2400 series 2 combustion analyzer

All manipulations were performed under an N₂ atmosphere in a VAC atmospheres glovebox or using standard Schlenk techniques. The ligand H₄dobpdc was purchased from Hangzhou Trylead Chemical Technology Co. N,N-dimethylacetamide (DMA) and methanol were dried over 3-Å molecular sieves and then degassed via three successive freeze-pump-thaw cycles. Toluene and N,N-dimethylformamide (DMF) were deoxygenated by purging with Ar for 1 h and dried using a commercial solvent purification system designed by JC Meyer Solvent Systems. All other reagents were purchased from commercial sources and used without further purification. Adsorption isotherms for CO₂ and N₂ were obtained by volumetric methods using a Micromeritics ASAP 2020 gas adsorption analyzer. All gases were 99.998% purity or higher. The CO₂ isotherm recorded at 25 °C was measured using a circulating water bath. The N₂ isotherm at 77 K was measured using a liquid nitrogen bath. Laboratory powder X-ray diffraction patterns were collected using a Bruker AXS D8 Advance diffractometer using CuKα radiation (λ = 1.5418 Å). Elemental analysis (H, C, and N) was conducted using a Perkin Elmer 2400 Series II combustion analyzer. Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) was conducting using an ICP Optima 7000 DV instrument.

The compound 4,4′-dihydroxy-(1,1′-biphenyl)-3,3′-dicarboxylic acid (H₄dobpdc) was either obtained from Combi-Blocks and purified by recrystallization from a 3:1 (v:v) acetone:water mixture or was synthesized as previously reported.³² All other reagents and solvents were obtained from commercial suppliers at reagent grade purity or higher and were used without further purification. Ultra-high purity (99.999%) He and N₂ and research grade (99.998%) CO₂ were used for all adsorption experiments. Elemental analyses were conducted at the Microanalytical Laboratory of the University of California, Berkeley, using a PerkinElmer 2400 Series II combustion analyzer.