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Non-merohedrally Twinned Crystal Structure of the Co-crystal Ethyl 6-(2-5-(Ethoxycarbonyl)-pyridin-2-yl-1,2-dihydroxyethyl)pyridine-3-carb-oxylateethyl 6-(2-5-(Ethoxycarbonyl)pyridin-2-yl-2-hydroxyacetyl)pyridine-3-carboxylate(0.69/0.31) 被引量：1

Non-merohedrally Twinned Crystal Structure of the Co-crystal Ethyl 6-(2-5-(Ethoxycarbonyl)-pyridin-2-yl-1,2-dihydroxyethyl)pyridine-3-carb-oxylateethyl 6-(2-5-(Ethoxycarbonyl)pyridin-2-yl-2-hydroxyacetyl)pyridine-3-carboxylate(0.69/0.31)
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摘要 The two component molecules of the co-crystal 0.69（C18H2ON206）.0.31（C18H18N2O6） lie on a center-of-inversion that exists midway along the ethylene chain connecting the two aromatic rings. The two molecules are superimposed. The crystal is also a non-morohedral twin with a minor 37.7（2）% component. The refinement of this twinned and disordered crystal structure is detailed. Crystal data： C18H19.38N2O6, monoclinic, P21/c, a = 17.1687（8）, b = 5.4389（2）, c = 9.3261（4） A, b = 95.270（5）° and V= 867.18（6） A3 at -173 ℃. The two component molecules of the co-crystal 0.69（C18H2ON206）.0.31（C18H18N2O6） lie on a center-of-inversion that exists midway along the ethylene chain connecting the two aromatic rings. The two molecules are superimposed. The crystal is also a non-morohedral twin with a minor 37.7（2）% component. The refinement of this twinned and disordered crystal structure is detailed. Crystal data： C18H19.38N2O6, monoclinic, P21/c, a = 17.1687（8）, b = 5.4389（2）, c = 9.3261（4） A, b = 95.270（5）° and V= 867.18（6） A3 at -173 ℃.
作者 ZHANG Wen-Hua NG Seik Weng
机构地区 Institute of Materials Research & Engineering Department of Chemistry Chemistry Department
出处 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2013年第8期1159-1162,共4页 结构化学（英文）
基金 the University of Malaya (grant No. UM.C/HIR/MOHE/SC/12) for supporting this study
关键词 CO-CRYSTAL non-merohedral twin co-crystal, non-merohedral twin
分类号 O626 [理学—有机化学]
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参考文献8

  • 1Zukerman-Schpector,J.; Tiekink,E.R.T.Z.Kristallogr.2008,223,233-234.
  • 2The sphere of 6567 reflections was measured on a SuperNova diffractometer equipped with Cu-Ka radiation (l 1.54184 )at-173℃to a 2qmaxof150°.The major component had 2332 isolated reflections and the second 2320 isolated reflections; 3135 were overlapping ones.The reflectionsaveraged (Rint0.025)to 3055 reflections,with 2909 satisfying the I > 2 (I)criterion.The structure refined on 130 parameters and 7 restraints to afinal R index of 0.057 (CCDC 918609).
  • 3Spek,A.L.Structure validation in chemical crystallography.Acta Cryst.2009,D65,148-155.
  • 4Cooper,R.I.; Gould,R.O.; Parson,S.; Watkins,D.J.The derivation of non-merohedral twin laws during refinement by analysis of poorly fittingintensity data and the refinement of non-merohedrally twinned crystal structures in the program CRYSTALS.J.Appl.Cryst.2002,35,168-174.
  • 5Indium trichloride (0.022 g,0.1 mmol)and 5-ethoxycarbonyl-2-hydroxymethylpyridine (0.036 g,0.2 mmol)were mixed in a glass bottle and amixture of DMF/H2O (3/3 mL)was added.The bottle was then sealed and heated at 95℃for 72 h and then cooled to room temperature.A whilepowder was removed by filtration; the faint yellow filtrate was allowed to evaporate to yield faint yellow crystals; these were colorless when viewedunder a microscope.1H NMR (400 MHz,CDCl3)δ9.21 (d,J = 1.6 Hz,1H),8.97 (d,J = 1.7 Hz,1H),8.39 (dd,J = 8.2,2.1 Hz,1H),8.23 (dd,J = 8.5,2.1 Hz,1H),8.06 (d,J = 8.2 Hz,1H),7.24 (d,J = 8.5 Hz,1H),6.99 (s,1H),4.38-4.46 (m,4H),1.49-1.35 (m,6H)ppm.13C {1H} NMR (101 MHz,CDCl3):δ164.24,161.27,156.97,150.62,147.01,138.42,138.15,126.71,122.50,120.32,97.67,61.84,61.72,14.68 ppm.MS (ESI)(CH2Cl2,150℃): 747.17 m/z: [M(diketone form)+ M(acyloin form)+ CH3OH + H]+.IR (KBr pellet): 2996 (w),2957 (w),2923 (w),2897 (w),2849 (w),1714(s),1590 (s),1555 (s),1473 (s),1448 (s),1394 (s),1368 (s),1298 (s),1267 (s),1131 (s),110.
  • 6Asiri,M.A.; Al-Youbi,A.O.; Faidallah,M.H.; Ng,S.W.2-Amino-4-phenyl-5,6-dihydrobenzo[h]quinolone-3-carbonitrile 3-amino-1-phenyl-9,10-dihydrophenanthrene-2,4-dicarbonitrile (5/3).Acta Cryst.2011,E67,o2872.
  • 7Asiri,M.A.; Al-Youbi,A.O.; Faidallah,M.H.; Ng,S.W.2-Amino-4-(3,4-dimethoxy)-5,6-dihydrobenzo[h]quinolin-3-carbonitrile 3-amino-1-(3,4-dimethoxylphenyl)-9,10-dihydrophenanthrene-2,4-dicarbonitrile (1/19).Acta Cryst.2011,E67,o2873.
  • 8Asiri,M.A.; Al-Youbi,A.O.; Faidallah,H.M.; Ng,S.W.2-Amino-4-(4-chlorophenyl)-5,6-dihydrobvenzo[h]quinolone-3-carbonitrile 3-amino-1-(4-chlorophenyl)-9,10-dihydrophenanthrene-2,4-dicarbonitrile (1/4).Acta Cryst.2011,E67,o2874.

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Chinese Journal of Structural Chemistry
2013年 第8期

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