The title compound 9-(2-hydroxy-5-nitrophenyl)-9H-dibenzo[c,h]-2,7,10-trioxan-thene-1,8-dione DMF solvate (C28H20N2O9,Mr=528.46) was synthesized and crystallized.The crystal belongs to the triclinic system,space group P1 with a=10.210(3),b=10.698(4),c=12.522(4),α=92.214(6),β=113.751(5),γ=105.040(5)°,Z=2,V=1193.0(7)3,Dc=1.471 g·cm-3,μ(MoKα)=0.112 mm-1,F(000)=548,R=0.0444 and wR=0.1141 for 2667 observed reflections (I > 2σ(I)).X-ray analysis reveals that atoms C(1),C(2),C(3),C(4),C(5) and O(1) on the new 4H-pyran ring are slightly distorted,forming a half-chair conformation.