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  • Crystal Structure  (22)
  • Nitrido ligand  (2)
  • 11
    Electronic Resource
    Electronic Resource
    Silanolato-Komplexe von Titan und Zirconium. Die Kristallstrukturen von Cp2TiCl(OSiPh3) und Cp2ZrCl(OSiPh3) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1719-1724 
    Details
    ISSN: 0044-2313
    Keywords: Silanolato Complexes of Titanium and Zirconium ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Silanolato Complexes of Titanium and Zirconium. The Crystal Structures of Cp2TiCl(OSiPh3) and Cp2ZrCl(OSiPh3)The title compounds have been prepared by the reaction of Cp2MCl2 (M = Ti, Zr) with triphenylsilanole in diethylether in the presence of piperidine. They form only sparingly moisture sensitive orange (Ti) or colourless (Zr) crystal needles, which were characterized by X-ray crystallography.Cp2TiCl(OSiPh3): Space group P21/n, Z = 4, structure solution with 3961 observed unique reflections, R = 0.057. Lattice dimensions at 20°C: a = 1029.6, b = 1719.3, c = 1388.9 pm, β = 100.69°. The compound forms monomeric molecules with bond lengths TiO of 184.2 pm, SiO of 161.5 pm, and a TiOSi bonding angle of 164.5°.Cp2ZrCl(OSiPh3): Space group P3, Z = 18, structure solution with 2799 observed unique reflections, R = 0.047. Lattice dimensions at -20°C: a = b = 3518, c = 1058.3 pm. The structure consists of three symmetry-independent monomeric molecules, which differ only slightly. The bond lengths are (in average): ZrO 196.4 pm, SiO 162.1 pm, the ZrOSi bond angle is 173.7°.
    Notes: Die Titelverbindungen werden aus Cp2MCl2 (M = Ti, Zr) und Triphenylsilanol in Diethylether in Gegenwart von Piperidin hergestellt. Sie bilden nur wenig feuchtigkeits-empfindliche orange (Ti) bzw. farblose Kristallnadeln (Zr), die wir kristallographisch charakterisiert haben.Cp2TiCl(OSiPh3): Raumgruppe P21/n, Z = 4, Strukturlösung mit 3961 unabhängigen, beobachteten Reflexen, R = 0,057. Gitterkonstanten bei -50°C: a = 1029,6; b = 1719,3; c = 1388,9 pm, β = 100,69°. Die Verbindung bildet monomere Moleküle mit Abständen TiO von 184,2 pm, SiO von 161,5 pm und einem TiOSi-Bindungswinkel von 164,5°.Cp2ZrCl(OSiPh3): Raumgruppe P3, Z = 18, Strukturlösung mit 2799 unabhängigen, beobachteten Reflexen, R = 0,047. Gitterkonstanten bei -20°C: a = b = 3518; c = 1058,3 pm. Die Struktur enthält drei symmetrieunabhängige monomere Moleküle, die sich nur wenig voneinander unterscheiden. Die Abstände ZrO betragen im Mittel 196,4 pm, SiO im Mittel 162,1 pm und die Bindungswinkel ZrOSi im Mittel 173,7°.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201010
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  • 12
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur des Nonaselenids [Sr(15-Krone-5)2]Se9 (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 416-420 
    Details
    ISSN: 0044-2313
    Keywords: Nonaselenide ; 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 Nonaselenide [Sr(15-crown-5)2]Se9The title compound was prepared by the reaction of excess selenium with strontium diselenide in DMF in the presence of 15-crown-5. [Sr(15-crown-5)2]Se9 forms black crystals, which are soluble in DMF. They were characterized by FIR spectroscopy and by an X-ray structure determination.Space group P21/n, Z = 4, 2 381 observed unique reflections, R = 0.073. Lattice dimensions at 19°C: a = 1 228.7, b = 1 893.4, c = 1 575.7 pm, β = 99.15°. The compound consists of [Sr(15-crown-5)2]2+ ions in which the strontium ion is coordinated by the oxygen atoms of the crown ether molecules in a sandwich-like fashion, and of Se92- ions with a chain structure, which has a topolocical resemblance with the bicyclic ion Se102-.
