Asap 2020m physisorption analyzer

Reagents were commercially available and used without further purification except otherwise stated. The monomer 4-pyC₂H₃ was distilled to remove polymerization inhibitor hydroquinone before use. ESI-MS was obtained using a Shimadzu LCMS-2010A mass spectrometer, for which samples were digested by sonication in a mixture of hydrochloric acid and MeOH after removal of the residual monomers by sublimation under vacuum. Elemental analyses (EA) were conducted using an Elementar Vario EL analyzer using guest-free samples (with a little water adsorbed from air). IR spectra were recorded on a Bruker TENSOR 27 FT-IR spectrometer in the 400–4,000 cm⁻¹ region with KBr pellets. ¹H NMR and ¹³C NMR spectra were recorded on a Bruker AVANCE III 400 MHz NMR spectrometer. Chemical shifts were quoted in p.p.m. referenced to the appropriate solvent peak or 0.0 p.p.m. for tetramethylsilicane. PXRD patterns were collected on a Bruker D8-Advance diffractometer with Cu Kα radiation and a LynxEye detector. Thermogravimetry analyses were performed on a TA Q50 system under N₂ at a heating rate of 5 °C min. N₂ sorption isotherms were measured by a Micromeritics ASAP 2020M physisorption analyzer.

Elemental analyses were performed using a Vario EL elemental analyser. The FT-IR (KBr pellet) spectra were recorded in the range of 400–4,000 cm⁻¹ on a Bruker TENSOR 27 FT-IR spectrometer. Thermogravimetric analyses were carried out using a TA Instruments Q50 thermogravimetric analyser under N₂ at a rate of 10 °C/min. PXRD patterns were recorded on a Bruker D8-Advance diffractometer using Cu Kα radiation and a LynxEye detector at room temperature except otherwise stated. Gas sorption isotherms were measured on a volumetric adsorption apparatus (Micromeritics ASAP 2020 M Physisorption Analyzer). Ultrahigh-purity-grade (purity>99.999%) N₂, O₂ and Ar gases were used in all adsorption measurements. As-synthesized samples were degassed under high vacuum at 493 K for 3 h before measurement. Temperatures were maintained by liquid nitrogen.