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  • 1
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur des Selenyl-Phosphaniminato-Komplexes SeO(NPPh3)2 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1171-1174 
    Details
    ISSN: 0044-2313
    Keywords: Selenium ; Phosphorane Iminato Complex of Selenium ; 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 Selenyl-Phosphoraneiminato Complex SeO(NPPh3)2SeO(NPPh3)2 has been prepared from SeO2 and Me3SiNPPh3 in a SeO2 suspension in acetonitrile, forming colourless crystals. The compound is characterized by IR spectroscopy and by a crystal structure determination. Space group P1, Z = 2, structure solution with 5 344 observed unique reflections, R = 0.064. Lattice dimensions at -40°C: a = 931.6, b = 947.6, c = 1 762 pm, α = 77.50°, β = 81.78°, γ = 79.23°. The compound forms monomeric molecules in which the selenium atom is ϕ-tetrahedrally surrounded with bond lengths SeO = 161.7 pm and SeN = 179.9 and 181.6 pm.
    Notes: SeO(NPPh3)2 entsteht in Form farbloser Kristalle bei der Reaktion einer Suspension von SeO2 mit Me3SiNPPh3 in Acetonitril. Die Verbindung wird durch das IR-Spektrum und durch eine Kristallstrukturanalyse charakterisiert. Raumgruppe P1, Z = 2, Strukturlösung mit 5 344 beobachteten unabhängigen Reflexen, R = 0,064. Gitterkonstanten bei -40°C: a = 931,6; b = 947,6; c = 1 762 pm, α = 77,50°, β = 81,78°, γ = 79,23°. Die Verbindung bildet monomere Moleküle, in denen das Selenatom verzerrt ϕ-tetraedrisch umgeben ist mit Abständen SeO = 161,7 pm und SeN = 179,9 und 181,6 pm.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210709
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  • 2
    Electronic Resource
    Electronic Resource
    [(Me3PN)3SNS(NPMe3)2]Cl2, ein gemischtvalenter Phosphaniminato-Komplex des Schwefels (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 863-866 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complex of Sulfur ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [(Me3PN)3SNS(NPMe3)2]Cl2, a Mixed Valenced Phosphorane Iminato Complex of SulfurThe title compound has been prepared from trithiazyl chloride and the silylated phosphaneimine Me3SiNPMe3 in acetonitrile solution, forming red crystals, which were characterized by IR spectroscopy and by a crystal structure determination.Space group P21/c, Z = 4, structure solution with 4250 independent reflections, R = 0.054. Lattice dimensions at 20°C: a = 1077.8, b = 2036.6, c = 1480.5 pm, β = 102.39°. The compound consists of dications [(Me3PN)3SNS(NPMe3)2]2+ and chloride ions. In the cations the sulfur atoms of oxidation number +VI and +IV are connected by an asymmetric, bent nitrido bridge with SN bond lengths of 156.9 and 167.0 pm.
    Notes: Die Titelverbindung entsteht als rote Kristalle bei der Reaktion von Trithiazylchlorid mit dem silylierten Phosphanimin Me3SiNPMe3 in Acetonitrillösung. Die Verbindung wird durch das IR-Spektrum und durch eine Kristallstruktur-analyse charakterisiert.Raumgruppe P21/c, Z = 4, Strukturlösung mit 4250 unabhängigen Reflexen, R = 0,054. Gitterabmessungen bei 20°C: a = 1077,8; b = 2036,6; c = 1480,5 pm, β = 102,39°. Die Verbindung besteht aus den Dikationen [(Me3PN)3SNS(NPMe3)2]2+ und Chloridionen. In den Kationen sind die Schwefelatome der Oxidationszahl +VI und +IV über eine asymmetrische, gewinkelte Nitridobrücke mit SN-Abständen von 156,9 und 167,0 pm verknüpft.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220519
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  • 3
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur des ionischen Tellurnitridchlorids [Te3N2Cl5(SbCl5)]+SbCl6- (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1375-1379 
    Details
    ISSN: 0044-2313
    Keywords: Tellurium Nitride Chloride ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of the Ionic Tellurium Nitride Chloride[Te3N2Cl5(SbCl5)]+SbCl6-The title compound has been prepared by the reaction of Te2NCl5 with antimony pentachloride in CH2Cl2 suspension. It is characterized by IR spectroscopy and by a crystal structure determination. Space group P21/c, Z = 4, lattice dimensions at -70°C: a = 1535.6, b = 1259.5, c = 1572.4 pm, β = 109.30°, R = 0.031. The compound forms an ionic pair with the central group of a (TeNCl)2 molecule in which the tellurium atoms are linked by the nitrogen atoms to give a planar Te2N2 four-membered ring. One of the nitrogen atoms is coordinated by a TeCl3+ unit, the other one by an antimony pentachloride molecule. According to the IR spectra a structure like [Te2N2Cl2(TeCl4)2] is proposed for Te2NCl5.
