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  • 1
    Electronic Resource
    Electronic Resource
    Se2NBr3, Se2NCl5, Se2NCl-6: New Nitride Halides of Selenium(III) and Selenium(IV) (1996)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 2 (1996), S. 1373-1378 
    Details
    ISSN: 0947-6539
    Keywords: ab initio calculations ; crystal structure ; halogen compounds ; nitrides ; selenium compounds ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Se2NBr3, a planar molecule shaped liked dividers, was formed by the reaction of SeBr4 with N(SiMe3)3, which reduced the selenium to the trivalent state. Under the same conditions, Se2NCl5 was obtained by the reaction of SeCl4 with N(SiMe3)3, retaining the tetravalent state of selenium. The molecule is formed by two edge-sharing pseudotrigonal bipyramids with selenium as their central atoms. Se2NCl5 reacts with PPh4Cl to form the Se2NCl-6 ion by the addition of a Cl- ion to only one of the two selenium atoms, resulting in pseudooctahedral coordination of this atom. Ab initio calculations for all the compounds reported confirm the experimentally determined structures.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chem.19960021108
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  • 2
    Electronic Resource
    Electronic Resource
    Über die Kronenetherkomplexe [K(15-Krone-5)2]3[Sb3I12], [TeCl3(15-Krone-5)][TeCl5] und [TeCl3(15-Krone-5)]2[TeCl6] (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 55-61 
    Details
    ISSN: 0044-2313
    Keywords: Crown ether complexes ; tellurium ; antimony ; syntheses ; i.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crown Ether Complexes [K(15-Crown-5)2]3[Sb3I12], [TeCl3(15-Crown-5)][TeCl5], and [TeCl3(15-Crown-5)]2[TeCl6]Orange-coloured crystals of [K(15-crown-5)2]3[Sb3I12] are formed in the reaction of potassium iodide with antimony triiodide and 15-crown-5 in acetonitrile solution. An X-ray structure determination reveals severe disorder of the crown ether molecules, which coordinate to the potassium atoms in a sandwich array; so only the [Sb3I12]3- ion and the potassium positions were ascertained. The anion is a centrosymmetric trimer (symmetry C2h), which can be understood as central SbI63- ion, coordinated by two SbI3 molecules. (Space group C2/m), Z = 2, 3263 observed, independent reflections, R = 0.06, lattice dimensions at 20°C: a = 2541.1 pm, b = 1441.7 pm, c = 1588.4 pm, β = 113.33°.The tellurium complexes [TeCl3(15-crown-5)] [TeCl5] and [TeCl3(15-crown-5)]2[TeCl6] are prepared by reaction of TeCl4 with 15-crown-5 in acetonitrile solution, forming yellow-green crystals sensitive to moisture. They are characterized by their i.r. spectra.
    Notes: Orange Kristalle [K(15-Krone-5)2]3[Sb3I12] entstehen durch Einwirkung von Kaliumiodid auf Antimontriiodid bei Anwesenheit von 15-Krone-5 in Acetonitrillösung. Wegen Fehlordnung der die Kaliumionen sandwichartig koordinierenden Kronenethermoleküle konnten röntgenogrpahisch in der Struktur nur das [Sb3I12]3--Ion sicher aufgeklärt werden. Es bildet ein zentrosymmetrisches Trimer (Symmetrie C2h), das sich als zentrales SbI63--Ion mit zwei koordinierten SbI3-Molekülen auffassen läßt. Raumgruppe C2/m, Z = 2, 3263 unabhängige beobachtete Reflexe, R = 6,2%. Gitterabmessungen bei 20 °C: a = 2541,1; b = 1441,7; c = 1588,4 pm, β = 113,33°.Die Tellurokomplexe [TeCl3(15-Krone-5)] [TeCl5] und [TeCl3(15-Krone-5)]2[TeCl6] entstehen aus TeCl4 und 15-Krone-5 in Acetonitrillösung als gelbgrüne, feuchtigkeitsempfindliche Kristalle, die durch ihre IR-Spektren charakterisiert werden.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915960108
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  • 3
    Electronic Resource
    Electronic Resource
    Benzamidinium-Hexachlorostannat Synthese und Kristallstruktur (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 133-138 
    Details
    ISSN: 0044-2313
    Keywords: Benzamidinium hexachlorostannate ; synthesis ; crystal structure ; i.r. spectrum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Benzamidinium Hexachlorostannate: Synthesis and Crystal Structure[Ph—C(NH2)2SnCl6] has been prepared by the reaction of hydrogen chloride with the amidinato complex [Ph—C(NSiMe3)2SnCl3] in CH2Cl2 solution, forming colourless crystals. which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P21/c, Z = 4, 3070 observed unique reflexions, R = 0.029. Lattice dimensions at -50°C: a = 892.5, b = 1076.7, c = 1175.6 pm, β = 109.3°. The compound consists of benzamidinium ions C6H5—C(NH2)2+ and anions SnCl62-, which are connected by a network of N—H…Cl hydrogen bridges.
