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The diacetylene monomer crystal of C 20 H 28 N 2 O 8  are triclinic, P[unk],  a  = 25.753(8),  b  = 13.966(2),  c  = 4.940(1) Å,  α  = 85.19(1),  β  = 90.38(2),  γ  = 84.52(2)°,  Z  = 3. The monomer crystals of C 22 H 32 N 2 O 8  present a monoclinic “orange form”,  C 2/ c  or  Cc ,  a  = 36.509(5),  b  = 7.983(1),  c  = 9.783(1) Å,  β  = 96.02(1)°,  Z  = 4, but a twin often gives them an orthorhombic appearance. This second compound presents a solid-state polymerization but the first one is inactive.

Crystal data for monomer forms of 2,4 hexadiyne-1,6-bis (butylcarboxymethylurethane) and 3,5 octadiyne-1,8-bis (butylcarboxymethylurethane)