    Notes: Die Titelverbindung wird durch Reaktion von Te2NCl5 mit Antimonpentachlorid in Dichlormethan hergestellt und durch das IR-Spektrum und eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, Gitterkonstanten bei -70°C: a = 1535,6; b = 1259,5; c = 1572,4 pm, β = 109,30°; R = 0,031. Die Verbindung bildet ein Ionenpaar, dessen Kation als zentrales Bauelement ein (TeNCl)2-Molekül enthält, in dem die Telluratome mit den Stickstoffatomen zu einem planaren Te2N2-Vierring verknüpft sind. Eines der N-Atome ist mit einem TeCl3+-Ion, das andere mit einem SbCl5-Molekül koordiniert. Aus dem Vergleich der IR-Spektren wird für Te2NCl5 eine Struktur gemäß [Te2N2Cl2(TeCl4)2] vorgeschlagen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230909
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  • 4
    Electronic Resource
    Electronic Resource
    Funktionalisierte Alkinkomplexe von Wolfram(VI). Synthese und Kristallstrukturen von [WCl4(Et—Se—C≡C—Se—Et)(THF)] und [WCl4(Et—Te—C≡C—Te—Et)(THF)]Professor Gerhard Fritz zum 75. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 388-392 
    Details
    ISSN: 0044-2313
    Keywords: Functionalized Alkyne Complexes of Tungsten ; Synthesis ; IR spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Functionalized Alkyne Complexes of Tungsten(VI). Syntheses and Crystal Structures of [WCl4(Et—Se—C≡C—Se—Et)(THF)] and [WCl4(Et—Te—C≡C—Te—Et)(THF)]The title compounds have been prepared by reactions of [WCl4(SEt2)2] with the alkynes Et—X—C≡C—X—Et (X = Se, Te) in CCl4 solution and subsequent addition of tetrahydrofurane. Both complexes were characterized by crystal structure determinations.[WCl4(Et—Se—C≡C—Se—Et)(THF)]: Space group P21/n, Z = 4, structure determination with 2942 unique reflections, R = 0.038. Lattice dimensions at 20°C: a = 934.2, b = 1639.5, c = 1189.5 pm, β = 96.497°.[WCl4(Et—Te—C≡C—Te—Et)(THF)]: Space group P21/n, Z = 4, structure determination with 4097 unique reflections, R = 0.067, Lattice dimensions at -70°C: a = 899.2, b = 1691.9, c = 1213.3 pm, β = 96.82°.The complexes have monomeric molecular structures with the oxygen atom of the THF molecules in trans-position to the side-on bound alkyne ligands.
    Notes: Die Titelverbindungen werden aus [WCl4(SEt2)2] und den Alkinen Et—X—C≡C—X—Et (X = Se, Te) in CCl4-Lösung nach Zusatz von Tetrahydrofuran erhalten und durch Kristallstrukturanalysen charakterisiert.[WCl4(Et—Se—C≡C—Se—Et)(THF)]: Raumgruppe P21/n, Z = 4, Strukturverfeinerung mit 2942 unabhängigen Reflexen, R = 0,038. Gitterabmessungen bei 20°C: a = 934,2; b = 1639,5; c = 1189,5 pm, β = 96,497°.[WCl4(Et—Te—C≡C—Te—Et)(THF)]: Raumgruppe P21/n, Z = 4, Strukturverfeinerung mit 4097 unabhängigen Reflexen, R = 0,067. Gitterabmessungen bei -70°C: a = 899,2; b = 1691,9; c = 1213,3 pm, β = 96,82°.Beide Verbindungen haben monomere Molekülstrukturen, in denen sich das O-Atom des THF-Moleküls in trans-Position zum seitlich gebundenen Alkinliganden befindet.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210308
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  • 5
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der Wolfram(VI)-Alkin-Komplexe [W2(O)(OMe)6(Et—Se—C≡C—Se—Et)2] und Li[W(OMe)5(Et—Te—C≡C—Te—Et)]Professor Karl-Heinz Thiele zum 65. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 393-399 
    Details
    ISSN: 0044-2313
