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Oligo- and polyMOFs based on DMOF-1 adopt distinct isomeric structures governed by the flexibility, length, and number of repeat units of tethering groups between terephthalate units. 

Multitopic phosphine ligands combined with Rh(i) or Ir(i) nodes assemble into low-valent metal–organic frameworks (LVMOFs) with a two-dimensional (2D) topology and catalytic activity. 

Metal-Organic Frameworks (MOFs) are the subject of intense research focus due to their potential applications in gas storage and separation, biomedicine, energy, and catalysis. Recently, low-valent MOFs (LVMOFs) have been explored for their potential use as heterogeneous catalysts, and multitopic phosphine linkers have been shown as a useful building block for the formation of LVMOFs. However, the synthesis of LVMOFs using phosphine linkers requires conditions that are distinct from the majority of the MOF synthetic literature, including the exclusion of air and water and the use of unconventional modulators and solvents, making it somewhat more challenging to access these materials. This work serves as a general tutorial for the synthesis of LVMOFs with phosphine linkers, including information on: 1) judicious choice of metal precursor, modulator, and solvent; 2) experimental procedures, air-free techniques, and required equipment; 3) proper storage and handling of the resultant LVMOFs; and 4) useful characterization methods for these materials. The intention of this report is to lower the barrier and make more accessible this new subfield of MOF research and facilitate advancements toward novel catalytic materials.