    Notes: Die Titelverbindung entsteht durch Einwirkung von überschüssigem Selen auf Strontiumdiselenid in Dimethylformamid (DMF) in Gegenwart von 15-Krone-5. [Sr(15-Krone-5)2]Se9 bildet schwarze, in DMF leicht lösliche Kristalle, die durch das FIR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert werden.Raumgruppe P21/n, Z = 4, 2 381 beobachtete unabhängige Reflexe, R = 0,073. Gitterabmessungen bei 19°C: a = 1 228,7; b = 1 893,4; c = 1 575,7 pm, β = 99,15°. Die Verbindung besteht aus [Sr(15-Krone-5)2]2+-Ionen, in denen das Strontiumion sandwichartig von den O-Atomen der beiden Kronenethermoleküle umgeben ist, und kettenförmigen Se92--Ionen, die topologische Verwandtschaft zu dem bicyclischen Se102--Ion aufweisen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190229
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  • 13
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    Electronic Resource
    Synthesen und Kristallstrukturen der Polytellurido-Komplexe [K(15-Krone-5)2]2[MTe7] mit M = Zn und Hg (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 500-506 
    Details
    ISSN: 0044-2313
    Keywords: Polytellurido Complexes of Zinc and Mercury ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of the Polyellurido Complexes [K(15-Crown-5)2]2[MTe7] with M = Zn and HgThe title compounds were obtained in the presence of 15-crown 5 from solutions of zinc and mercury acetate, respectively, in DMF by addition of a solution of K2Te3 in DMF at 0°C (M = Zn) and -50°C (M = Hg). They form black crystal needles with metallic luster. Their crystal structures were determined by X-ray diffraction. The structures of [K(15-crown-5)2]2ZnTe7 and [K(15-crown-5)2]2HgTe7 show two-dimensional disorder as evidence by diffuse scattering. The averaged structures that were determined with the Bragg reflexions correspond to space group Pbcn and have very similar lattice parameters. Nevertheless, the structures differ. [HgTe7]2- ions consist of two condensed five membered rings. They are arranged to form strands in the c direction; within of one strand the ions have a definite orientation, but in different strands two different orientations occur randomly. A [ZnTe7]2- ion can be thought of consisting of a Zn2+ ion, a Te42- ion bonded in a chelate manner and a Te32- ion bonded with one terminal Te atom to the Zn2+. The [ZnTe7]2- ions are associated to strands in the c direction with two different strand orientations occuring randomly.