    Keywords: Alkoxy-Alkyne Complexes of Tungsten ; Synthesis ; 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 Tungsten(VI)-alkyne Complexes [W2(O)(OMe)6(Et—Se—C≡C—Se—Et)2] and Li[W(OMe)5(Et—Te—C≡C—Te—Et)]The title compounds have been prepared by reactions of lithium methanolate with [WCl4(Et—Se—C≡C—Se—Et)(THF)] and [WCl4(Et—Te—C≡C—Te—Et)(THF)], respectively, in diethylether suspensions. Both complexes were characterized by crystal structure determinations.[W2(O)(OMe)6(Et—Se—C≡C—Se—Et)2]: Space group P1, Z = 2, structure determination with 4 320 observed unique reflections, R = 0.041. Lattice dimensions at -70°C: a = 949.3, b = 1 225.3, c = 1 285.0 pm, α = 82.48°; γ = 82.44°; β = 81.44°. The tungsten atoms are bridged by three μ2-O-atoms of the OMe groups; the alkyne ligands are coordinated side-on in a metallacyclopropene-like fashion.Li[W(OMe)5(Et—Te—C≡C—Te—Et)]: Space group P1, Z = 2, structure determination with 9 381 observed unique reflections, R = 0.038. Lattice dimensions at -70°C: a = 983.4, b = 1606.9, c = 1971.5 pm, α = 66.09°, β = 84.29°, γ = 79.83°. The lithium ions link the [W(OMe)5(Et—Te—C≡C—Te—Et)]- anions to a trimeric ion ensemble via the O atoms of three OMe groups of each anion.
    Notes: Die Titelverbindungen werden durch Reaktion von Lithiummethanolat mit [WCl4(Et—Se—C≡C—Se—Et)(THF)] bzw. mit [WCl4(Et—Te—C≡C—Te—Et)(THF)] in Diethylether hergestellt und durch Kristallstrukturanalysen charakterisiert.[W2(O)(OMe)6(Et—Se—C≡C—Se—Et)2]: Raumgruppe P1, Z = 2, Strukturlösung mit 4 320 beobachteten unabhängigen Reflexen, R = 0,041. Gitterabmessungen bei -70°C: a = 949,3; b = 1225,3; c = 1285,0 pm, α = 82,48°; β = 82,44°; γ = 81,44°. Die beiden Wolframatome sind über drei μ2-OMe-Brücken verknüpft; die Alkinliganden sind seitlich entsprechend von Metallacyclopropengruppen koordiniert.Li[W(OMe)5(Et—Te—C≡C—Te—Et)]: Raumgruppe P1, Z = 2, Strukturlösung mit 9 381 beobachteten unabhängigen Reflexen, R = 0,038. Gitterabmessungen bei -70°C: a = 983,4; b = 1606,9; c = 1971,5 pm, α = 66,09°; β = 84,29°; β = 79,83°. Die Lithiumionen verknüpfen die [W(OMe)5(Et—Te—C≡C—Te—Et)]--Anionen über die O-Atome dreier OMe-Gruppen zu einem trimeren Ionenensemble.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210309
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  • 6
    Electronic Resource
    Electronic Resource
    Kristallstrukturen von [TiF3(NPPh3)(HNPPh3)]2 und von HNPPh3Professor H.-G. von Schnering zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1091-1096 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato-Phosphaneimine Complex of Titanium ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of [TiF3(NPPh3)(HNPPh3)]2 and of HNPPh3The phosphoraneiminato-phosphaneimine complex [TiF3(NPPh3)(HNPPh3)]2 was obtained by the reaction of TiF4 with Me3SiNPPh3 in boiling dichloromethane. It crystallizes from 1,2-dichloroethane as yellow crystals which include four molecules C2H4Cl2 per dimeric formula unit. Space group P21/n, Z = 2, structure solution with 7270 independent reflections, R = 0.060 for reflections with I 〉 2σ(I). Lattice dimensions at -50°C: a = 1417.5, b = 1896.9, c = 1586.6 pm, β = 101.22°. The compound forms centrosymmetric dimeric molecules via μ2-F bridges with TiF distances of 194.6 and 223.3 pm, the longer one being in trans-position to the N atom of the (NPPh3)- ligand. Its TiN bond length of 177.7 pm corresponds with a double bond. The TiN bond length of the HNPPh3 donor molecule of 213.4 pm is typical for a donor acceptor bond.According to the crystal structure determination the phosphaneimine HNPPh3 forms monomeric molecules without intermolecular hydrogen bridges with a PN bond length of 152.4 pm. Space group P21/c, Z = 4, structure solution with 3229 independent reflections, R = 0.062 for reflections with I 〉 2σ(I). Lattice dimensions at -70°C: a = 1460.4, b = 928.9, c = 1096.6 pm, β = 93.35°.
