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  • 1
    ISSN: 0044-2313
    Keywords: Li(THF)2[η2-(tBu2P)2P] ; Li(TMEDA)[η2-(tBu2P)2P] ; Li(THF)2[η2-(iPr2P)2P] ; Li(THF)2[η2-(Et2N)2P—P—PtBu2] ; Li(THF)2[η2-(tBu2P—P—PiPr2)] ; (tBu2P)2P—SiMe3 ; crystal structures ; 1H, 31P, 7Li-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation and Structure of Li(THF)2[η2-(tBu2P)2P], Li(TMEDA)[η2-(tBu2P)2P], Li(THF)2[η2-(iPr2P)2P], Li(THF)2[η2-(Et2N)2P—P—PtBu2], Li(THF)2[η2-(tBu2P—P—PiPr2] and (tBu2P)2P—SiMe3The formation and crystal structures of the compounds (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA)[η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 and Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 are reported. Compounds 3-6 are formed by reacting the corresponding silylated triphosphanes with nBuLi: 2 and 3 result from (tBu2P)2P—SiMe3 1, 4 from (iPrP)2P—SiMe3, 5 from (Et2N)2P—P(SiMe3)—PtBu2 and 6 from tBu2P—P(SiMe3)—PiPr2. 1 crystallizes in the orthorhombic space group P212121 (no. 19) with a = 910.87(7) pm, b = 1132.5(1) pm, c = 2373.5(2) pm (determined at 90 K). The structure determination of 2 was performed at 293 K and 200 K, respectively. 2 crystallizes in the monoclinic space group P21/n (no. 14) with a = 1069.7(3) pm, b = 1802.5(3) pm, c = 1604.0(7) pm, β = 98.11(2)° (200 K); 3 also in P21/n (no. 14) with a = 904.3(2) pm, b = 1936.4(5) pm, c = 1653.2(3) pm, β = 94.52(1)° (200 K). 4 crystallizes monoclinically in C2/c (no. 15) with a = 1650.0(5) pm, b = 945.6(3) pm, c = 1779.8(5) pm, β = 108.81(2)° (200 K); 5 in P21/n (no. 14) with a = 939.4(5) pm, b = 1736.8(6) pm, c = 1943.3(7) pm, β = 98.17(4)° (200 K). All compounds contain Z = 4 molecules in the unit cell.The 1H, 31P and 7Li NMR spectra of 2-6 are discussed.
    Notes: Es wird über die Verbindungen (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA) · [η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 und Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 berichtet. Letztere bilden sich durch Umsetzung der entsprechenden silylierten Triphosphane mit nBuLi: 2 und 3 aus (tBu2P)2P—SiMe3 1, 4 aus (iPr2P)2P—SiMe3, 5 aus (Et2N)2—P · (SiMe3)—PtBu2, 6 aus tBu2P—P(SiMe3)—PiPr2.1 kristallisiert orthorhombisch in P212121 (Nr. 19) mit a = 910,87(7) pm, b = 1132,5(1) pm, c = 2373,5(2) pm (bei 90 K bestimmt). Die Strukturbestimmung von 2 erfolgte bei 293 K und 200 K. 2 kristallisiert monoklin in P21/n (Nr. 14) mit a = 1069,7(3) pm, b = 1802,5(3) pm, c = 1604,0(7) pm, β = 98,11(2)° (200 K), 3 ebenfalls in P21/n (Nr. 14) mit a = 904,3(2) pm, b = 1936,4(5) pm, c = 1653,2(3) pm, β = 94,52(1)° (200 K). 4 kristallisiert monoklin in C2/c (Nr. 15) mit a = 1650,0(5) pm, b = 945,6(3) pm, c = 1779,8(5) pm, β = 108,81(2)° (200K), 5 in P21/n (Nr. 14) mit a = 939,4(5) pm, b = 1736,8(6) pm, c = 1943,3(7) pm, β = 98,17(4)° (200 K). Alle fünf Verbindungen enthalten jeweils vier Formeleinheiten in der Elementarzelle.Es wird über die Untersuchung der 1H-, 31P- und 7Li-NMR-Spektren der Verbindungen 2-6 berichtet.
    Additional Material: 5 Ill.
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  • 2
    ISSN: 0044-2313
    Keywords: Asymmetric [As3]7- anion ; Zintl phase ; defect Ca14AlSb11 structure ; tetraarsaniobate(V) anion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sr13□NbAs11 und Eu13□NbAs11, Defektvarianten der Ca14AlSb11-Struktur mit asymmetrischen [As3]7--AnionenDie neuen Verbindungen Sr13NbAs11 und Eu13NbAs11 wurden aus den Elementen Sr, Nb und As sowie den binären Komponenten SrAs und Eu5As4 synthetisiert (Niobampullen; 1173 - 1273 K). Die tetragonalen tI 200-Phasen sind Defektvarianten der Ca14AlSb11-Struktur (Raumgruppe I41/acd (Nr. 142); Sr13□NbAs11: a = 1649.8(2) und c = 2214.1(3); Eu13□NbAs11: a = 1632.9(8) und c = 2197.3(8) pm; Z = 8). Die Strukturen sind aufgebaut aus den Kationen Sr2+ und Eu2+, den Anionen [NbAs4]7- und As3- sowie dem linearen Polyanion [As3]7-. Das Polyanion (isoster mit I3-) ist asymmetrisch mit den Bindungslängen d(As—As) = 273.0 und 346.0 pm (Sr) bzw. d(As—As) = 274.7 und 335.6 pm (Eu). Die Bindungslängen in den tetraedrischen Anionen betragen d(Nb—As) = 250.8 bzw. 251.1 pm. Die gesamte strukturelle Anordnung entspricht derjenigen von Cu2O durch die Ausbildung zweier sich durchdringender Netzwerke. Dabei werden die O-Atome durch As4-Tetraeder ersetzt (zentriert durch Nb) und die Cu-Atome durch As6-Oktaeder (zentriert durch Sr bzw. Eu). Die zentralen As-Atome der Polyanionen verbinden die Netze miteinander. Beide As-Netze werden von den restlichen Kationen eingehüllt, welche Würfel, tetragonale Antiprismen und überkappte trigonale Prismen ausbilden.
    Notes: The novel compounds Sr13NbAs11 and Eu13NbAs11 have been synthesized from SrAs, Eu5As4, Sr, Nb and As in niobium ampoules at 1173-1273 K. The tetragonal tI 200 phases are defect variants of the Ca14AlSb11 structure (space group I41/acd (no. 142); Sr13□NbAs11: a = 1649.8(2) and c = 2214.1(3); Eu13□NbAs11: a = 1632.9(8) and c = 2197.3(8) pm; Z = 8). The structures are built from the cations Sr2+, and Eu2+, respectively, and from the anions [NbAs4]7-, As3-, and the linear polyanion [As3]7-. This polyanion (isosteric to I3-) is asymmetric with d(As—As) = 273.0 and 346.0 pm (Sr) and 274.7 and 335.6 pm (Eu), respectively. The bond lengths in the tetrahedral anions are d(Nb—As) = 250.8 and 251.1 pm. The complete structural arrangement is related to that of Cu2O by forming two interpenetrating networks. The oxygen atoms are substituted by niobium centered As4 tetrahedra, and the Cu atoms are substituted by As6 octahedra (centered by Sr, Eu). The central As atoms of the polyanions connect the nets. Both As networks are enveloped by the remaining cations forming cubes, tetragonal antiprisms and capped trigonal prisms.
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