    Notes: [Ph—C(NH2)2]2SnCl6 entsteht in Form farbloser Einkristalle durch Einwirkung von Chlorwasserstoff auf eine Lösung des Amidinatokomplexes [Ph—C(NSiMe3)2SnCl3] in Dichlormethan. Die Verbindung wird durch das IR-Spektrum und durch eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, 3070 beobachtete unabhängige Reflexe, R = 2,9%. Gitterabmessungen bei -50°C: a = 892,5; b = 1076,7; c = 1175,6 pm; β = 109,3°. Die Verbindung besteht aus Benzamidinium-Kationen C6H5—C(NH2)2+ und SnCl62--Ionen, in denen ein Netz von N—H…Cl-Wasserstoffbrücken besteht.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915960118
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  • 4
    Electronic Resource
    Electronic Resource
    Trimethylsilyl-substituierte Amidinatokomplexe von Thallium(III). Die Kristallstruktur von [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2 TICI3]Herrn Professor Eberhard Hoyer zum 60. Geburtstage am 26. Mai 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 600 (1991), S. 7-14 
    Details
    ISSN: 0044-2313
    Keywords: Amidinato complexes of thallium(III) ; syntheses ; i.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trimethylsilyl Substituted Amidinato Complexes of Thallium(III). The Crystal Structure of [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3]The amidinato complexes [Ph—C(NSiMe3)2TlCl3] and [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] have been prepared by the reaction of TlCl3 with N,N,N′-tris(trimethylsilyl)benzamidine in THF solution. They were characterized by IR spectroscopy, [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] additionally by an X-ray structure determination. Space group P21/c, Z = 4, 4300 observed unique reflexions, R = 0.053. Lattice dimensions at -43°C: a = 1157.2, b = 2346.3, c = 1536.9 pm, β = 105.98°. The structure consists of amidinium cations, and of anions [Ph—C(NSiMe3)2TlCl3]-, in which the thallium atom is fivefold surrounded by three chlorine atoms and by two nitrogen atoms of the amidinato chelate.
