten Diamagnetismus und zeigen, daß Nb in der formalen Oxidationsstufe + V vorliegt. Die ionische Schreibweise lautet daher ∞1[Te72+] ∞1[NbOX4-] (X-). Die Synthese und Charakterisierung der beiden niobhaltigen Vertreter klärt die Ladungsverteilung im Strukturtyp Te7MOX5 (M = W, Nb; X = Cl, Br).
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 65-68 
    ISSN: 0044-2313
    Keywords: Thallium(III) complex ; di(4,4′-phenyltriazenido)-phenylmethane ligand ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of [Tl2(PhN3C6H4CH2C6H4N3Ph)3], a Dinuclear TlIII Complex with a Novel, Bridging Bistriazenido LigandTris[di(4,4′-phenyltriazenido)phenylmethane]-dithallium(III) is formed by the reaction of TlNO3 with di(4,4′-phenyltriazeno)phenylmethane in the presence of NaOH and air in an ethanol/H2O mixture. The compound is obtained as red, needlelike crystals from THF-hexane. It crystallizes monoclinic, space group I 2/a (a = 1375.2(5) pm, b = 2615(2) pm, c = 1957.0(8) pm, β = 93.49(3)°) with four dinuclear complexes in the unit cell. Each complex contains three doubly deprotonated bistriazenido ions (PhN3C6H4CH2C6H4N3Ph)2- and two Tl3+ ions. The Tl ions are each coordinated by three chelating triazenido groups resulting in a trigonal prismatic coordination of six N atoms. The Tl-N distances vary between 227 and 239 pm, all N-N distance of the triazenido groups are equal within standard deviations with a mean of 130 pm.
    Notes: Tris[di(4,4′-phenyltriazenido)phenylmethan]-di-thallium(III) entsteht durch Reaktion von TlNO3 mit Di(4,4′-phenyltriazeno)phenylmethan in Gegenwart von NaOH und Luft in einem Ethanol/H2O-Gemisch. Die Verbindung kann in Form roter, nudelförmiger Kristalle aus einem THF/Hexan-Gemisch erhalten werden. Sie kristallisiert monoklin in der Raumgruppe I 2/a mit den Gitterkonstanten a = 1375,2(5) pm, b = 2615(2) pm, c = 1957,0(8) pm, β = 93,49(3)° mit vier zweikernigen Komplexen in der Elementarzelle, von denen jeder aus drei doppelt deprotonierten Bistriazenido-Ionen (PhN3C6H4CH2C6H4N3Ph)2- und zwei Tl3+-Ionen aufgebaut ist. Die Tl-Ionen sind jeweils von drei Triazenidogruppen chelatförmig koordiniert, wodurch für die Kationen ein trigonal prismatisches Koordinationspolyeder aus sechs N-Atomen resultiert. Die Tl-N-Abstände variieren zwischen 227 und 239 pm, alle N-N-Abstände in den Triazenidogruppen sind innerhalb der Standardabweichungen gleich und betrugen im Mittel 130 pm.
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