Accupyc 1340 gas pycnometer

The true density of amorphous FLU and SOL powders was determined using AccuPyc 1340 Gas pycnometer (Micromeritics, Norcross, GA, USA). Each sample was filled in a 10.0 cm³ sample cup and the weight of each sample was noted. A true density measurement was then carried out at an equilibration rate of 0.0050 psig·min⁻¹ using a set of 10 purges. Calibration was performed prior to each run.

All of the reactions were carried out in the air. Ammonium 4-amino-3,5-dinitropyrazolate monohydrate [37 (link)] was prepared following procedures found in the literature. Other commercial reagents and solvents were obtained from commercial providers and used without further purification. ¹H NMR and ¹³C NMR spectra were recorded at 25 °C on a Bruker 400 MHz and 125 MHz, respectively, and TMS as the internal standard. Chemical shifts were reported in parts per million (ppm). The onset decomposition temperature was measured using a TA Instruments DSC25 differential scanning calorimeter at a heating rate of 10 °C min⁻¹ under a dry nitrogen atmosphere. Infrared spectra (IR) were obtained on a PerkinElmer Spectrum BX FT-IR instrument equipped with an ATR unit at 25 °C. Elemental analyses of C/H/N were investigated on a Thermo Scientific Flash 2000 Elemental Analyzer. A BAM fallhammer and friction tester tested impact and friction sensitivities. Densities were determined at room temperature by employing a Micromeritics AccuPyc 1340 gas pycnometer. The crystal structures were produced employing Mercury 2021.1.0 software.

¹H and ¹³C NMR spectra were tested using a Bruker 400 MHz spectrometer (400 and 100 MHz, respectively) in d-DMSO. Chemical shifts are reported as δ values relative to internal standard d-DMSO (δ 2.50 for ¹H NMR and 39.52 for ¹³C NMR). Infrared spectra (IR) were obtained on a PerkinElmer Spectrum BX FT-IR instrument equipped with an ATR unit at 25 °C. Elemental analyses of C/H/N/I were investigated on a Vario EL III Analyzer. The onset decomposition temperature was measured using a TA Instruments DSC25 differential scanning calorimeter at a heating rate of 5 °C min⁻¹ under dry nitrogen atmosphere. Densities were determined at room temperature by a Micromeritics AccuPyc 1340 gas pycnometer.
Fully iodinated monocyclic compound precursors 3,4,5-triiodo-1H-pyrazole (TIP), 2,4,5-triiodo-1H-imidazole (TIM), and 2,3,4,5-tetraiodo-1H-pyrrole (TIPL) were synthesized as references [16 ,20 ,21 (link)].