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  • 1
    Electronic Resource
    Electronic Resource
    Die Kristallstrukturen von (NH4)2[ReCl6], [ReCl2(CH3CN)4]2[ReCl6] · 2CH3CN und [ReCl4(18-Krone-6)] (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 525-530 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium Complexes ; Syntheses ; IR spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structures of (NH4)2[ReCl6], [ReCl2(CH3CN)4]2[ReCl6] · 2CH3CN and [ReCl4(18)(Crown-6)]Brown single crystals of (NH4)2[ReCl6] are formed by the reaction of NH4Cl with ReCl5 in a suspension of diethylether. [ReCl2(CH3CN)4]2[ReCl6] · 2CH3CN crystallizes as brown crystal plates from a solution of ReCl5 in acetonitrile. Lustrous green single crystals of [ReCl4(18-crown-6)] are obtained by the reaction of 18-crown-6 with ReCl5 in a dichloromethane suspension. All rhenium compounds are characterized by IR spectroscopy and by crystal structure determinations.(NH4)2[ReCl6]: Space group Fm3m, Z = 4, 75 observed unique reflections, R = 0.01. Lattice constant at -70°C: a = 989.0(1) pm. The compound crystallizes in the (NH4)2[PtCl6] type, the Re—Cl distance is 235.5(1) pm.[ReCl2(CH3CN)4]2[ReCl6] · 2CH3CN: Space group P1, Z = 1, 2459 observed unique reflections, R = 0.12. Lattice dimensions at -60°C: a = 859.0(1), b = 974.2(7), c = 1287.3(7) pm, α = 102.69(5)°, b̃ = 105.24(7)°, γ = 102.25(8)°. The structure consists of two symmetry-independent [ReCl2(CH3CN)4]+ ions with trans chlorine atoms, [ReCl6]2- ions, and included acetonitrile molecules. In the cations the Re—Cl bond lengths are 233 pm in average, in the anion they are 235 pm in average.[ReCl4(18-crown-6)]: Space group P21/n, Z = 4, 3 633 observed unique reflections, R = 0.06. Lattice dimensions at -70°C: a = 1040.2(4), b = 1794.7(5), c = 1090.0(5) pm, b̃ = 108.91(4)°. The compound forms a molecular structure, in which the rhenium atom is octahedrally coordinated by the four chlorine atoms and by two oxygen atoms of the crown ether molecule.
    Notes: Braune Einkristalle von (NH4)2[ReCl6] entstehen durch Reaktion von NH4Cl mit ReCl5 in einer Diethylethersuspension. [ReCl2(CH3CN)4]2[ReCl6] · 2CH3CN kristallisiert als braune Kristallplättchen aus einer Lösung von ReCl5 in Acetonitril. Leuchtend grüne Einkristalle von [ReCl4(18-Krone-6)] entstehen durch Reaktion von 18-Krone-6 mit ReCl5 in einer Dichlormethansuspension. Die drei Rhenium-Verbindungen werden durch ihre IR-Spektren und durch Kristallstrukturanalysen charakterisiert.(NH4)2[ReCl6]: Raumgruppe Fm3m, Z = 4, 75 unabhängige beobachtete Reflexe, R = 0,01. Gitterkonstante bei -70°C: a = 989,0(1) pm. Die Verbindung kristallisiert im (NH4)2[PtCl6]-Typ, der Re—Cl-Abstand beträgt 235,5(1) pm.[ReCl2(CH3CN)4]2[ReCl6] · 2CH3CN: Raumgruppe P1, Z = 1, 2459 beobachtete unabhängige Reflexe, R = 0,12. Gitterkonstanten bei -60°C: a = 859,0(1); b = 974,2(7); c = 1287,3(7) pm, α = 102,69(5)°; b̃ = 105,24(7)°; γ = 102,25(8)°. Die Struktur besteht aus zwei symmetrieunabhängigen [ReCl2(CH3CN)4]+-Ionen mit trans-ständigen Chloratomen, [ReCl6]2--Ionen und eingelagerten Acetonitrilmolekülen. In den Kationen betragen die Re—Cl-Abstände im Mittel 233 pm, im Anion im Mittel 235 pm.[ReCl4(18-Krone-6)]: Raumgruppe P21/n, Z = 4, 3 633 beobachtete unabhängige Reflexe, R = 0,06. Gitterkonstanten bei -70°C: a = 1040,2(4); b = 1794,7(5); c = 1090,0(5) pm; b̃ = 108,91(4)°. Die Verbindung bildet eine Molekülstruktur, in der das Rheniumatom oktaedrisch von den vier Chloratomen und von zwei Sauerstoffatomen des Kronenethers koordiniert ist.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210404
