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  • 1H, 31P, 7Li-NMR spectra  (1)
  • Alkali metal germanides and stannides  (1)
  • Asymmetric [As3]7- anion  (1)
  • G44-, Sn44;  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Die inneren Schwingungen der Tetrahetero-Tetrahedran-Anionen Ge44, Sn44- und Pb44Herrn Professor Josef Grobe zum 60. Geburtstag am 2. November 1991 Gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 608 (1992), S. 131-134 
    Details
    ISSN: 0044-2313
    Keywords: Tetrahetero-tetrahedrane anions ; G44-, Sn44; ; infrared, Raman spectra; ; internal vibrations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Internal Vibration of the Tetrahetero-Tetrahedrane Anions Ge44-, Sn44-, and Pb44The Frequencies of the internal vibrations ν1 (A1), ν2(E), ν3(T2) of the tetrahetero-tetrahedrane an ions Ge44- and Sn44- are determined from the infrared and Raman spectra of K7LiGe8 and KSn, respectively. A comparison of the characteristic vibration of tetrahedrane anions X44- (X = Si, Ge, Sn)and the isoelectronic neutral tetrahedranes Y4 of the neighbouring elements (Y = P, As, Sb) shows a rather constant ratio of the corresponding frequencies k = v˜(X44-) = 0,77. This allows for an estimate of v˜(Pb44-) from the known Bi4data. In the inflated spectrum of KPb bands are observed in the predicted frequency range.
    Notes: Aus den Infrarot-und Raman-Spektren von K7LiGe8 und KSn werden die Frequenzen der inneren Schwingungen ν1(A1), ν2(E) und ν3(T3) der Tetrahetero-Tetrahedran -Anionen Ge44- und Sn44- bestimmt. Der Vergleich der charakteristischen Schwingungen von Tetrahedran-Anionen X44-(X = Si, Ge, Sn) und isoelektronischen neutralen Tetrahedranen Y4 der Nachbarelemente (Y = P,As, Sb)ergibt ein nahezu konstantes Verhältnis für die einander entsprechenden Frequenzen k = v˜(X44-)/v˜(Y4) = 0,77. Damit werden aus den Frequenzen v˜(Bi4) Werte für v˜(Pb44-) abgeschätzt, welche mit Banden im Infrarot-Spektrum von KPb übereinstimmen.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926080219
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  • 2
    Electronic Resource
    Electronic Resource
    Komplexchemie P-reicher Phosphane und Silylphosphane. XII. Bildung und Struktur von 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] und (tBu2P)2P—SiMe3Professor Kurt Dehnicke zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1564-1572 
    Details
    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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220920
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  • 3
    Electronic Resource
    Electronic Resource
    Binary alkali metal compounds with the zintl anions [Ge9]4- and [Sn9]4-Professor Welf Bronger zum 65. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1037-1039 
    Details
    ISSN: 0044-2313
    Keywords: Alkali metal germanides and stannides ; Zintl cluster anions ; Vibrational spectra ; Thermal decomposition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The binary germanides M12Ge17 and M4Ge9 (M = Na, K, Rb, Cs) and the stannides M12Sn17 and M4Sn9 (M = K, Rb, Cs) were identified by a combination of direct synthesis, thermogravimetric analysis, vibrational spectroscopy, X-ray powder data and single crystal structure analysis. The M12E17 phases contain the cluster anions [E9]4- and [E4]4- in the ratio 1:2, forming a hierarchical structure with the cluster anions at the atomic positions of the hexagonal Laves phase MgZn2. Like the M4E4 phases, the M4Ge9 compounds are hierarchical derivatives of the cubic Cr3Si structure but with [Ge9]4- anions. The thermogravimetric analyses give strong evidence for the existence of at least one more phase with [E9]4- and [E4]4- clusters and of the clathrate phases M6E136 in addition to the well-known M8E44□2 chlathrates.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230704
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  • 4
    Electronic Resource
    Electronic Resource
    Sr13□NbAs11 and Eu13□NbAs11 - Defect Variants of the Ca14AlSb11 Structure with asymmetric [As3]7- anionsDedicated to Professor John D. Corbett on the Occasion of his 70th Birthday (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 518-524 
    Details
    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.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220322
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