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  • crystal structure  (10)
  • IR Spectra  (5)
  • syntheses  (5)
  • 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
    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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  • 3
    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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  • 4
    Electronic Resource
    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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915930110
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  • 5
    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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  • 6
    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.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926110525
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  • 7
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    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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  • 8
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    Electronic Resource
    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.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201125
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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.
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    URL: http://dx.doi.org/10.1002/anie.198104133
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    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.
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    URL: http://dx.doi.org/10.1002/zaac.19926130108
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