A complex from copper(II) perchlorate with 4‐amino‐1,2,4‐triazole (4‐AT, C2H4N4) was synthesized, and elemental composition, molecular structure, and explosive properties were determined. To this end, elemental and X‐ray analyses were carried out, sensitivity to mechanical and thermal stimuli was measured, mechanism of thermal decomposition was investigated, and kinetic parameters of decomposition were determined. In the next step measurements of heat of combustion and detonation velocity were performed. Detonation parameters were also calculated. It was stated that the complex has slightly distorted square bipyramidal (4+2) coordination. The four basal bonds are formed by nitrogen atoms of four 4‐AT molecules. The coordination of the metal is completed by two axial oxygen atoms, one of the perchlorate ion, and one of the water molecule. With respect to explosive properties, tetrakis(4‐AT)copper(II) perchlorate monohydrate belongs to the group of sensitive secondary explosives.

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In the condensation reaction of nitromethane with glyoxal carried out in an aqueous solution of sodium hydroxide, 3,6-dinitro-cyclohexane-1,2,4,5-tetraol was obtained (the expected product, described in the literature) and, unexpectedly, also tricyclic nitro-triol (6b-nitrohexahydro-2H-1,3,5-trioxacyclopenta[cd]-pentalene-2,4,6-triol), which has been unknown until now, was obtained as the main product. The structure of the compound was confirmed with 1 H NMR and 13 C NMR spectroscopy, LR, and HR-MS techniques and with single-crystal X-ray diffractometry.The tricyclic triol (formally a hemiacetal) was transformed into 6b-nitrohexahydro-2H-1,3,5-trioxacyclopenta[cd]-pentalene-2,4,6-triyl trinitrate by reaction with 98 % HNO 3 . Some explosive properties of this compound were determined including: friction and impact sensitivity, activation energy, detonation velocity, heat of combustion in an oxygen atmosphere and enthalpy of formation. The nitrate ester is a powerful explosive with performance close to that of pentaerythritol tetranitrate (PETN).

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