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  • Electronic Resource  (3)
  • trinuclear  (2)
  • Hexanuclear zirconium cluster  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Journal of cluster science 9 (1998), S. 63-91 
    ISSN: 1572-8862
    Keywords: Hexanuclear zirconium cluster ; pentanuclear zirconium cluster ; cluster hydrogen atom ; bromide ; chloride ; arsine ; amine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Reduction of ZrBr4 with HSnBu3 yielded a blue solid. When this blue solid was treated with PMe3, a hexanuelear cluster [Zr6Br14H4( PMe3)4] (2) was isolated. Reaction of the blue solid with [PPh4]Br in CH2Cl2 resulted in the formation of a paramagnetic and unstable cluster anion, [Zr6Br18H5]2− (3′), which disproportionated to form a new cluster anion, [Zr6Br18H5]3− (4′) and some Zr(IV) species. Compounds containing 4′ can also be obtained from reaction of the blue solid with Br− in MeCN. Reduction of ZrCl4 with HsnBu3 gave a red–brown solid, and [Zr6Cl14H4(AsMe3)4] (9) and [Zr5Cl12H4(AsMe3)5](8) were obtained by reaction of the red–brown solid with AsMe3. No cluster compounds containing amine ligands were obtained in the reaction of the red–brown solid with amines; only compounds containing the [Zr6Cl18 H5]3− anion and ammonium cations were isolated. Altogether ten products were characterized by single crystal X-ray diffraction and where possible, by 1H NMR studies.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1572-8862
    Keywords: Tungsten ; clusters ; preparation ; triangular ; trinuclear
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Synthetic methods are reported for the preparation of compounds containing the trinuclear triangular cluster [W3S4Br3(depe)3[+. These involve reactions between WBr5 and NaB(C2 H5)3H or NaBH4 as reducing agent in THF, and subsequent addition of methanolic solutions of NaHS and depe ligand. Both compounds, [W3S3Br3(depe)3]PF6·0.5C7H8,1, and [W3S4Br3(depe)3]Br·2CH3OH,2, are characterized by x-ray single crystal studies. Compounds1 and2 crystallize in space group $$P\bar 1$$ . For1,a=10.427 (3) Å,b=15.415(4) Å,c=18.140(5) Å, α=79.36(2)°, β=73.59(2)°, γ=81.54(2)°, andV=2734.8(2) Å3;R=0.050 and for 2a=10.491(3) Å,b=15.074(3) Å,c=18.246 Å, α=95.76(2)°, β=105.82(2)°, γ=98.18(2)°, andV=2718.4(3) Å3;R=0.081. The two cations in1 and2 possess C3 symmetry. The W-W distances are in the range 2.783−2.891 Å (for1) and 2.778−2.785 Å (for2) and the average W-Br distances in1 and2 are 2.616[2] Å and 2.594[4] Å, respectively. Each metal atom in the [W3S4Br3(depe)3]+ ions is attached to one capping sulfur atom, two bridging sulfur atoms, one bromine atom, and one chelating depe ligand. One P atom in depe ligand istrans to μ3-S and the otherP atom istrans to a μ2-S atom. UV-Vis and NMR spectra for these compounds are also reported.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 1572-8862
    Keywords: Molybdenum ; trinuclear ; oxo ligand ; briding halide ; bridging acetate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The reaction of MoCl3(H2O)3 with a mixture of acetic acid and acetic anhydride in the presence of [N(C4H9)4][BF4] followed by crystallization from acetone/hexane gives a 77% yield of dark purple [NBu4][Mo3OCl6(OAc)3]·Me2CO (1). A similar reaction employing MoBr3(H2O)3 gives purple [NBu4][Mo3OBr6(OAc)3]·Me2CO (2) in 50% yield. Also produced in this reaction in low (10–20%) yields are [NBu4]2[Mo4OBr12] · 0.5Me2CO and [NBu4]2[Mo3OBr6(OAc)3] · Me2CO which will be discussed elsewhere Compounds (1) and (2) are isomorphous, space groupP21/n,Z=4 with the following unit cell dimensions, where the values for (1) and (2) are given in that order for each one:a=13.406(4), 13.726(5) Å;b=15.701(4), 15.839(5) Å;c=19.250(5), 19.831(6) Å; β=101.61(2), 102.92(3)°. Both (1) and (2) are eight-electron species in which the mean Mo-Mo distances are 2.578(1) Å and 2.597(1) Å, respectively.
    Type of Medium: Electronic Resource
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