    Notes: Die Titelverbindungen entstehen aus Lösungen der Acetate von Zink bzw. Quecksilber in DMF bei Anwesenheit von 15-Krone-5 nach Zugabe einer Lösung von K2Te3 in DMF bei 0°C (M = Zn) bzw. -50°C (M = Hg). Die Verbindungen bilden schwarze, metallisch glänzende Kristallnadeln, die wir durch röntgenographische Strukturanalysen charakterisiert haben. Die Kristallstrukturen von [K(15-Krone-5)2]2[ZnTe7] und [K(15-Krone-5)2]2[HgTe7] sind zweidimensional fehlgeordnet, wie die entsprechende diffuse Streuung zeigt. Die Überlagerungsstrukturen, die mit Hilfe der Braggschen Reflexe bestimmt wurden, entsprechen bei beiden Verbindungen der Raumgruppe Pbcn bei sehr Ähnlichen Gitterparametern. Trotzdem unterscheiden sich die Strukturen. Die [HgTe7]2--Ionen bestehen aus zwei kondensierten Fünferringen. Sie sind zu Strängen längs c angeordnet, wobei sie innerhalb eines Stranges eine definierte Orientierung haben, aber von Strang zu Strang eine von zwei entgegengesetzten Orientierungen statistisch vorkommt. Ein [ZnTe7]2--Ion kann man sich aufgebaut denken aus einem Zn2+-Ion, einem chelatartig gebundenen Te42--Ion und einem Te32--Ion, das über ein terminales Te-Atom an das Zn2+ gebunden ist. Die [ZnTe7]2--Ionen sind zu Strängen längs c assoziiert, wobei statistisch zwei Strangorientierungen vorkommen.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190311
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  • 14
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    Electronic Resource
    [Mo(NPPh3)4]2+ [MoNCl3(NPPh3)]2- · C7H8, ein Phosphaniminato-Komplex mit einem Dikation von Molybdän(VI) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 507-512 
    Details
    ISSN: 0044-2313
    Keywords: Phosphoraneiminato Complex of Molybdenum ; Synthesis ; IR Spectrum ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Mo(NPPh3)4]2+ [MoNCl3(NPPh3)]2- · C7H8, a Phosphoraneiminato Complex with a Dication of Molybdenum(VI).The title compound was prepared by the reaction of MoNCl3 with Me3SiNPPh3 in acetonitrile solution. Red single crystals separated upon addition of toluene. They were characterized by IR spectroscopy and by an X-ray structure determination. (Space group P1, Z = 2, 6918 observed unique reflections, R = 0.059. Lattice dimensions at 20°C: a = 1 181.4, b = 2 021.4, c =2 409.7pm; α = 65.87°, β = 101.09°, γ= 78.97°). In the dication [Mo(NPPh3)4]2+ the molybdenum atom is surrounded in a tetrahedral fashion by the four nitrogen atoms of the phosphorane iminato ligands. The MoN and PN bond lengths correspond well with double bonds. In the two anions [MoNCl3(NPPh3)]-, which occur in different conformations, the molybdenum atoms are fivefold coordinated by the terminal nitride ligand Mo≡N: in axial positions and by the three chlorine atoms and the nitrogen atom of the (NPPh3)- ligand in the equatorial positions.
    Notes: Die Titelverbindung entsteht in Form leuchtend roter Einkristalle bei der Einwirkung von Me3SiNPPh3 auf MoNCl3 in Acetonitrillösung nach Zugabe von Toluol. Sie wird durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P1, Z = 2, 6918 beobachtete unabhängige Reflexe, R = 5,9%. Gitterabmessungen bei 20°C: a = 1 181,4; b = 2 021,4; c = 2 409,7pm; α = 65,87°; β = 101,09°; γ= 78,97°. In dem Dikation [Mo(NPPh3)4]2+ ist das Molybdänatom tetraedrisch von den vier N-Atomen der Phosphaniminatoliganden umgeben mit MoN- und PN-Abständen, die Doppelbindungen entsprechen. Die beiden symmetrieunabhängigen Anionen [MoNCl3(NPPh3)]- besitzen verschiedene Konformationen. In ihnen sind die Molybdänatome fünffach von dem terminalen Nitridoliganden Mo≡N: in axialer Position und von den drei Chloratomen und dem N-Atom des Phosphaniminatoliganden Äquatorial koordiniert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190312
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  • 15
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der Nitridodiolato-Osmate(VI) PPh4[OsNCl2(O2C2H4)] und PPh4[OsNCl2(O2C2Me4)] · 2 THF (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 853-858 
    Details
    ISSN: 0044-2313
    Keywords: Nitrido Diolato Osmates(VI) ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Nitridodiolato Osmates(VI) PPh4[OsNCl2(O2C2H4)] and PPh4[OsNCl2(O2C2Me4)] · 2 THFThe title compounds were prepared by the reaction of PPh4[OsNCl4] with glycole and pinacole, respectively, in CH2Cl2 and THF, respectively, in the presence of triethylamine, forming orange-red single crystals. According to the crystal structure determinations the compounds have ionic structures. In the anions the nitrido ligand occupies the apical position of the distorted tetragonal pyramid, and the two chlorine atoms and the two oxygen atoms of the diolato ligands are in equatorial positions.PPh4[OsNCl2(O2C2H4)]: Space group P21/n, Z = 4, 3 331 observed unique reflections, R = 0.031. Lattice dimensions at 19°C: a = 1 750.3, b = 816.8, c = 1 816.5 pm, β = 95.16°.PPh4[OsNCl2(O2C2Me4)] · 2 THF: Space group P1, Z = 2, 5 238 observed unique reflections, R = 0.051. Lattice dimensions at -80°C: a = 898.9, b = 1 405.1, c = 1 518.6 pm, α = 93.66°, β = 92.89°, γ = 92.51°.
