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  • Syntheses  (10)
  • synthesis  (7)
  • syntheses  (5)
  • Molybdenum  (2)
  • Nitrido ligand  (2)
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  • 1
    Electronic Resource
    Electronic Resource
    Donor-Akzeptorkomplexe [SnCl4(Se4N2)2] und [TiCl4(Se4N2)] (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 73-78 
    Details
    ISSN: 0044-2313
    Keywords: Complexes of tetraselenium-dinitride ; syntheses ; IR-spectra ; 119Sn-Mössbauer spectrum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Donor-Acceptor Complexes [SnCl4(Se4N2)2] and [TiCl4(Se4N2)]The donor-acceptor complexes [SnCl4(Se4N2)2] and [TiCl4(Se4N2)] have been prepared by the reactions of Se4N2 with SnCl4 and TiCl4, respectively, in CH2Cl2 suspensions, forming red-brown, moisture sensitive crystal powders. The complexes are characterized by i. r. spectroscopy, the tin compound additionally by 119Sn Mössbauer spectroscopy. According to the spectra, in the tin complex both Se4N2 molecules are bonded with one of the nitrogen atoms at the tin atom in transposition (symmetry Ci), whereas in the titanium complex we assume both nitrogen atoms to be bonded in a chelating fashion at the titanium atom.
    Notes: Die Donorakzeptorkomplexe [SnCl4(Se4N2)2] und [TiCl4(Se4N2)] werden aus den Komponenten Se4N2 und SnCl4 bzw. TiCl4 in CH2Cl2-Suspensionen in Form rotbrauner, feuchtigkeitsempfindlicher Kristallpulver hergestellt. Die Komplexe werden durch ihre IR-Spektren, die Zinnverbindung zusätzlich durch das 119Sn-Mößbauer-Spektrum charakterisiert. Danach sind die Se4N2-Moleküle in der Zinnverbindung in trans-Position über je ein N-Atom an das Zinnatom koordiniert (Symmetrie Ci), während in dem Titankomplex vermutlich beide N-Atome des Se4N2-Moleküls chelatartig an das Titanatom gebunden sind.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916060107
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  • 2
    Electronic Resource
    Electronic Resource
    Halogeno-Nitrosylkomplexe von Molybdän und Wolfram. Die Kristallstrukturen von [Na2(15-Krone-5)2(CH3CN)][MoCl4(NO)2] und [Na(15-Krone-5)]2[MoF4Cl(NO)]Professor Ekkehard Fluck zum 60. Geburtstag am 27. Februar 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 592 (1991), S. 59-72 
    Details
    ISSN: 0044-2313
    Keywords: Molybdenum ; Tungsten ; Halogenonitrosyl Complexes ; Syntheses ; IR Spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Halogeno-Nitrosyl Complexes of Molybdenum and Tungsten. Crystal Structures of [Na2(15-Crown-5)2(CH3CN)][MoCl4(NO)2] and [Na(15-Crown-5)]2[MoF4Cl(NO)]MoCl2(NO)2 and WCl2(NO)2, respectively, react with excess sodium fluoride in acetonitrile at room temperature and in the presence of 15-crown-5 to give crystalline mixtures, which consist of the title compounds, respectively of [Na(15-crown-5)]2[WCl4(NO)2] and [Na(15-crown-5)]2[WF4Cl(NO)], and which can be separated by selection. The complexes are characterized by their i.r. spectra, the molybdenum compounds additionally by crystal structure determinations.[Na2(15-crown-5)2(CH3CN)][MoCl4(NO)2]: Space group P21, Z = 2, 5415 independent unique reflexions, R = 0.039. Lattice dimensions at -10°C: a = 984.3, b = 1231.1, c = 1483.0 pm, β = 105.67°. The compound consists of cations [Ne(l5-crown-5)(CH3CN)]+, in which the sodium ion is surrounded by the five O-atoms of the crown ether and by the N-atom of the acetonitrile molecule, as well as of anions, which form an ion pair {Na(15-crown-5)[MoCl4(NO)2]}-. In the in pairs the sodium ion is coordinated by the five oxygen atoms of the crown ether and by two chlorine atoms of the [MoCI4(NO)2]2- unit. The nitrosyl ligands take the cis-position a t the molybdenum atom which is in a distorted octahedrally fashion.[Na(15-crown-5)]2[MoF4Cl(NO)]. Space group C2/c, Z = 4, 1933 independent unique reflexions, R = 0.078. Lattice dimensions at -7O°C: D : 1.585.8, b = 1171.5, c = 1771.5 pm, β = 114.91°. The compound forms an ion triple, in which the sodium ions are linked to five oxygen atoms each of the crown ether molecules, and to two F-atoms of the [MoF4Cl(NO)]2- unit. The F-atom which is arranged in trans-position to the nitrosyl ligand coordinates with both sodium ions; thus an unusual T-shaped arrangement results for this F-atom. The sole terminal F-Atom and the Cl-atom are disordered in two positions.
