01623nas a2200205   4500008004100000022001400041245012600055210006900181260007500250300001200325490000700337520079400344653003301138653001901171653001801190653002901208100003001237700002801267856012201295       2013                        eng d  a0039-788100aEasy and multigram-scale synthesis of pillar[5]quinone by the hypervalent iodine oxidation of 1,4-dimethoxypillar[5]arene0 aEasy and multigramscale synthesis of pillar5quinone by the hyper  aRUDIGERSTR 14, D-70469 STUTTGART, GERMANYbGEORG THIEME VERLAG KGcAPR  a896-8980 v453 a<p>Pillar[5]quinone (P[5]Q), a potential molecule for anion recognition and supramolecular host-guest chemistry, has not as yet been used for practical purposes, presumably due to the synthetic difficulties in obtaining it in large amounts. Herein, we reveal an easy-to-operate and chromatography-free synthetic strategy that can furnish P[5]Q on a multigram scale; its success relies on the utility of hypervalent iodine, generated in situ from Oxone/ iodobenzene, as an efficient oxidant. Pillar[5]quinone was obtained in multigram quantities by oxidation of 1,4-dimethoxypillar[5]arene with Oxone/iodobenzene and simple purification by crystallization from 1,1,2,2-tetrachloroethane, thus opening up the opportunity to explore the properties of this interesting macrocyclic quinone.</p>10ahypervalent iodine oxidation10amacromolecules10apillar-arenes10asupramolecular chemistry1 aShivakumar, Kilingaru, I.1 aSanjayan, Gangadhar, J.  uhttp://library.ncl.res.in/content/easy-and-multigram-scale-synthesis-pillar5quinone-hypervalent-iodine-oxidation-14-001990nas a2200205   4500008004100000022001400041245013000055210006900185260007100254300001400325490000700339520115900346100003001505700001801535700002201553700002401575700002701599700002801626856013001654       2015                        eng d  a1528-748300aExploiting powder x-ray diffraction to establish the solvent-assisted solid-state supramolecular assembly of pillar[5]quinone0 aExploiting powder xray diffraction to establish the solventassis  a1155 16TH ST, NW, WASHINGTON, DC 20036 USAbAMER CHEMICAL SOCcAPR  a1583-15870 v153 a<p>We report the solvent-mediated supramolecular assembly of pillar[5]quinone (P[5]Q), a symmetric cyclamer containing five benzoquinone moieties bridged by five alternating methylene units. The supramolecular assembly of P[5]Q is shown to be facilitated by 1,1,2,2-tetrachloroethane (TCE) as solvent, producing a microcrystalline solvate material P[5]Q(.)2TCE with a fluffy texture. Optical and electron microscopy reveal that this material has a rod-shaped morphology, extending to several micrometers in length. Due to the microcrystalline nature of the material, structure determination was carried out directly from powder X-ray diffraction data, augmented by high-resolution solid-state C-13 NMR. The two crystallographically distinct TCE molecules occupy different types of void in the structure and have different dynamic properties. Crystallization of P[5]Q was attempted from a large number of different solvents, but only TCE was found to facilitate the formation of a crystalline phase. Indeed, features of the crystal structure suggest that the TCE component plays an important role in promoting the columnar assembly of P[5]Q molecules.</p>1 aShivakumar, Kilingaru, I.1 aYan, Yuncheng1 aHughes, Colan, E.1 aApperley, David, C.1 aHarris, Kenneth, D. M.1 aSanjayan, Gangadhar, J.  uhttp://library.ncl.res.in/content/exploiting-powder-x-ray-diffraction-establish-solvent-assisted-solid-state-supramolecular-1