    Notes: Die Amidinatokomplexe [Ph—C(NHSiMe3)2TlCl2] und [Ph—C(NHSiMe3)2TlCl2] [Ph—C(NSiMe3)2TlCl3] entstehen bei der Einwirkung von Thallium(III)-chlorid auf N,N,N′-Tris(trimethylsilyl)benzamidin in Tetrahydrofuranlösung. Sie werden durch ihre IR-Spektren, und [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] zusätzlich durch eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, 4300 unabhängige beobachtete Reflexe, R = 5,3%. Die Gitterkonstanten betragen bei -43°C: a = 1157,2; b = 2346,3; c = 1536,9 pm; β = 105,98°. Die Verbindung besteht aus einem Amidiniumkation und einem [Ph—C(NSiMe3)2TlCl3]--Anion, in dem das Thalliumatom verzerrt trigonal-bipyramidal von drei Cl-Atomen und chelatartig von den beiden N-Atomen des Amidinatoliganden umgeben ist.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916000102
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  • 5
    Electronic Resource
    Electronic Resource
    Synthese, Kristallstruktur und 121Sb-Mößbauer-Spektrum von [SbCl2(18-Krone-6)]+SbCl6- (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 93-97 
    Details
    ISSN: 0044-2313
    Keywords: Crown ether complex of antimony ; synthesis ; 121Sb-Mössbauer spectrum ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure, and 12Sb-Mössbauer Spectrum of [SbCl2(18-Crown-6)]+SbCl6-The title compound, which has been prepared by the reaction of antimony trichloride and antimony pentachloride in the presence of 18-crown-6 in acetonitrile solution, is characterized by its 121Sb-Mössbauer spectrum and by an X-ray structure determination. Space group P21, Z = 2, 2439 observed unique reflections, R = 0.045, wR = 0.043. Lattice dimensions at -80°C: a = 780.6(7), b = 1297.5(9), c = 1 278.5(10) pm, β = 100.56(7)°. The structure of [SbCl2(18-crown-6)]+SbCl6- contains cations in which the antimony atom in the first coordination sphere is surrounded in a φ-trigonal-bipyramidal fashion by two oxygen atoms of the crown ether in axial position as well as in the equatorial position by the two chlorine atoms and the lone electron pair.
    Notes: Die Titelverbindung entsteht aus Antimontrichlorid und Antimonpentachlorid in Gegenwart von 18-Krone-6 in Acetonitrillösung. Sie wird durch ihr 121Sb-Mößbauer-Spektrum und durch eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P21, Z = 2, 2439 beobachtete unabhängige Reflexe, R = 4,50%, wR = 4,25%. Die Gitterkonstanten betragen bei -80°C: a = 780,6(7); b = 1 297,5(9); c = 1 278,5(10) pm, β = 100,56(7)°. [SbCl2(18-Krone-6)]+SbCl6- enthält Kationen, in denen das Antimonatom in erster Koordinationssphäre φ-trigonal-bipyramidal von zwei O-Atomen des Kronenethers in Axialposition und von den beiden Cl-Atomen sowie dem freien Elektronenpaar äquatorial umgeben ist.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926180117
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  • 6
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur von [Li(12-Krone-4)2][ReCl5(CH3CN)] · CH3CNHerrn Professor Joseph Grobe zum 60. Geburtstage am 2. November 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 109-117 
    Details
    ISSN: 0044-2313
    Keywords: Pentachlorohenate(IV)-acetonitrile solvate ; synthesis ; IR spectrum ; 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 [Li(12-Crown-4)2][ReCl5(CH3CN)] · CH3CNThe title compound has been prepared by the reaction of lithium chloride with rhenium pentachloride in the presence of 12-crown-4 in acetonitrile solution.[Li(12-crown-4)2][ReCl5(CH3CN)] · CH3CN has been characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P1, Z = 2, 4 450 observed unique reflections, R = 0.047, Lattice dimensions at 20°C: a = 1 445.8, b = 1 463.2, c = 1 580.2 pm, α = 89.28°, β = 114.19°, γ = 89.40°. The compound is ionic, the cation being formed by a lithium ion coordinated by the eight oxygen atoms of two crown ether molecules 12-crown-4 in sandwich fashion. In the anions [ReCl5(CH3CN)]- the rhenium atoms are in a distorted octahedral shape by the five chlorine atoms and by the N atom of the acetonitrile molecule. The two crystallographically independent cations and anions, respectively, are only slightly different.