    Notes: Die Titelverbindungen entstehen als orangefarbene Einkristalle bei Reaktionen von PPh4[OsNCl4] mit Glykol bzw. mit Pinakol in Dichlormethan bzw. in Tetrahydrofuran in Gegenwart von Triethylamin. Nach den Ergebnissen der Kristallstrukturanalysen haben die Verbindungen ionischen Aufbau. In den Anionen sind die Osmiumatome verzerrt tetragonal von dem Nitridoliganden in der Apicalposition und von zwei Chloratomen und von den zwei Sauerstoffatomen der chelatisierenden Diolatoliganden in den Äquatorialpositionen umgeben.PPh4[OsNCl2(O2C2H4)]: Raumgruppe P21/n, Z = 4, 3 331 beobachtete unabhängige Reflexe, R = 3,1%. Gitterkonstanten bei 19°C: a = 1 750,3; b = 816,8; c = 1 816,5 pm; β = 95,16°.PPh4[OsNCl2(O2C2Me4)] · 2 THF: Raumgruppe P1, Z = 2, 5 238 beobachtete unabhängige Reflexe, R = 5,1%. Gitterkonstanten bei -80°C: a = 898,9; b = 1 405,1; c = 1 518,6 pm; α = 93,66°; β = 92,89°; γ = 92,51°.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190508
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  • 16
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    Electronic Resource
    [W(NPPh3)4]Cl2  -  Ein Phosphaniminato-Komplex mit einem Wolfram-DikationProfessor Heinrich Nöth zum 65. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 999-1003 
    Details
    ISSN: 0044-2313
    Keywords: Phosphoraneiminato 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: [W(NPPh3)4]Cl2  -  a Phosphoraneiminato Complex with a Dication of TungstenThe title compound has been prepared by the reaction of Me3SiNPPh3 with WNCl3 and WO2Cl2, respectively, in acetonitrile, forming colourless crystals, which were characterized by IR spectroscopy and by an X-ray structure determination. Space group P21/n, Z = 4, 4 424 observed unique reflections, R = 0.045. Lattice dimensions at 20°C: a = 1 206.5(2), b = 2 225.3(2), c = 2 421.0(3) pm, β = 101.09(1)°. In the dication [W(NPPh3)4]2+ the tungsten atom is surrounded in a tetrahedral fashion by the four nitrogen atoms of the phosphoraneiminato ligands. The bond lengths WN and PN correspond with double bonds.