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  • 2
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der Phosphanimin-Komplexe MCl2(Me3SiNPMe3)2 mit M = Zn und Co, und CoCl2(HNPMe3)2 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 431-437 
    Details
    ISSN: 0044-2313
    Keywords: Phosphaneimine Complexes of Zinc and Cobalt ; Synthesis ; IR spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Phosphaneimine Complexes MCl2(Me3SiNPMe3)2 with M = Zn and Co, and CoCl2(HNPMe3)2The molecular complexes MCl2(Me3SiNPMe3)2 (M = Zn, Co) have been prepared by the reaction of the dichlorides of zinc and cobalt with Me3SiNPMe3 in CH3CN and CH2Cl2, respectively, whereas the complex CoCl2(HNPMe3)2 has been prepared by the reaction of CoCl2 with NaF in boiling acetonitrile in the presence of Me3SiNPMe3. All complexes were characterized by IR spectroscopy and by crystal structure determinations. The complexes MCl2(Me3SiNPMe3)2 crystallize isotypically.ZnCl2(Me3SiNPMe3)2: Space group P212121, Z = 4, 2677 observed unique reflections, R = 0.024. Lattice dimensions at -70°C: a = 1243.6; b = 1319.0; c = 1464.7 pm.CoCl2(Me3SiNPMe3)2: Space group P212121, Z = 4, 3963 observed unique reflections, R = 0,071. Lattice dimensions at -80°C: a = 1236.3; b = 1317.4; c = 1457.6 pm.CoCl2(HNPMe3)2 · CH2Cl2: Space group Pbca, Z = 8, 1354 observed unique reflections, R = 0.055. Lattice dimensions at -80°C: a = 1247.3; b = 998.4; c = 2882.4 pm.All complexes have monomeric molecular structures, in which the metal atoms are coordinated in a distorted tetrahedral fashion by the two chlorine atoms and by the nitrogen atoms of the phosphaneimine molecules.
    Notes: Die Molekülkomplexe MCl2(Me3SiNPMe3)2 (M = Zn, Co) entstehen aus den wasserfreien Dichloriden von Zink und Cobalt mit Trimethylsilyl-trimethylphosphanimin in Dichlormethan bzw. Acetonitril, während der Trimethylphosphanimin-Komplex CoCl2(HNPMe3)2 aus CoCl2 mit Natriumfluorid in Gegenwart von Me3SiNPMe3 in siedendem Acetonitril gebildet wird. Die Verbindungen werden durch ihre IR-Spektren und durch Kristallstrukturanalysen charakterisiert. Die Komplexe MCl2(Me3SiNPMe3)2 (M = Zn, Co) sind miteinander isotyp.ZnCl2(Me3SiNPMe3)2: Raumgruppe P212121, Z = 4, Strukturlösung mit 2677 beobachteten unabhängigen Reflexen, R = 0,024. Gitterkonstanten bei -70°C: a = 1243,6; b = 1319,0; c = 1464,7 pm.CoCl2(Me3SiNPMe3)2: Raumgruppe P212121, Z = 4, Strukturlösung mit 3963 beobachteten unabhängigen Reflexen, R = 0,071. Gitterkonstanten bei -80°C: a = 1236,3; b = 1317,4; c = 1457,6 pm.CoCl2(HNPMe3)2 · CH2Cl2: Raumgruppe Pbca, Z = 8, Strukturlösung mit 1354 beobachteten unabhängigen Reflexen, R = 0,055. Gitterkonstanten bei -80°C: a = 1247,3; b = 998,4; c = 2882,4 pm.Alle Komplexe haben monomere Molekülstrukturen, in denen die Metallatome verzerrt tetraedrisch von den beiden Chloratomen und den N-Atomen der beiden Phosphaniminmoleküle koordiniert sind.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200305
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  • 3
