Co-crystallization with acetylene. Part III. Molecular complexes with aromatic azacycles

Using C–H⋯N interactions, acetylene can be introduced at increased pressure to form molecular complexes with azacyclic N-acceptors which can be crystallized and investigated by X-ray methods. With pyridine, we expected dumbbell-like 2∶1 complexes with acetylene in the middle, instead a 1∶1 zigzag chain is formed where each of the N-atoms accepts two hydrogen atoms from two acetylene molecules. The same happens with 2,5-dimethylpyridine which, together with water, results in a complex having the water chains networked by acetylene molecules. With 2,5-dimethylpyrazine, linear chains are found which are additionally stabilized by sp3 and sp2 C–H⋯N interactions. 2,6-Di-tert-butylpyridine forms a clathrate with acetylene.

[1]  W. E. Billups,et al.  Gas hydrate single-crystal structure analyses. , 2004, Journal of the American Chemical Society.

[2]  Jack D. Dunitz,et al.  Crystal and co-crystal: A second opinion , 2003 .

[3]  Gautam R. Desiraju,et al.  Crystal and co-crystal , 2003 .

[4]  W. E. Billups,et al.  Cocrystallization with acetylene: molecular complexes with acetone and dimethyl sulfoxide. , 2003, Angewandte Chemie.

[5]  A. Gavezzotti,et al.  Cocrystallization with acetylene. The 1:1 Complex with benzene: Crystal growth, X-ray diffraction and molecular simulations. , 2003 .

[6]  J. Davies,et al.  2,5-Lutidine , 2002 .

[7]  C. Wilson Migration of the proton in the strong O-H.O hydrogen bond in urea-phosphoric acid (1/1). , 2001, Acta crystallographica. Section B, Structural science.

[8]  P. van der Sluis,et al.  BYPASS: an effective method for the refinement of crystal structures containing disordered solvent regions , 1990 .

[9]  B. Ault,et al.  Infrared matrix isolation study of hydrogen bonds involving C-H bonds: Substituent effects , 1989 .

[10]  B. Ault,et al.  Infrared matrix isolation study of hydrogen bonds involving carbon-hydrogen bonds: alkynes with oxygen bases , 1987 .

[11]  D. Mootz,et al.  Crystal structures of pyridine and pyridine trihydrate , 1981 .

[12]  R. Fourme,et al.  A redetermination and group‐refinement of the molecular packing of benzene II at 25 kilobars , 1971 .

[13]  C. E. Weir,et al.  Crystal Structure of Benzene II at 25 Kilobars , 1969, Science.