    Notes: Die Titelverbindung entsteht durch Reaktion von Me3SiNPPh3 mit WNCl3 bzw. mit WO2Cl2 in Acetonitril in Form farbloser Kristalle, die wir durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert haben. [W(NPPh3)4]Cl2 kristallisiert monoklin in der Raumgruppe P21/n mit Z = 4 (4 424 beobachtete unabhängige Reflexe, R = 4,5%). Gitterabmessungen bei 20°C: a = 1 206,5(2); b = 2 225,3(2); c = 2 421,0(3) pm; β = 101,09(1)°. In dem Dikation [W(NPPh3)4]2+ ist das Wolframatom tetraedrisch von den vier N-Atomen der Phosphaniminatoliganden umgeben mit WN- und PN-Abständen, die Doppelbindungen entsprechen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190607
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  • 17
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    Electronic Resource
    Die Kristallstrukturen der Polyselenide [Cs(18-Krone-6)]2Se5 · DMF, [Rb(222-Crypt)]2Se6, [Ba(15-Krone-5)2]Se6 · DMF und [Na(12-Krone-4)2]2Se7Professor Dietrich Mootz zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1247-1256 
    Details
    ISSN: 0044-2313
    Keywords: Polyselenides ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of the Polyselenides [Cs(18-Crown-6)]2Se5 · DMF, [Rb(222-Crypt)]2Se6, [Ba(15-Crown-5)2]Se6 · DMF, and [Na(12-Crown-4)2]Se7.The title compounds have been prepared by reactions of the corresponding diselenides with excess selenium in the presence of crown ethers in dimethylformamide solutions, forming black crystals.[Cs(18-Crown-6)]2Se5 · DMF: Space group P21/m, Z = 2, 2 194 observed unique reflections, R = 0.119. Lattice dimensions at 20°C: a = 1 041.2; b = 1 496.3; c = 1 459.7 pm; β = 100.39°. The compound forms an ionic triple with Cs…Se-contacts between 374 and 381 pm.[Rb(222-Crypt)]2Se6: Space group P1, Z = 2, 7 405 observed unique reflections, R = 0.056. Lattice dimensions at - 70°C: a = 1 106.8; b = 1 460.8; c = 1 718.8 pm; α = 89.22°; β = 86.65°; γ = 71.53°. The compound contains Se62- chains without direct contact with each other.[Ba(15-Crown-5)2]Se6 · DMF: Space group P21/n, Z = 4, 2 680 observed unique reflections, R = 0.055. Lattice dimensions at - 80°C: a = 1 051.9; b = 1 322.4; c = 2 729.9 pm; β = 100.93°. The compound contains Se62- chains, which are isolated from each other by the cations and the included DMF molecules.[Na(12-Crown-4)2]2Se7: Space group P1, Z = 2, 7 313 observed unique reflections, R = 0.042. Lattice dimensions at - 70°C: a = 1 260.9; b = 1 433.6; c = 1 462.9 pm; α = 80.27°; β = 78.60°; γ = 69.34°. The compound contains Se72- chains without direct contacts with each other.
    Notes: Die Titelverbindungen entstehen aus den entsprechenden Diseleniden mit überschüssigem Selen in Gegenwart von Kronenethern in Dimethylformamid-Lösungen in Form schwarzer Kristalle.[Cs(18-Krone-6)]2Se5 · DMF: Raumgruppe P21/m, Z = 2, 2 194 beobachtete unabhängige Reflexe, R = 0,119. Gitterabmessungen bei 20°C: a = 1 041,2; b = 1 496,3; c = 1 459,7 pm; β = 100,39°. Die Verbindung bildet ein Ionentripel mit Cs…Se-Kontakten zu dem kettenförmigen Se52--Ion von 374 bis 381 pm.[Rb(222-Crypt)]2Se6: Raumgruppe P1, Z = 2, 7 405 beobachtete unabhängige Reflexe, R = 0,056. Gitterabmessungen bei - 70°C: a = 1 106,8; b = 1 460,8; c = 1 718,8 pm; α = 89,22°; β = 86,65°; γ = 71,53°. Die Verbindung enthält kettenförmige Se62--Ionen, die keine Kontakte untereinander ausbilden.