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(2,4,6-Trinitrophenyl)guanidine (picrylguanidine), C7H6N6O6, from the reaction of picrylsulfonic acid with guanidine carbonate, forms a three-dimensional framework structure through extensive hydrogen-bonding interactions, extending the centrosymmetric cyclic R22(16) dimer association which includes duplex R22(8) guanidine N—H...Onitro interactions. The guanidine substituent chain has an endo [Ph—N=C(NH2)2] bond sequence rather than the less sterically encumbered exo [Ph—NH—C=NH(NH2)] sequence of the tautomeric form. As a result, there is significant bond-angle distortion about C(—N=) of the aromatic ring.