    Notes: MoCl2(NO)2 bzw. WCl2(NO)2 reagieren mit überschüssigem Natriumfluorid in Acetonitril bei R.T. und Anwesenheit von 15-Krone-5 zu Kristallgemischen, die aus den Titelverbindungen bzw. aus [Na(15-Krone-5)]2[WCl4(NO)2] und [Na(15-Krone-5)]2[WF4Cl(NO)] bestehen, und die sich durch Auslesen trennen lassen. Die Komplexe werden durch ihre IR-Spektren, die Molybdänverbindungen zusätzlich durch Kristallstrukturanalysen charakterisiert.[Na2(15-Krone-5)2(CH3CN)][MoCl4(NO)2]: Raumgruppe P21, Z = 2, 5415 unabhängige beobachtete Reflexe, R = 3,9%. Gitterabmessungen bei -10°C: a = 984,3; b = 1 251,1; c = 1 483,0 pm, β = 105,67°. Die Verbindung besteht aus Kationen [Na(15-Krone-5)(CH3CN)]+, in denen das Natriumion von den fünf O-Atomen des Kronenethers und von dem N-Atom des Acetonitrilmoleküls umgeben ist, sowie aus Anionen, die ein Ionenpaar {Na(15-Krone-5)[MoCl4(NO)2]}- bilden. In ihnen ist das Natriumion durch die fünf O-Atome des Kronenethers und durch zwei Chloratome der [MoCl4(NO)2]2--Einheit koordiniert. Die Nitrosylliganden nehmen die cis-Positionen am verzerrt oktaedrisch koordinierten Molybdänatom ein.[Na(15-Krone-5)]2[MoF4Cl(NO)]: Raumgruppe C2/c, Z = 4, 1933 unabhängige beobachtete Reflexe, R = 7,8%. Gitterabmessungen bei -70°C: a = 1 585,8; b = 1 171,2; c = 1 771,5 pm; β = 114,91°. Die Verbindung bildet ein Ionentripel, in dem die Natriumionen mit je fünf O-Atomen der Kronenethermoleküle und mit zwei F-Atomen der [MoF4Cl(NO)]2--Einheit verbunden sind. Das in trans-Position zum Nitrosylliganden angeordnete F-Atom koordiniert mit beiden Natriumionen, so daß für dieses F-Atom eine ungewöhnliche T-förmige Anordnung resultiert. Das einzige terminal gebundene F-Atom und das Cl-Atom sind in zwei Positionen fehlgeordnet.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915920107
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  • 3
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    Electronic Resource
    Sterisch abgeschirmte Nitridokomplexe von Molybdän und Wolfram Die Kristallstrukturen von [MoN(NPh2)3] und [W4N4(NPh2)6(OnC4H9)2]Professor Josef Goubeau in memoriam (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 593 (1991), S. 99-110 
    Details
    ISSN: 0044-2313
    Keywords: Molybdenum ; Tungsten ; Nitrido Complexes ; Syntheses ; 1H, 13C NMR ; IR Spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Stericly Shielded Nitrido Complexes of Molybdenum and Tungsten. The Crystal Structures of [MoN(NPh2)3] and [W4N4(NPh2)6(OnC4H9)2]The reactions of MoNCl3 and WNCl3, respectively, with lithium diphenylamide in tetrahydrofurane produce the monomeric nitrido complexes MN(NPh2)3 with CN = 4 at the metal atoms. In the presence of lithium-n-butyl LiNPh2 and WNCl3 also form the tetrameric nitrido complex [W4N4(NPh2)6(OnC4H9)2] which contains WV and WVI. The compounds are characterized by their i.r. spectra, by X-ray structural analysis, and, partially, by 1H and 13C n.m.r. spectroscopy.MoN(NPh2)3: Space group P1, Z = 2, 4060 observed independent reflexions, R = 0.031. Lattice dimensions at 20°C: a = 956.2(4) pm, b = 1 015.9(2) pm, c = 1 598.1(3) pm; α = 79.06(2)°, β = 85.67(3)°, γ = 82.57(3)°. The compound forms monomeric molecules with Mo≡N bond lengths of 163.4 pm and mean Mo—NPh2 distances of 199.2 pm.[W4N4(NPh2)6(OnC4H9)2]: Space group P21/n, Z = 2, 1903 observed independent reflexions, R=0.039. Lattice parameters at 19°C: a = 1582.2(3) pm, b = 1182.4(2) pm, c = 2053.3(4) pm; β = 103.77(2)°. The compound forms centrosymmetric molecules, in which the central W-W dumb-bell (bond length 253.5 pm) is linked by the nitrido ligands of two WN2(NPh2)2=units in a T shaped order of the N-atoms.