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der Phosphaniminato-Komplexe [SbF2(NPEt3)]2 und [SbF(NPEt3)2]2 sowie von NMe4+SbF4-Professor Lothar Beyer zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 2016-2022 
    Details
    ISSN: 0044-2313
    Keywords: Phosphoraneiminato Complexes of Antimony(III) ; Fluoro Complexes ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of the Phosphoraneiminato Complexes [SbF2(NPEt3)]2 and [SbF(NPEt3)2]2 as well as of NMe4+SbF4-The title compounds have been prepared from antimony trifluoride with the silylated phosphaneimine Me3SiNPEt3 and [NMe4]F, respectively. They were characterized by IR spectroscopy and by crystal structure determinations.[SbF2(NPEt3)]2: Space group Pbca, Z = 8, structure determination with 1264 unique reflections, R1 = 0.028 for reflections with I 〉 2σ(I). Lattice dimensions at -80°C: a = 1284.8, b = 1162.4, c = 1380.4 pm. The compound forms centrosymmetric dimeric molecules, in which the Ψ-trigonal-bipyramidal coordinated antimony atoms are linked via μ2-N bridges of the NPEt3- ligands.[SbF(NPEt3)2]2: Space group P21/c, Z = 4, structure determination with 2270 unique reflections, R1 = 0.029 for reflections with I 〉 2μ(I). Lattice dimensions at -75°C: a = 815.8, b = 1121.2, c = 2068.5 pm, β = 101.09°. The compound forms centrosymmetric dimeric molecules, in which the Ψ-trigonal-bipyramidal coordinated antimony atoms are linked via μ2-N bridges of one of the two NPEt3- ligands. The other NPEt3- group is terminally connected.NMe4+SbF4-: Space group P21/c, Z = 4, structure determination with 1503 unique reflections, R1 = 0.069 for reflections with I 〉 2μ(I). Lattice dimensions at -50°C: a = 539.80, b = 896.10, c = 1760.3 pm, β = 90.338°. The compound includes monomeric SbF4- ions with distorted Ψ-trigonal-bipyramidal environment of the antimony atoms.
    Notes: Die Titelverbindungen entstehen durch Reaktion von Antimontrifluorid mit dem silylierten Phosphanimin Me3SiNPEt3 bzw. mit Tetramethylammonium-Fluorid. Sie werden IR-spektroskopisch und durch Kristallstrukturanalysen charakterisiert.[SbF2(NPEt3)]2: Raumgruppe Pbca, Z = 8, Strukturlösung mit 1264 unabhängigen Reflexen, R1 = 0,028 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -80°C: a = 1284,8; b = 1162,4; c = 1380,4 pm. Die Verbindung bildet zentrosymmetrische dimere Moleküle, in denen die Ψ-trigonal-bipyramidal koordinierten Antimonatome über μ2-N-Brücken der NPEt3--Liganden verknüpft sind.[SbF(NPEt3)2]2: Raumgruppe P21/c, Z = 4, Strukturlösung mit 2270 unabhängigen Reflexen, R1 = 0,029 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -75°C: a = 815,8; b = 1121,2; c = 2068,5 pm; β = 101,09°. Die Verbindung bildet zentrosymmetrische dimere Moleküle, in denen die Ψ-trigonal-bipyramidal koordinierten Antimonatome über μ2-N-Brücken eines der beiden NPEt3--Liganden verknüpft sind. Die zweite NPEt3--Gruppe ist terminal gebunden.NMe4+SbF4-: Raumgruppe P21/c, Z = 4, Strukturlösung mit 1503 unabhängigen Reflexen, R1 = 0,069 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -50°C: a = 539,80; b = 896,10; c = 1760,3 pm; β = 90,338°. Die Verbindung enthält monomere SbF4--Ionen mit verzerrt Ψ-trigonal-bipyramidaler Umgebung der Antimonatome.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966221203
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