Synthesis and crystal structure of 13-phenyl-1,10-dithia-4,7-dioxa-13-aza-15-Crown-5

Crystal structure of the title Compound C-16 H-25 O-2 NS2 has been determin ed by Xray diffraction method. Its crystallographic data were as follows: M -r = 327.51, triclinic, space group P1, a = 8.864(3), b = 10.127(4), c = 10 .390(3) Angstrom, alpha = 105.94(3), beta = 103.10(2), gamma = 90.96(3)degr ees, V = 870.3(7) Angstrom (3), Z = 2, D-c = 1.250g.cm(-3), mu (MoK alpha) = 2.966cm(-1), F(000) = 176, a total of 3275 reflections measured (2 theta (max) = 50 degrees), 2246 [I greater than or equal to 5 sigma (I)] used in the refinement, R = 0.067, R-w = 0.082. The result shows that the distances of N(1) - C(2) and N(1) - C(3) are longer than that of N(1) - C(11), which indicates that the interaction of C-Lambdar - N-sp(2) is stronger than tha t of C-sp(3) - N-sp(2). Oxygen, nitrogen and sulfur atoms of the ring in th e same plane was deduced from the least-squares planes and the dihedral ang les.