    Notes: Der Phosphaniminato-Phosphanimin-Komplex [TiF3(NPPh3)(HNPPh3)]2 wird aus TiF4 und Me3SiNPPh3 in siedendem Dichlormethan erhalten. Er kristallisiert aus 1,2-Dichlorethan als gelbe Kristalle unter Einschluß von vier Molekülen C2H4Cl2 pro dimere Formeleinheit. Raumgruppe P21/n, Z = 2, Strukturlösung mit 7270 unabhängigen Reflexen, R = 0,060 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -50°C: a = 1417,5; b = 1896,9; c = 1586,6 pm; β = 101,22°. Die Verbindung bildet zentrosymmetrische Dimere, in denen die Titanatome über μ2-F-Brücken mit TiF-Abständen von 194,6 und 223,3 pm verknüpft sind. Die lange Ti—F-Bindung befindet sich in trans-Position zum N-Atom des (NPPh3)--Liganden, dessen TiN-Bindung mit 177,7 pm einer Doppelbindung entspricht. Der vom HNPPh3-Liganden ausgehende Ti—N-Abstand beträgt 213,4 pm.Das Phosphanimin HNPPh3 bildet nach der Kristallstrukturanalyse monomere Moleküle mit einer PN-Bindungslänge von 152,4 pm ohne intermolekulare Wasserstoffbrücken. Raumgruppe P21/c, Z = 4, Strukturlösung mit 3229 unabhängigen Reflexen, R = 0,062 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -70°C: a = 1460,4; b = 928,9; c = 1096,6 pm; β = 93,35°.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220626
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  • 7
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der silylierten Tris-Phosphanimine R—C(CH2PPh2NSiMe3)3 mit R = H und CH3Professor Rudolf Hoppe zum 75. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1739-1743 
    Details
    ISSN: 0044-2313
    Keywords: Silylated λ5-Phosphazenes ; Synthesis ; NMR spectra ; 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 Silylated λ5-Phosphazenes R—C(CH2PPh2NSiMe3)3 with R = H and CH3The title compounds are obtained by Staudinger reaction from the corresponding tripodal phosphanes R—C(CH2PPh2)3 and trimethylsilylazide. Both complexes are characterized by their IR and NMR spectra and by crystal structure analyses.H—C(CH2PPh2NSiMe3)3 (1): Space group P21/c, Z = 4, structure determination with 7833 independent reflections, R = 0.055. Lattice dimensions at -50°C: a = 1399.5, b = 2311.4, c = 1678.9 pm, β = 112.92°.CH3—C(CH2PPh2NSiMe3)3 (2): Space group P1, Z = 2, structure determination with 9251 independent reflections, R = 0.057. Lattice dimensions at -50°C: a = 1276.5, b = 1386.9, c = 1790.2 pm; α = 85.55°, β = 69.39°, γ = 62.99°.1 and 2 form monomeric molecules which are distinguished by their conformation.
    Notes: Die Titelverbindungen werden durch Staudinger-Reaktion aus den entsprechenden tripodalen Phosphanen R—C(CH2PPh2)3 und Trimethylsilylazid hergestellt und durch ihre IR- und NMR-Spektren sowie durch Kristallstrukturanalysen charakterisiert.H—C(CH2PPh2NSiMe3)3 (1): Raumgruppe P21/c, Z = 4, Strukturbestimmung mit 7833 unabhängigen Reflexen, R = 0,055. Gitterkonstanten bei -50°C: a = 1399,5; b = 2311,4; c = 1678,9 pm; β = 112,92°.CH3—C(CH2PPh2NSiMe3)3 (2): Raumgruppe P1, Z = 2, Strukturbestimmung mit 9251 unabhängigen Reflexen, R = 0,057. Gitterkonstanten bei -50°C: a = 1276,5; b = 1386,9; c = 1790,2 pm; α = 85,55°; β = 69,39°; γ = 62,99°.1 und 2 bilden monomere Moleküle, die sich durch ihre Konformation unterscheiden.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976231112
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