A new 5,5’ -bisdiazo-dipyrromethane, compound 2, has been synthesized and cha- racterized. The crystal of 2 is of monoclinic, space group P21/c with a = 16.3185(10), b = 20.8225(13), c = 18.5985(11) , β = 114.5280(10)°, V = 5749.3(6) 3 , Z =8, C25H26N6O2 , Mr = 442.52, Dc = 1.022 g/cm, F(000) = 1872, μ(MoKα) = 0.068 mm -1 . The final R = 0.0469 and wR = 0.1143 for 10119 observed reflections with I > 2σ(I), and R = 0.0677 and wR = 0.1231 for all reflections. The title compound prefers to form interlocked type dimer through quadruple N-H N hydrogen bonds. The dimers self-assemble into a porous 3-D structure through O-H O and C-H N hydrogen bonds.