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  • 1990-1994  (2)
  • 1955-1959
  • Molybdenum tetranuclear cluster  (1)
  • bridging acetate  (1)
  • 1
    Electronic Resource
    Electronic Resource
    The structure of Mo4Cl8(PEt3)4: How unrecognized disorder previously reduced the quality of the refinement (1991)
    Springer
    Journal of cluster science 2 (1991), S. 121-129 
    Details
    ISSN: 1572-8862
    Keywords: Molybdenum tetranuclear cluster ; rectangular ; triethylphosphine ligand ; preparation ; crystal structure
    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 preparation and structure of the title compound were reported several years ago by McCarly and co-workers ((1978).J. Am. Chem. Soc. 100, 7900). Curiously, it was reported that refinement of the structure converged at exceptionally high figures of merit (R=0.126;R w =0.158), but no reason was given. In view of a recent observation in this laboratory (Chen and Cotton (1991).J. Am. Chem. Soc. 113, 5857) that a similar type of compound, [Re4Cl8(μ-O)2(μ-OMe)2]2− exhibited a subtle but elegant disorder, we reexamined the crystal structure of the title compound. It is found to have 92% of the Mo4 rectangles in one orientation (the only one previously included in the refinement) and 8% in an orientation perpendicular to the main one. In both orientations the ligand positions are approximately the same. The figures of merit are nowR=0.041;R w =0.064. The three structure parameters previously reported are now only slightly different: Mo-Mo=2.210(1) vs. 2.211(3) Å; Mo-Mo'=2.897(1) vs. 2.901(2) Å; angle Mo-Clb-Mo=74.2[8]° vs. 74.4(2)°. We report here the complete structure.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00702953
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    Paper (German National Licenses)
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  • 2
    Electronic Resource
    Electronic Resource
    Preparation and structural characterization of the isomorphous compounds: [Bu4N][Mo3(μ3-O)(μ-X)3(μ-OAc)3 X 3]·(CH3)2CO,X=Cl, Br (1992)
    Springer
    Journal of cluster science 3 (1992), S. 109-121 
    Details
    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
    URL: http://dx.doi.org/10.1007/BF00702877
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    Paper (German National Licenses)
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