Detailed Characterization of Metal-Organic Frameworks

¹H NMR spectra were collected on a Bruker AMX 300 MHz spectrometer and referenced to residual dimethyl sulfoxide (δ = 2.50 ppm). Powder X-ray diffraction (PXRD) patterns were collected with a laboratory Bruker AXS D8 Advance diffractometer with Cu Kα radiation (λ = 1.5418 Å) or at the Advanced Photon Source with synchrotron radiation (λ = 0.45399 Å), as specified in the figure captions. Additional details for synchrotron PXRD experiments under controlled atmospheres are given in Supporting Information Section 15. All synthetic manipulations were carried out under air unless noted otherwise. All solvents and reagents, including diamines, were purchased from commercial sources and used without further purification unless otherwise noted. The linker H₄dobpdc was purchased from Hangzhou Trylead Chemical Technology Co. The linker H₄dotpdc was prepared according to the literature procedure.^{53 (link)} The metal–organic frameworks Mg₂(dobpdc),^{51 (link)} Mn₂(dobpdc),^{52 (link)} Ni₂(dobpdc),^{52 (link)} Co₂(dobpdc),^{52 (link)} Zn₂(dobpdc),^{61 (link)} and Mg₂(dotpdc)^{53 (link)} were prepared according to literature procedures (Supporting Information Section 1). Ultrahigh purity (>99.998%) gases were used for all adsorption experiments.