    Notes: Die Umsetzungen von MoNCl3 bzw. WNCl3 mit Lithium-Diphenylamid in Tetrahydrofuran führen zu den monomeren Nitridokomplexen MN(NPh2)3 mit KZ = 4 an den Metallatomen. Bei Anwesenheit von Lithium-n-butyl reagiert LiNPh2 mit WNCl3 auch zu dem tetrameren, Wolfram(V) und Wolfram(VI) enthaltenden Nitridokomplex [W4N4(NPh2)6(OnC4H9)2]. Die Verbindungen werden durch ihre IR-Spektren, zum Teil durch die 1H- und 13C-Kernresonanzspektren sowie durch Röntgenstrukturanalysen charakterisiert.MoN(NPh2)3: Raumgruppe P1, Z = 2, 4060 unabhängige beobachtete Reflexe, R = 3,1%. Gitterabmessungen bei 20°C: a = 956,2(4); b = 1015,9(2); c = 1598,1(3) pm; α = 79,06(2)°; β = 85,67(3)°; γ = 82,57(3)°. Die Verbindung bildet monomere Moleküle mit Bindungslängen Mo≡N 163,4 pm und Mo—NPh2 von im Mittel 199,2 pm.[W4N4(NPh2)6(OnC4H9)2]: Raumgruppe P21/n, Z = 2, 1903 beobachtete unabhängige Reflexe, R = 3,9%. Gitterabmessungen bei 19°C: a = 1 582,2(3); b = 1 182,4(2); c = 2 053,3(4) pm; β = 103,77(2)°. Die Verbindung bildet zentrosymmetrische Moleküle, deren zentrale W - W-Hantel (Bindungslänge 253,5 pm) über die Nitridoliganden zweier WN2(NPh2)2-Einheiten mit T-förmiger Anordnung der N-Atome verknüpft ist.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915930110
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  • 4
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    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.
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    URL: http://dx.doi.org/10.1002/zaac.19916000102
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  • 5
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der Polytelluridokomplexe (PPh4)4[M2Te12] von Kupfer(I) und Silber(I)Professor Hartmut Bärnighausen zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 253-260 
    Details
    ISSN: 0044-2313
    Keywords: Polytellurido complexes of copper and silver ; synthesis ; 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 Polytellurido Complexes (PPh4)4[M2Te12] of Copper(I) and Silver(I)The title compounds have been prepared as black crystal needles by reactions of Na2Te3 with CuCl and AgNO3, respectively, in dimethylformamide in the presence of PPh4Br. With regard to the large cell dimensions the crystal structure determinations were done by an imaging plate instrument.(PPh4)4[Cu2Te12]: Space group P21/n, Z = 6, 51 338 detected reflections, structure determination with 14 177 unique reflections with I 〉 4σ(I), R = 0.081. Lattice dimensions at - 50°C: a = 1 704.5, b = 1 694.5, c = 5 044 pm, β = 94.20°.(PPh4)4[Ag2Te12]: Space group P21/n, Z = 6, 80 811 detected reflections, structure determination with 16 092 unique reflections with I 〉 3σ(I), R = 0.052. Lattice dimensions at - 50°C: a = 1 703.8, b = 1 722.9, c = 5 123 pm, β = 94.65°.The structures of the isotypic compounds consist of six symmetry independent PPh4+ ions and two symmetry independent anions [M2Te12]4-, in which the metal atoms of two (MTe4)--fivering fragments are linked by a Te42- chain.