    Notes: Die Titelverbindung wurde durch Reaktion von Lithiumchlorid mit Rheniumpentachlorid in Gegenwart von 12-Krone-4 in Acetonitrillösung hergestellt und durch ihr IR-Spektrum und durch eine röntgenographische Strukturanalyse charakterisiert.[Li(12-Krone-4)2][ReCl5(CH3CN)] · CH3CN kristallisiert triklin in der Raumgruppe P1 mit zwei Formeleinheiten pro Elementarzelle, 4 450 beobachtete unabhängige Reflexe, R = 4,7%. Gitterabmessungen bei 20°C: a = 1 445,8; b = 1 463,2; c = 1 580,2 pm; α = 89,28°; β = 114,19°; γ = 89,40°. Die Verbindung hat einen ionischen Aufbau, in dem die Lithiumionen sandwichartig von den acht Sauerstoffatomen zweier Kronenethermoleküle 12-Krone-4 koordiniert sind. In den Anionen [ReCl5(CH3CN)]- sind die Rheniumatome verzerrt oktaedrisch von den fünf Chloratomen und von dem N-Atom des Acetonitrilmoleküls umgeben. Die beiden kristallographisch unabhängigen Kationen bzw. Anionen unterscheiden sich nur wenig voneinander.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916060112
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  • 7
    Electronic Resource
    Electronic Resource
    Die Kristallstruktur von [MoO2F2(2,2′-Bipyridyl)] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 117-120 
    Details
    ISSN: 0044-2313
    Keywords: 2,2′-Bipyridyl molybdenum difluoridedioxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of [MoO2F2(2,2′-bipyridyl)]The title compound crystallizes in the space group P21/n with a = 869.6(1), b = 1390.1(3), c = 959.0(1) pm, β = 110.967(5)°, Z = 4; structure determination with 1718 observed independent reflections, R = 0.031. The compound consists of molecules having two cis oxo ligands and a bipyridyl chelate in the MoO2 plane.
    Notes: Die Titelverbindung kristallisiert in der Raumgruppe P21/n mit a = 869,6(1); b = 1390,1(3); c = 959,0(1) pm; β = 110,967(5)°, Z = 4; Strukturbestimmung mit 1718 beobachteten unabhängigen Reflexen, R = 3,1%. Die Verbindung besitzt eine Molekülstruktur mit cis-ständigen Oxoliganden und dem Bipyridylchelat in der MoO2-Ebene.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926100119
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  • 8
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur des tetrameren Nitridokomplexes [Cu(CH3CN)4]2[W4N4Cl14(CH3CN)2] (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 775-778 
    Details
    ISSN: 0044-2313
    Keywords: Nitrido complex of tungsten ; synthesis ; IR-spectrum ; 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 the Tetrameric Nitrido Complex [Cu(CH3CN)4]2[W4N4Cl14(CH3CN)2].The title compound has been prepared by the reaction of CuCl with WNCl3 in acetonitrile solution, forming red, moisture sensitive crystals. They were characterized by IR spectroscopy and by an X-ray structure determination. Space group I2/a, Z = 4, 2 027 observed unique reflections, R = 0.049. Lattice dimensions at -80°C: a = 2 527.0, b = 971.9, c = 2 137.5 pm, β = 106.01°. The compound consists of [Cu(CH3CN)4]+ ions, which are arranged to form strands, and of anions [W4N4Cl14(CH3CN)2]2-, in which the tungsten atoms were located at the vertices of a square and are linked with one another via linear W≡N—W bridges. Two of the four tungsten atoms have four chlorine atoms as terminal ligands, the other two tungsten atoms have three chlorine atoms and an acetonitrile molecule as terminal ligands.
