Study on a new cyclodextrin based metal–organic framework with chiral helices
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A mixture of a β-CD (0.25mol) and Na2C2O4 (1mol) and 10mL CH3OH/H2O (8/2, v/v) was stirred for 1h at room temperature, then sealed in an 18mL Telfon-lined reactor and heated at 160°C for 3days. After slow cooling to room temperature, white like block crystal 1 was obtained (42% yield based on Na). Elemental analysis found: C, 41.18; H, 6.22; Calc. for compound 1, C84H146O84Na4 (2446.1): C, 41.21; H, 5.97.
Crystal data for C84H146O84Na4 (CD-MOF-1): Mr=2446.1. Orthorhombic, space group P212121, a=10.353(5)A°, b=19.678(5)A°, c=29.790(5)A°, α=β=γ=90°, V=6069(3), Z=4, Dc=1.38Mg/m3, 3.37<θ<25.00, F(000)=2580, T=293(2) K. The final R1 and wR2 were 0.0961 and 0.2667 respectively [I>2sigma(I)]. The X-ray crystallographic data were collected on on a Rigaku RAXIS RAPID IP with Mo-Kα monochromatic radiation (λ=0.71073Å) at 293K. The structures were solved by direct methods and refined using full-matrix least squares on F2. All calculations were performed using the SHELXL-97 program package. Absorption effects were empirically collected. All atoms except hydrogen atoms were refined anisotropically. The CCDC number is 1404895. Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB2 2EZ, UK (Fax: (+44) 1223–336033; e-mail: [email protected]).
Drug–CD-MOF inclusion complexes were prepared by grinding method at room temperature. In brief, 5-Fu and CD-MOF-1 were accurately weighted at a molar ration of 1:1, respectively. The result compounds were grinded with absolute alcohol as wetter. After grinding for 1h, the products were rinsed 3 times by using certain amount of absolute alcohol. The inclusion complexes were desiccated at 60°C until constant weight was obtained. Drug–β-CD inclusion complexes were prepared in a manner similar to that described for Drug–CD-MOF, except the β-CD replaced the CD-MOF.