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  • 1
    ISSN: 0044-2313
    Keywords: K2Fe[P2S6] ; Hexathiodiphosphate(IV) ; Hexathiohypodiphosphate ; Crystal Structure ; Magnetism ; Vibrational Spectrum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese, Kristallstruktur, Magnetismus und Schwingungsspektrum von Dikaliumeisen(II)hexathiodiphosphat(IV), K2Fe[P2S6]K2Fe[P2S6] wurde aus den Elementen bei 1173 K in evakuierten, abgeschmolzenen Quarzampullen dargestellt. Die Verbindung bildet transparente, orangefarbene, luft- und feuchtigkeitsbeständige Kristalle. K2Fe[P2S6] kristallisiert monoklin, Raumgruppe P21/n (Nr. 14), mit den Gitterkonstanten (T = 298,5 K): a = 6,0622(4), b = 12,172(1) und c = 7,3787(8) Å, β = 101,113(7)°, Z = 2. Der neuartige Strukturtyp (mP22) wird durch Säulen von alternierend flächenverknüpften S6-Oktaedern und trigonalen Antiprismen (beide verzerrt) charakterisiert, die parallel zur a-Achse verlaufen und durch K+-Kationen (KZ 10; {2,6,2}-Polyeder; d(K—S) = 3,231 - 3,845 Å) miteinander verbunden sind. Die S6-Polyeder der Säulen werden alternierend durch Fe (d̄(Fe—S) = 2,577 Å) bzw. P2-Paare zentriert, die zur a-Achse um 73,4° geneigt sind. Die Bindungslängen in den Hexathiodiphosphat(IV)-Anionen [P2S6]4- mit angenäherter 32/m - D3d-Symmetrie betragen d(P—P) = 2,20 und d̄(P—S) = 2,02 Å. Die Titelverbindung ist oberhalb TN = 28 K paramagnetisch mit μ = 4,69 B.M. und ordnet unterhalb TN antiferromagnetisch. Die beobachteten inneren Moden der Raman- und Infrarotspektren von K2Fe[P2S6] stehen im Einklang mit der Faktorgruppenanalyse. Die Schwingungsbanden werden auf der Basis von [P2S6]4--Einheiten unter Berücksichtigung der Abweichungen von der D3d-Symmetrie zugeordnet.
    Notes: K2Fe[P2S6] was synthesized from the elements at 1173 K in sealed quartz tubes. The compound forms transparent orange crystals, stable against air and moisture. K2Fe[P2S6] crystallizes in the monoclinic system, space group P21/n (No. 14), with cell dimensions (T = 298.5 K) a = 6.0622(4), b = 12.172(1) and c = 7.3787(8) Å, β = 101.113(7)°, Z = 2. The novel structure type (mP22) is characterized by columns of alternating face-sharing S6 octahedra and trigonal antiprisms (both distorted) parallel to the a axis, which are interconnected by inserted K+ (CN 10; {2,6,2}-polyhedra; d(K—S) = 3.231 - 3.845 Å). The S6 polyhedra of the columns are centered alternately by Fe (d̄(Fe—S) = 2.577 Å) and P2 pairs which are inclined to the a axis by 73.4°. The bond lengths in the hexathiodiphosphate(IV) anions, [P2S6]4-, with approximate 3 2/m - D3d symmetry, are d̄(P—P) = 2.20 and d̄(P—S) = 2.02 Å. The compound is paramagnetic above TN = 28 K with μ = 4.69 B.M. and orders antiferromagnetically below TN. The internal modes of the observed Raman and FIR spectra of K2Fe[P2S6] are in accord with the factor group analysis, and the spectra are assigned on the basis of [P2S6]4- units, taking into account the deviation from D3d symmetry.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 2
    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
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