    Notes: Die Titelverbindung wird durch Umsetzung von Kupfer(I)chlorid mit WNCl3 in Acetonitril in Form roter feuchtigkeitsempfindlicher Kristalle gewonnen. Sie wird durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe I2/a, Z = 4, 2 027 beobachtete unabhängige Reflexe, R = 4,9%. Gitterkonstanten bei -80°C: a = 2 527,0; b = 971,9; c = 2 137,5 pm; β = 106,01°. Die Verbindung besteht aus [Cu(CH3CN)4]+-Ionen, die zu Strängen angeordnet sind, und Anionen [W4N4Cl14(CH3CN)2]2-, in denen die Wolframatome an den Ecken eines Quadrats angeordnet sind und über lineare W≡N—W-Brücken verknüpft sind. Zwei der Wolframatome haben je vier Chloratome als terminale Liganden, die beiden anderen je drei Chloratome und je ein N-Atom eines Acetonitrilmoleküls als terminale Liganden.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190423
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  • 9
    Electronic Resource
    Electronic Resource
    Synthese, Kristallstrukturen und 121Sb-Mößbauer-Spektren von [SbBr3(15-Krone-5)], [SbBr2Me(15-Krone-5)] und [SbBr2Ph(15-Krone-5)] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 611 (1992), S. 149-157 
    Details
    ISSN: 0044-2313
    Keywords: Antimony crown ether complexes ; preparation ; crystal structure ; IR, 121Sb-Mössbauer spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure, and 121Sb-Mössbauer Spectra of [SbBr3(15-Crown-5)], [SbBr2Me(15-Crown-5)], and [SbBr2Ph(15-Crown-5)]The compounds [SbBr3(15-crown-5)] (1), [SbBr2Me(15-crown-5)] (2), [SbBr2Ph(15-crown-5)] (3), and [SbCl2Me(15-crown-5)] (4) are formed by the reaction of 15-crown-5 with SbBr3, SbBr2Me, SbBr2Ph, and SbCl2Me, respectively, in toluene solution at -40°C. The complexes were characterized by IR spectroscopy, 121Sb-Mössbauer spectroscopy, 1-3 as well as by X-ray structure determinations. 1: Space group P212121, Z = 4, 1735 observed, independent reflections, R = 0.050, Lattice dimensions at -65°C: a = 787.03(7); b = 1313.0(2); c = 1619.3(2) pm.2: Space group Pca21, Z = 8, 2730 observed, independent reflections, R = 0.050, Lattice dimensions at -65°C: a = 1308.2(2); b = 1611.8(2); c = 1640.5(3) pm.3: Space group P21/n, Z = 4,2458 observed, independent reflections, R = 0.040, Lattice dimensions at -60°C: a = 900.3(3); b = 1390.6(6); c = 1618.5(7) pm, β = 96.32(3)°.The complexes 1-3 have molecular structures, in which the antimony atoms are surrounded by the five oxygen atoms of the crown ether molecule and by three ligands Br3, Br2CH3, Br2Ph, respectively.
    Notes: Die Molekülkomplexe [SbBr3(15-Krone-5)] (1), [SbBr2Me(15-Krone-5)] (2), [SbBr2Ph(15-Krone-5)] (3) und [SbCl2Me(15-Krone-5)] (4) entstehen in Toluol bei -40°C aus den Komponenten 15-Krone-5 und SbBr3, SbBr2Me, SbBr2Ph, bzw. SbCl2Me. Die Komplexe werden durch IR-Spektren, durch 121Sb-Mößbauer-Spektren und 1-3 durch Kristallstrukturanalysen charakterisiert. 1: Raumgruppe P21212121, Z = 4, 1 735 beobachtete unabhängige Reflexe, R = 5,0%, Gitterabmessungen bei -65°C: a = 787,03(7); b = 1313,0(2); c = 1619,3(2)pm.2: Raumgruppe Pca21, Z = 8,2730 beobachtete, unabhängige Reflexe, R = 5,0%, Gitterabmessungen bei -65°C: a= 1308,2(2); b = 1611,8(2); c = 1640,5(3) pm.3: Raumgruppe P21/n, Z = 4, 2 458 beobachtete, unabhängige Reflexe, R = 4,0%, Gitterabmessungen bei -60°C: A = 900,3(3); b= 1 390,6(6); c =1 618,5(7) pm, β = 96,32(3)°.Die Komplexe 1, 2 und 3 haben Molekülstrukturen, in denen die Antimonatome von den fünf O-Atomen des Kronenethers 15-Krone-5 und jeweils drei Ligandatomen Br3, Br2CH3 bzw. Br2Ph koordiniert sind. Das freie Elektronenpaar an den Antimon(III)-Atomen weist vermutlich in Richtung auf den durch die Kronenethermoleküle gebildeten Hohlraum.
