Journal
INORGANIC CHEMISTRY
Volume 51, Issue 15, Pages 8629-8635Publisher
AMER CHEMICAL SOC
DOI: 10.1021/ic301405r
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Funding
- Fundacao para a Ciencia e a Tecnologia (FCT), COMPETE
- European Union [PDTC/QUI-QUI/098098/2008, FCOMP-01-0124-FEDER-010785]
- FCT [SFRH/BD/45116/2008, SFRH/BD/64224/2009, SFRH/BPD/73540/2010]
- Associate Laboratory CICECO [Pest-C/CTM/LA0011/2011]
- Fundação para a Ciência e a Tecnologia [SFRH/BD/64224/2009, SFRH/BD/45116/2008, SFRH/BPD/73540/2010] Funding Source: FCT
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The reaction of [MoO2Cl2(pypzEA)] (1) (pypzEA = ethyl[3-(pyridin-2-yl)-1H-pyrazol-1-yl]acetate) with water in a Teflon-lined stainless steel autoclave (100 degrees C) or in an open reflux system leads to the isolation of the molybdenum oxide/pyrazolylpyridine composite material [Mo2O6(HpypzA)] (2; HpypzA = [3-(pyridinium-2-yl)-1H-pyrazol-1-yl]-acetate). The solid state structure of 2 was solved through single crystal and powder X-ray diffraction analyses in conjunction with information derived from FT-IR and C-13 CP MAS NMR spectroscopies and elemental analyses. In the asymmetric unit of 2, two crystallographically distinct Mo6+ centers are bridged by a syn,syn-carboxylate group of HpypzA. The periodic repetition of these units along the a axis of the unit cell leads to the formation of a one-dimensional composite polymer, (1)(infinity)[Mo2O6(HpypzA)]. The outstretched pyrazolylpyridine groups of adjacent polymers interdigitate to form a zipper-like motif, generating strong onset pi-pi contacts between adjacent rings of coordinated HpypzA molecules. The composite oxide 2 is a stable heterogeneous catalyst for liquid-phase olefin epoxidation.
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