[Ba(15-Krone-5)2]Se6 … DMF: Raumgruppe P21/n, Z = 4, 2 680 beobachtete unabhängige Reflexe, R = 0,055. Gitterabmessungen bei - 80°C: a = 1 051,9; b = 1 322,4; c = 2 729,9 pm; β = 100,93°. Die Verbindung enthält kettenförmige Se62--Ionen, die im Gitter durch die Kationen und die eingelagerten DMF-Moleküle voneinander isoliert sind.[Na(12-Krone-4)2]2Se7: Raumgruppe P1, Z = 2, 7 313 beobachtete unabhängige Reflexe, R = 0,042. Gitterabmessungen bei - 70°C: a = 1 260,9; b = 1 433,6; c = 1 462,9 pm; α = 80,27°; β = 78,60°; γ = 69,34°. Die Verbindung enthält kettenförmige Se72--Ionen, die keine direkten Kontakte untereinander ausbilden.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190717
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  • 18
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    Electronic Resource
    Phosphaniminato-Komplexe des Iods. Synthese und Kristallstrukturen von Ph3PNIO2 und Ph3PNSiMe3 · I2Professor Wolfgang Sawodny zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 329-333 
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    ISSN: 0044-2313
    Keywords: Phosphoraneiminato Complexes of Iodine ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphoraneiminato Complexes of Iodine. Syntheses and Crystal Structures of Ph3PNIO2 and Ph3PNSiMe3 · I2Ph3PNIO2 has been prepared as yellow crystals by the reaction of Ph3PNSiMe3 with I2O5 in boiling acetonitrile, whereas the molecular complex Ph3PNSiMe3 · I2 is formed as brown crystals by the reaction of Ph3PNSiMe3 with iodine in acetonitrile solution. Both complexes were characterized by crystal structure determinations.Ph3PNIO2: Space group P21/n, Z = 4, 2 858 observed unique reflections, R = 0.039. Lattice dimensions at 19°C: a = 972.8(2), b = 1 743.4(3), c = 1 073.7(2) pm, β = 115.46(3)°. The compound forms monomeric molecules with pyramidal geometry at the iodine atom. The bond angle PNI (126.9°) is unusually small; the PN bond length of 159.2 pm corresponds with a double bond.Ph3PNSiMe3 · I2: Space group P1, Z = 2, 3 560 observed unique reflections, R = 0.033. Lattice dimensions at 19°C: a = 941.2(2), b = 1 041.7(2), c = 1 287.4(3) pm, α = 78.34(1)°, β = 72.00(2)°, γ = 86.08(2)°. The compound forms monomeric molecules, in which the I2 molecule and the nitrogen atom of the phosphoraneimine molecule realize a linear N—I—I axis with a bond length N—I of 243.2 pm.
    Notes: Ph3PNIO2 entsteht als gelbe Kristalle durch Reaktion von Ph3PNSiMe3 und I2O5 in siedendem Acetonitril, während der Molekülkomplex Ph3PNSiMe3 · I2 aus Ph3PNSiMe3 und Iod bei Raumtemperatur in Acetonitril in Form brauner Kristallnadeln gebildet wird. Beide Komplexe haben wir durch röntgenographische Strukturanalysen charakterisiert.Ph3PNIO2: Raumgruppe P21/n, Z = 4, 2858 beobachtete unabhängige Reflexe, R = 0,039. Gitterabmessungen bei 19°C: a = 972,8(2); b = 1 743,4(3); c = 1 073,7(2) pm, β = 115,46(3)°. Die Verbindung bildet monomere Moleküle mit pyramidaler Geometrie am Iodatom. Der Bindungswinkel PNI ist mit 126,9° ungewöhnlich klein; der Abstand PN entspricht mit 159,2 pm einer Doppelbindung.Ph3PNSiMe3 · I2: Raumgruppe P1, Z = 2, 3 560 beobachtete unabhängige Reflexe, R = 0,033. Gitterabmessungen bei 19°C: a = 941,2(2); b = 1 041,7(2); c = 1 287,4(3) pm; α = 78,34(1)°; β = 72,00(2)°; γ = 86,08(2)°. Die Verbindung bildet monomere Moleküle, in denen das I2-Molekül mit dem N-Atom des Phosphanimins eine lineare N—I—I-Achse mit einem N—I-Abstand von 243,2 pm realisiert.
