X pert pro diffractometer

IR spectra were recorded neat at 25 °C using a Perkin Elmer Spectrum GX series with FT system spectrophotometer using the ATR device. ¹³C-CPMAS spectra were recorded on a Bruker Avance DPX-400 (101 MHz). The following conditions were applied: spectral width 30.242 kHz, acquisition time 33.8 ms, contact time 2000 ms, rotation rate 8 kHz, relaxation delay 5 s, and up to 256 scans for each spectrum were collected. Room temperature X-ray powder diffraction data were collected on a PAN Analytical X′Pert PRO diffractometer with Cu Kα1 radiation (λ = 1.5405 Å, 45 kV, 40 mA) or on a D8 Focus Bruker AXS instrument using Cu Kα1 radiation (λ = 1.542 Å, 35 kV, 25 mA). Texture analysis of H₂Mf(HpOXA)₂ was performed in an ASAP-2050 Xtended Pressure Sorption Analyzer of Micromeritics. Prior to measurement, vacuum sample activation was performed for 10 min to 150 °C, the measuring temperature was 75.15 K and it was maintained through a liquid nitrogen dewar. The gas used for the analysis was N₂ (gas). For measurements, 40.8 mg of the activated mass sample were taken. DSC and TG measurements were performed in a Q2000 equipment and a Thermobalance Q5000 IR, respectively, of TA instruments. In both cases, approximately 3.0–5.0 mg of sample was used and a gradient of 5.00 °C/min from room temperature to 350 °C under air flux of 25 mL/min in an open (TG) or pin-holed panels (DSC).