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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

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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.

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Authors and Affiliations

  1. Department of Chemistry and Laboratory for Molecular Structure and Bonding, Texas A & M University, 77843, College Station, TX

    F. Albert Cotton, Maoyu Shang & Zhong Sheng Sun

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  1. F. Albert Cotton
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  2. Maoyu Shang
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  3. Zhong Sheng Sun
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Cotton, F.A., Shang, M. & Sun, Z.S. 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. J Clust Sci 3, 109–121 (1992). https://doi.org/10.1007/BF00702877

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  • DOI: https://doi.org/10.1007/BF00702877

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