Tetraethyl　2,4,8,10-tetra　methy1-6,1　2-bis(4-fluorophenyl)-3,9-dioxapentacyclol[6.4.0.0(2.7).0(4.11).0(5,10)]dode-cane-1,5,7,11-tetracarboxylate　(1,　simplified　as　6,12-bis(4-fluorophenyl)-3,9-dioxatetraasterane)　was　synthesized　by　[2　+　2]　photocyclization　of　diethyl　2,6-dimethyl-4-(4-fluorophenyl)-4H-pyran-3,5-dicarboxylate　(2)　in　solution.　The　NMR　analysis　of　1　is　discussed　in　detail　by　the　splittings　and　assignments　of　signals　according　to　the　three-dimensional　structure.　Single-crystal　X-ray　diffraction　shows　that　1　is　situated　on　an　inversion　center.　The　molecular　symmetry　is　close　to　C-2h　except　for　the　terminal　ethyl　groups.　(C)　2011　Elsevier　B.V.　All　rights　reserved.