    Notes: Die Titelverbindungen entstehen als schwarze Kristallnadeln aus Na2Te3 und CuCl bzw. AgNO3 in Dimethylformamid in Gegenwart von PPh4Br. Wegen der großen Zellabmessungen wurden die Kristallstrukturen mit Hilfe des Flächendetektors der Firma Stoe vermessen.(PPh4)4[Cu2Te12]: Raumgruppe P21/n, Z = 6, 51 338 gemessene Reflexe, Strukturlösung mit 14 177 unabhängigen Reflexen mit I 〉 4σ(I), R = 0,081. Gitterabmessungen bei - 50°C: a = 1 704,5; b = 1 694,5; c = 5 044 pm; β = 94,20°.(PPh4)4[Ag2Te12]: Raumgruppe P21/n, Z = 6, 80 811 gemessene Reflexe, Strukturlösung mit 16 092 unabhängigen Reflexen, mit I 〉 3σ(I), R = 0,052. Gitterabmessungen bei - 50°C: a = 1 703,8; b = 1 722,9; c = 5 123 pm; β = 94,65°.Die beiden miteinander isotypen Strukturen enthalten sechs symmetrieunabhängige PPh4+-Ionen und zwei symmetrieunabhängige Anionen [M2Te12]4-. In diesen sind die Metallatome zweier (MTe4)--Fünfringfragmente über eine Te42--Kette miteinander verknüpft.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190206
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  • 6
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    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.
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    URL: http://dx.doi.org/10.1002/zaac.19936190423
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  • 7
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    Phosphaniminato-Komplexe des Schwefels. Synthese und Kristallstrukturen von [SO(Cl)(NPPh3)], [SO2(Cl)(NPPh3)] und [SCl(NPPh3)2]ClProfessor Egon Uhlig zum 65. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1986-1991 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes of Sulfur ; Syntheses ; IR Spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorane Iminato Complexes of Sulfur. Synthesis and Crystal Structures of [SO(Cl)(NPPh3)], [SO2(Cl)(NPPh3)], and [SCl(NPPh3)2]ClThe title compounds have been prepared by the reaction of Me3SiNPPh3 with SOCl2, SO2Cl2, and SCl2, respectively. They form colourless, moisture sensitive crystals, which were characterized by IR spectroscopy and by crystal structure determinations.[SO(Cl)(NPPh3)]: Space group P21/n, Z = 4, structure determination with 2 434 observed unique reflections, R = 0.047. Lattice dimensions at 19°C: a = 1 304.8, b = 996.5, c = 1 339.5 pm, β = 93.75°. The compound forms monomeric molecules with a remarkably long S—Cl bond of 234.2 pm and distances SN and PN of 154.6 and 161.6 pm, respectively, which agree with double bonds.[SO2(Cl)(NPPh3)]: Space group P21/n, Z = 4, structure solution with 2 872 observed, unique reflections, R = 0.047. Lattice dimensions at 20°C: a = 956.9, b = 1 909, c = 1 002.0 pm, β = 106.06°. The compound forms monomeric molecules with distances S—Cl of 207.1 pm, SN of 154.5 pm, and PN of 161.6 pm.[SCl(NPPh3)2]Cl: Space group P21/c, Z = 4, structure solution with 5 224 observed, unique reflections, R = 0.042. Lattice dimensions at 20°C: a = 1 108.6, b = 1 603.8, c = 1 840.5 pm, β = 99.98°. The compound forms ions [SCl(NPPh3)2]+ and Cl-. In the cation the sulfur atom is ϕ-tetrahedrally coordinated with a long S—Cl distance of 248.5 pm and SN bond lengths of 154.5 and 156.0 pm.
    Notes: Die Titelverbindungen entstehen durch Umsetzung von Me3SiNPPh3 mit Thionylchlorid, Sulfurylchlorid bzw. Schwefeldichlorid als farblose, feuchtigkeitsempfindliche Kristalle, die wir durch die IR-Spektren und durch Kristallstrukturanalysen charakterisiert haben.[SO(Cl)(NPPh3)]: Raumgruppe P21/n, Z = 4, Strukturlösung mit 2 434 unabhängigen beobachteten Reflexen, R = 0,047. Gitterabmessungen bei 19°C: a = 1 304,8; b = 996,5; c = 1 339,5 pm, β = 93,75°. Die Verbindung bildet monomere Moleküle mit einer auffällig langen S—Cl-Bindung von 234,2 pm und Abständen SN und PN von 154,6 bzw. 161,6 pm, die Doppelbindungen entsprechen.[SO2(Cl)(NPPh3)]: Raumgruppe P21/n, Z = 4, Strukturlösung mit 2 872 unabhängigen beobachteten Reflexen, R = 0,047. Gitterabmessungen bei 20°C: a = 956,9; b = 1 909; c = 1 002,0 pm, β = 106,06°. Die Verbindung bildet monomere Moleküle mit Abständen S—Cl von 207,1 pm, SN von 154,5 pm und PN von 161,6 pm.[SCl(NPPh3)2]Cl: Raumgruppe P21/c, Z = 4, Strukturlösung mit 5 224 unabhängigen beobachteten Reflexen, R = 0,042. Gitterabmessungen bei 20°C: a = 1 108,6; b = 1 603,8; c = 1 840,5 pm, β = 99,98°. Die Verbindung bildet Ionen [SCl(NPPh3)2]+ und Cl-. Im Kation ist das Schwefelatom ϕ-tetraedrisch koordiniert mit einem langen S—Cl-Abstand von 248,5 pm und SN-Bindungslängen von 154,5 und 156,0 pm.
