The hydro/solvothermal reactions of Cu(I)/Cu(II) salt, NaN3, and acetonitrile in water or methanol yield two noninterpenetrated supramolecular networks containing 1D hexagonal and square nanochannels, {[Cu(Mtta)]center dot 0.17H(2)O}(n) (1) and its pseudopolymorph [Cu(Mtta)](n) (2) (Mtta = 5-methyl tetrazolate), involving ligand in-situ formation by cycloaddition of nitriles and azides. The copper(1) centers in both complexes are all bridged by Mtta ligands, forming the different shapes of the cavity. 1 exhibits an unprecedented uniform (8, 3) topological metal network, whereas 2 is a 3-connected (8(2)10) metal net.
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