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    URL: http://dx.doi.org/10.1002/zaac.19926110525
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  • 10
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    Electronic Resource
    Chelatkomplexe von Rheniumtetrachlorid. Die Kristallstrukturen von ReCl4(DME) und ReCl4(DPPE) · Tolan (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 49-54 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium tetrachloride chelate complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chelate Complexes of Rhenium Tetrachloride. The Crystal Structures of ReCl4(DME) and ReCl4(DPPE) · TolanBright green crystals of ReCl4(DME) have been prepared by the reaction of rhenium pentachloride with dimethoxyethane (DME) in dichloromethane. ReCl4(DPPE) · tolan was obtained in form of red crystals by the reaction of the alkyne complex [ReCl4(Ph—C≡C—Ph)(POCl3)] with bis(diphenylphosphino)ethane (DPPE) in dichloromethane. The complexes were characterized by X-ray structure determinations.ReCl4(DME): Space group I42d, Z = 8, 829 observed unique reflexions, R = 0.022. Lattice dimensions at 19.5°C: a = b = 960.60(6), c = 2337.2(6) pm. The complex forms monomeric molecules with DME as chelating ligand; the Re—O bond lengths are 213.1 pm. The chlorine atoms, arranged in trans position to the chelating ligand, have slightly shorter Re—Cl bonds than the chlorine atoms in cis position (232,1 pm).ReCl4(DPPE) · tolan: Space group P21/n, Z = 4,4313 observed unique reflexions, R = 0.040. Lattice dimensions at -80°C: a = 1095.7(1), b = 1764.2(2), c = 1898.0(2) pm, β = 99.229(8)°. The compound consists in form of monomeric molecules [ReCl4(DPPE)] and diphenylacetylene molecules, which are incorporated in the lattice. The two phenyl rings of the tolan molecules are twisted towards each other along the C—C axis with a dihedral angle of 21°. The DPPE molecules are bonded to the rhenium atom in a chelating fashion with medium Re—P lengths of 250.4 pm. The chlorine atoms, arranged in trans position to this ligand, with Re—Cl bond lengths of 234.5 pm are slightly longer than the Re—Cl bonds in cis position with 232.3 pm.
    Notes: ReCl4(DME) wird in Form leuchtend grüner Kristalle durch Reaktion von Rheniumpentachlorid mit Dimethoxyethan (DME) in Dichlormethan hergestellt. ReCl4(DPPE) · Tolan erhielten wir als rote Kristalle bei der Reaktion des Alkinkomplexes [ReCl4(Ph—C≡C—Ph)(POCl3)] mit Bis(diphenylphosphino)ethan (DPPE) in Dichlormethan. Die Komplexe wurden durch röntgenographische Strukturanalysen charakterisiert.ReCl4(DME): Raumgruppe I42d, Z = 8, 829 beobachtete unabhängige Reflexe, R = 2,2%. Gitterkonstanten bei 19,5°C: a = b = 960,60(6); c = 2337,2(6) pm. Der Komplex bildet monomere Moleküle mit dem DME-Liganden als Chelat und Re—O-Abständen von 213,1 pm. Die hierzu trans-ständig angeordneten Chloratome haben mit 228,1 pm etwas kürzere Re—Cl-Bindungen als die cis-ständigen Cl-Atome (232,1 pm).ReCl4(DPPE) · Tolan: Raumgruppe P21/n, Z = 4, 4313 beobachtete, unabhängige Reflexe, R = 4,0%. Gitterkonstanten bei -80°C: a = 1095,7(1); b = 1764,2(2); c = 1898,0(2) pm, β = 99,229(8)°. Der Komplex bildet monomere Moleküle [ReCl4(DPPE)] und in das Gitter eingelagerte Diphenylacetylenmoleküle, deren Phenylringe einen Diederwinkel von 21° zueinander bilden. Die DPPE-Moleküle sind chelatartig am Rheniumatom gebunden mit Abständen Re—P von im Mittel 250,4 pm. Die hierzu trans-ständig angeordneten Chloratome sind mit Re—Cl—Abständen von 234,5 pm etwas länger als die cis-ständigen Re—Cl-Bindungen mit 232,3 pm.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926130108
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