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    URL: http://dx.doi.org/10.1002/zaac.19946201125
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  • 8
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    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 
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    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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  • 9
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    The Transition Metal-Nitrogen Multiple BondDedicated to Professor Josef Goubeau on the occasion of his 80th birthday (1981)
    Weinheim : Wiley-Blackwell
    Angewandte Chemie International Edition in English 20 (1981), S. 413-426 
    Details
    ISSN: 0570-0833
    Keywords: Multiple bonds ; Bond theory ; Nitrido ligand ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Numerous nitrido complexes of transition metals show very short metal-nitrogen bond lengths, suggesting M≡N-triple bonds. At present, compounds of this type are being intensively investigated. In particular the molybdenum complexes are considered as model substances for the study of at least an intermediate step of N2-assimilation. This article contains a review of the structure and bonding, as well as syntheses and reactions of these complexes.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/anie.198104133
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  • 10
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    [Sb(12-Krone-4)2(CH3CN)][SbCl6]3 und [Bi(12-Krone-4)2(CH3CN)][SbCl6]3, die ersten Trikationen von Antimon(III) und Bismut(III)Professor Hartmut Bärnighausen zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 271-276 
    Details
    ISSN: 0044-2313
    Keywords: Crown ether complexes of Sb3+ and Bi3+ ; synthesis ; IR spectra ; 121Sb Mössbauer spectrum ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Sb(12-Crown-4)2(CH3CN)][SbCl6]3 and [Bi(12-Crown-4)2(CH3CN)][SbCl6]3, first Trications of Antimony(III) and Bismuth(III)The crown ether complexes [M(12-crown-4)2(CH3CN)][SbCl6]3 with M = Sb and Bi are formed by the reaction of antimony trichloride and bismuth trichloride, respectively, with antimony pentachloride in acetonitrile solution in the presence of 12-crown-4. They form colourless, moisture sensitive crystals, which were characterized by X-ray structure determinations and by IR spectroscopy. The complex with M = Sb was also characterized by 121Sb Mössbauer spectroscopy.Both complexes crystallize isotypically in the orthorhombic space group Pbcn with four formula units per unit cell.M = Sb: 3 483 observed unique reflections, R = 0.038. M = Bi: 2 958 observed unique reflections, R = 0.036. The compounds consist of SbCl6- ions and trications [M(12-crown-4)2(CH3CN)]3+, in which the M3+ ions are ninefold coordinated by the eight oxygen atoms of the crown ether molecules and by the nitrogen atom of the acetonitrile molecule. The lone pair of the M3+ ions has no steric effect.
    Notes: Die Kronenetherkomplexe [M(12-Krone-4)2(CH3CN)][SbCl6]3 mit M = Sb und Bi entstehen durch Reaktion von Antimontrichlorid bzw. Bismuttrichlorid mit Antimonpentachlorid in Acetonitrillösung in Gegenwart von 12-Krone-4. Sie bilden farblose, feuchtigkeitsempfindliche Kristalle, die wir durch kristallographische Strukturanalysen und durch die IR-Spektren charakterisiert haben. Von dem Komplex mit M = Sb wurde ein 121Sb-Mößbauer-Spektrum aufgenommen.Beide Komplexe kristallisieren isotyp in der orthorhombischen Raumgruppe Pbcn mit vier Formeleinheiten pro Elementarzelle. M = Sb: 3 483 beobachtete unabhängige Reflexe, R = 0,038. M = Bi: 2 958 beobachtete unabhängige Reflexe, R = 0,036. Die Verbindungen enthalten neben den SbCl6--Ionen Trikationen [M(12-Krone-4)2(CH3CN)]3+, in denen die M3+-Ionen durch die acht O-Atome der beiden Kronenethermoleküle und durch das N-Atom des Acetonitrilmoleküls neunfach koordiniert sind. Das freie Elektronenpaar an den M3+-Ionen bleibt ohne sterische Wirksamkeit.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190208
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