(R)-乙基-2-吡啶亚砜与(4R,5R)-TADDOL包结晶体[C_7H_9NOS·C_(31)H_(30)O_4]的晶体结构分析

Studies on Crystal Structure of Inclusion Chiral Crystal of ( R) Ethyl 2 pyridyl Sulfoxide with ( 4R,5R ) TADDOL

（Ｒ）－乙基－２－吡啶亚砜与（４Ｒ，５Ｒ）－二（羟基－二苯基－甲基）－２，２－二甲基－１，３－二氧戊环（ＴＡＤ－ＤＯＬ）可以形成物质的量比为１∶１的手性包结晶体，Ｘ射线衍射分析确定该晶体属单钭晶系，Ｐ２１空间群，ａ＝０．９７０１（２）ｎｍ，ｂ＝０．９９５３（２）ｎｍ，ｃ＝１．７３９２（２）ｎｍ；β＝９２．０７９°（１４），Ｖ＝１．６７８１（５）ｎｍ３，Ｚ＝２，Ｄｃ＝１．２３０ｇ／ｃｍ３，分子式Ｃ３８Ｈ３９ＮＯ５Ｓ，Ｍｒ＝６２１．７６，最终偏离因子Ｒ＝０．０３５１，ＲＷ２＝０．０７７２，Ｆｌａｃｋ值为０．１（２）．结构分析表明，主客体存在分子间氢键．光学纯的ＴＡＤＤＯＬ与消旋的乙基吡啶亚砜（１）作用时，ＴＡＤＤＯＬ对１具有很好的手性识别能力，选择性地与１的一个对映体形成氢键，长成晶体．

The synthesis and crystal structure of 1∶1 inclusion chiral crystal formed from ( R ) ethyl 2 pyridyl sulfoxide with ( 4R,5R ) α,α,α,α tetraaryl 1,3 dioxolane 4,5 dimethanol(TADDOL) were reported here. The crystal belongs to monoclinic, space group P2 1, a= 0.970 1(2) nm, b = 0.995 3(2) nm, c = 1.739 2(2) nm; β= 92.079° (14), V= 1.678 1(5) nm 3, M r= 621.76 , Z =2, D c= 1.230 g/cm 3. The final refinement converges to R = 0.053 1 and R w 2 = 0.077 2 for 2 335 observed independent reflections. Flack value is 0.1 (2). There is an intermolecular hydrogen bond in the inclusion crystal. Chiral TADDOL and ethyl 2 pyridyl sulfoxide(1) can be recognized each other in the inclusion crystal. Moreover, sulfoxide(1) in high enantiomeric excess was preparaed by resolution through inclusion complexation with the chiral TADDOL. The absolute configuration of (-) ethyl 2 pyridyl sulfoxide was confirmed to be ( R ), which was assigned by the ( R,R ) absolute configuration of the TADDOL as an internal reference.