Study on the preparation and crystal structure of 3,4- diaminofurazanofuroxan

A new furazano (furoxano) energetic compound 3,4-diaminofurazanofuroxan (DAFF) was first prepared under thermal conditions by losing HCl followed by [4 + 2] ring-closure reaction of 3-amino-4-chloroximinofurazan. Its single crystal was cultivated and the structure was characterized by X-ray single crystal diffraction, IR and elemental analysis. Its crystal is triclinic, space group P1 with crystal parameters a=0.6400(4) nm, b=1.0609(8) nm, c=1.4634(7) nm, α=83.53(5)°, β=87.27(4)°, γ= 77.74(5)°, V=0.9645(11) nm³, Z=4, D_c=1.737 g·cm^-3, F(000)=512, μ(Mo Kα)=0.149 mm^-1; R₁= 0.0568, wR₂=0.1137. The obtained results indicate that DAFF is not a kind of planar molecule, the three ring-planes twist with the two clamp-angles between them are 27.18(1.99)° and 30.48(2.07)°, respectively. There are intramolecular and intermolecular hydrogen bonds in the crystal.