Two polymorphic 2D-coordination polymers of composition [ZnL(HCO2)]∞ were synthesized from an in situ generated ligand [PO2(NH4Py)2]− (L−). The ligand L− was generated by a facile metal-assisted P–N bond hydrolysis reaction from the corresponding phosphonium salt 1, [P(NH4Py)4]Cl, or from the neutral phosphoric triamide 2, [PO(NH4Py)3]. The de-solvated sample of the polymer [ZnL(HCO2)]∞ features polar micropores and shows a type I isotherm for CO2sorption whereas a type II behaviour was observed for N2. The vapour sorption isotherm of the de-solvated sample of [ZnL(HCO2)]∞ shows preferential adsorption of water vapour over aliphatic alcohols.
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