The divalent nickel isothiocyanate coordination polymer [Ni(NCS)2(dpa)2] (1) has been prepared in high yield via the hydrothermal combination of Ni(SCN)2 with the kinked tethering ligand 4,4′‐dipyridylamine (dpa), and characterized via single crystal X‐ray diffraction, infrared spectroscopy and elemental and thermal analysis. 1 manifests offset stacked 2‐D (4,4)‐topology layered motifs organized into 3‐D via interlamellar supramolecular N–H···S hydrogen bonding. Hydrothermal reaction of CuCl2·2H2O, NaSCN, and dpa afforded the copper (I) thiocyanate coordination polymer [Cu2(SCN)2(dpa)] (2), whose single crystal structure revealed unprecedented 1‐D [Cu2(SCN)2] zig‐zag staircase motifs constructed via connection of the Cu2S2 “stair steps” at their adjacent sides via μ3‐1,1,3‐SCN anions. The 3‐D structure of 2 is propagated by covalent linkage of each [Cu2(SCN)2] staircase to four others through dipodal dpa tethering ligands, enhanced by N–H···S and C–H···S supramolecular interactions to two other staircases.
The title salt, C13H15N2+·C10H5O8−, manifests hydrogen‐bonded one‐dimensional chains parallel to the crystallographic b‐axis direction, consisting of alternating monoprotonated 1,3‐di‐4‐pyridylpropane molecules and singly deprotonated pyromellitic acid anions. The chains interact via C—H⋯O hydrogen bonds to form two‐dimensional layers parallel to the bc plane, which in turn stack to establish the three‐dimensional crystal structure.
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