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2
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84885433987
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All operations were carried out under an inert atmosphere employingstandard Schlenk-line or glovebox techniques. Ethylenediamine (99, Aldrich) wasdistilled over sodium metal while toluene (99.9, Rathbum Chemicals. Ltd, andTHF (99.9, Rathbum Chemicals, Ltd, were purified through an MBraun MB SPS-800solvent system. All solvents were stored in gas-tight ampoules under argon. Theintermetallic precursor. K4Ge9. was synthesized from astoichiometric mixture of the elements (K: 99.95, Aldrich; Ge: 99.999% Strem)according to a previously reported synthetic procedure, K(2,2.2-crypt)]3[Fe@Ge10]·2en: K 4Ge9 (62 mg,0.077 mmol, FeAr2 (26 mg, 0.038 mmol, and 2,2,2-crypt (50 mg,0.133 mmol) were weighed out into a test tube inside a nitrogen-filled glovebox.The solids were dissolved in ethylenediamine (2 mL) and trace amounts of THFwere added to aid in the dissolution of FeAr 2. The reaction mixturew
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+.
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3
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84885429487
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Single crystal X-ray diffraction data were collected at 150 K on anEnrafNonius Kappa-CCD diffractometer equipped with an Oxford Cryosystemslow-temperature device. The crystal was mounted on a glass fiber usingN-Paratone oil and quickly placed under the nitrogen flow of the cryostream.Data were collected using graphite-monochromated Mo Kα radiation (λ= 0.710 73 A°, equivalent reflections were merged, and the images wereprocessed with the DENZO and SCALEPACK programs. Corrections for Lorentzpolarization effects and absorption were performed, and the structures weresolved by direct methods using SIR92. The structures were refined on F 2 using SHELXL. Crystallographic data for [K(2,2,2ctypt, 3[Fe@Ge10]·2en: triclinic. P1̄, a =14.4014(1, b, 15.7227(1, c, 21.6608(2, α, 93.2587(3, β =100.4043(3, γ, 107.2794(4, V, 4574.29(6, Z, 2, Rl/wR24.38/11.88% for the observed data (I ≥ 2σI, R1/wR
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10]·2en: triclinic. P1̄, a =14.4014(1), b = 15.7227(1), c = 21.6608(2), α = 93.2587(3). β =100.4043(3), γ = 107.2794(4), V = 4574.29(6). Z = 2, Rl/wR24.38/11.88% for the observed data (I ≥ 2σ(I)). R1/wR2 5.72, 12.56% forall the data.
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4
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85134131804
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Urnèźeius, E.; Brennessel, W. W.; Cramer, C. J.; Ellis. J.E.; von R. Schleyer, P. Science 2002, 295, 832.
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Urnèźeius, E.; Brennessel, W. W.; Cramer, C. J.; Ellis. J.E.; von R. Schleyer, P. Science 2002, 295, 832.
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5
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33845262269
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For a recent review of the solution reactivity of deltahedral Zintl ions,see: S. C.; Goicoechea, J. M. Oreanometallics 2006, 25,5678.
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For a recent review of the solution reactivity of deltahedral Zintl ions,see: S. C.; Goicoechea, J. M. Oreanometallics 2006, 25,5678.
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8
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54349114926
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(c) Scharfe, S.; Fässler, T. F.; Stegmaier, S.; Hoffmann, S. D.;Ruhland, K. Chem. - Eur. J. 2008, 14, 4479.
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Hermes. A, R.; Girolami, G. S. Oreanometallics 1987.6, 763.
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(b) Hermes. A, R.; Girolami, G. S. Oreanometallics 1987.6, 763.
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A pseudo-[4]prismane with eight vertices and six organic ligands has beenreported bv Schepf and Köppe in: A.; Köppe. R. Angew. Chem., Int.Ed. 2003,42,911.
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A pseudo-[4]prismane with eight vertices and six organic ligands has beenreported bv Schepf and Köppe in: A.; Köppe. R. Angew. Chem., Int.Ed. 2003,42,911.
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