Crystal structure of 3,4-diacetyl-15,21-dioxatetracyclo-[23.4.0.02,7.06,11]nonacosa-1(29),2,4,6,8,10,25,27-octaene-14,22-dione — water (1:2), C31H32O6 · 2H2O
| Autor: | Annika Matthes, Pablo Wessig, Uwe Schilde |
|---|---|
| Rok vydání: | 2010 |
| Předmět: | |
| Zdroj: | Zeitschrift für Kristallographie - New Crystal Structures. 225:744-746 |
| ISSN: | 2197-4578 1433-7266 |
| DOI: | 10.1524/ncrs.2010.0328 |
| Popis: | C31H36O8 ,m onoclinic, P121/a 1( no. 14), a =1 2.956(1) A, b =1 5.054(2) A, c =1 5.446(2) A, * =1 05.120(7)°, V =2 908.4 A 3 , Z =4 , Rgt(F) =0 .057, wRref(F 2 ) =0 .168, T =2 10 K. Source of material The title compound was synthesized via Photo-Dehydro-DielsAlder (PDDA) reaction by irradition of the pentane-1,5-diyl-(3[2-{3-oxobut-1-ynyl}phenyl)propanoate for 50 min in t-butanol (yield 29 %) .T he product (37 mg, 0.076 mmol) was solved in 2m lo fam ixture of diethylether/isopentane/ethanol (5:5:2) after isolation by column chromatography (hexane/ethyl acetate 3:2) and removing the solvent. Colourless needle-like crystals were formed by slowly vaporizing the solvent. Experimental details The O3···C28 moiety is disordered over two sides with an occupation ratio of 0.5/0.5. The hydrogen atoms on the aromatic rings were located from the difference Fourier map. The other hydrogen atoms were calculated in their expected positions. All H atoms were included in the refinement as riding atoms with Uiso(H) =1 .2 Ueq(C). The crystal structure contains disordered water as solvate molecules. In spite of several attempts, the electronic density in this area could not be resolved satisfactorily. Therefore the contribution of the disordered solvent species was subtracted from the structure factor calculations by the SQUEEZE instruction of the program PLATON. Using that pro |
| Databáze: | OpenAIRE |
| Externí odkaz: |
|