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    URL: http://dx.doi.org/10.1002/zaac.19946200221
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  • 19
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    Electronic Resource
    [Yb3OBr4{N(SiMe3)2}3 (THF)3], ein Amido-Komplex des Ytterbiums mit clusterähnlichem Aufbau (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1203-1204 
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    ISSN: 0044-2313
    Keywords: Ytterbium Complex ; Amido Compound ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [Yb3OBr4{N(SiMe3)2}3(THF)3], an Amido Complex of Ytterbium with a Clusterlike StructureThe title compound has been prepared from YbBr3 and NaN(SiMe3)2 in THF suspension, forming yellow single crystals from hexane solutions which were characterized by a crystal structure determination. Space group P1, Z = 2, lattice dimensions at -100°C: a = 1085.4(1), b = 1410.2(1), c = 1912.0(1) pm; α = 78.62(1)°, β = 80.61(1)°, γ = 73.45(1)°, R = 0.025.In the molecular structure of [Yb3OBr4{N(SiMe3)2}3(THF)3] the three ytterbium atoms together with the μ3-oxygen atom and a μ3-bromine atom form a distorted trigonal bipyramid. In addition, three μ2-Br atoms coordinate the Yb atoms in the equatorial plane, whereas the THF molecules and the N(SiMe3)2- ligands are terminally coordinated, thus forming a distorted octahedrally surrounding of the Yb atoms.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230803
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    Electronic Resource
    Electronic Resource
    [Li7(CHPMe2NSiMe3)3(OSiMe2nBu)]2, ein Gemischtligand-Li14-Cluster mit dem Carbdianion (CHPMe2NSiMe3)2- (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1306-1310 
    Details
    ISSN: 0044-2313
    Keywords: Lithium Cluster ; Carbdianion ; NMR spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Li7(CHPMe2NSiMe3)3(OSiMe2nBu)]2, a Mixed-Ligand-Li14 Cluster with the Carbdianion (CHPMe2NSiMe3)2-The title compound is formed as colourless moisture and oxygen sensitive crystals by the reaction of [LiCH2PMe2NSiMe3]4 with zinc or cobalt chloride in a toluene suspension in the presence of silicongrease (-OSiMe2-)n and n-butyllithium. It is characterized by multinucleus NMR spectroscopy and by crystal structure determinations of two different crystal individuals.1. Space group P1, Z = 1, lattice dimensions at -70 °C: a = 1272.0, b = 1392.6, c = 1417.6 pm, α = 115.33°, β = 96.75°, σ = 106.81°; R = 0.042.2. Space group P21/n, Z = 2, lattice dimensions at -50 °C: a = 1424.8, b = 1457.1, c = 1997.0 pm, β = 90.32, R = 0.069.
    Notes: Die Titelverbindung (farblose, feuchtigkeits- und sauerstoffempfindliche Kristalle) entsteht bei der Reaktion von [LiCH2PMe2NSiMe3]4 mit wasserfreiem Zink- oder Cobaltchlorid in einer Toluolsuspension in Gegenwart von Siliconfett (-OSiMe2-)n und n-Butyllithium. Sie wird durch Multikern-NMR-Spektroskopie und durch Kristallstrukturanalysen zweier kristallchemisch verschiedener Individuen charakterisiert.1. Raumgruppe P1, Z = 1, Gitterkonstanten bei -70 °C: a = 1272,0; b = 1392,6; c = 1417,6 pm; α = 115,33°; β = 96,75°; σ = 106,81°; R = 0,042.2. Raumgruppe P21/n, Z = 2, Gitterkonstanten bei -50 °C: a = 1424,8; b = 1457,1; c = 1997,0 pm; β = 90,32°; R = 0,069.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230822
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