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Molybdenum (Vi) imido complexes derived from chelating phenols: Synthesis, characterization and ɛ-caprolactone rop capability

Catalysts, ISSN: 2073-4344, Vol: 5, Issue: 4, Page: 1928-1947
2015
  • 18
    Citations
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  • 9
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Metrics Details

  • Citations
    18
    • Citation Indexes
      18
  • Captures
    9

Article Description

Reaction of the bulky bi-phenols 2,2′-RCH[4,6-(t-Bu)2C6H2OH]2 (R = Me LH, Ph LH) with the bis(imido) molybdenum(VI) tert-butoxides [Mo(NR)(NR)(Ot-Bu)] (R = R = 2,6-CH-i-Pr; R = t-Bu, R = CF) afforded, following the successive removal of tert-butanol, the complexes [Mo(NCHi-Pr-2,6)2L] (1), [Mo(NCHi-Pr-2,6)2L] (2) and [Mo(Nt-Bu)(μ-NCF)(L)]2 (3). Similar use of the tri-phenol 2,6-bis(3,5-di-tert -butyl-2-hydroxybenzyl)-4-methylphenol (LH) with [Mo(NCHi-Pr-2,6)(Ot-Bu)] afforded the oxo-bridged product [Mo(NCHi-Pr-2,6)(NCMe)(μ-O)LH] (4), whilst use of the tetra-phenols α,α,α′,α′-tetrakis(3,5-di-tert-butyl-2-hydroxyphenyl)-p- or -m-xylene LpH/LH led to {[Mo(NCHi-Pr-2,6)](μ-L)} (5) or {[Mo(NCHi-Pr-2,6)](μ-L)} (6), respectively. Similar use of [Mo(NCF)(Ot-Bu)] with LH afforded, after work-up, the complex {[Mo(NCF)(Ot-Bu)](μ-L)}·6MeCN (7·6MeCN). Molecular structures of 1, 2·CHCl, 3, 4·6MeCN, 6·2CH, and 7·6MeCN are reported and these complexes have been screened for their ability to ring open polymerize (ROP) ε-caprolactone; for comparative studies the precursor complex [Mo(NCHi-Pr-2,6)Cl(DME)] (DME = 1,2-dimethoxyethane) has also been screened. Results revealed that good activity is only achievable at temperatures of ≥100 °C over periods of 1 h or more. Polymer polydispersities were narrow, but observed molecular weights (M) were much lower than calculated values.

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