We report the syntheses and crystal structures of novel porous assemblies of coordination complexes (PACs) with/without guest molecules, α-[Cu(A)2(py)4] (α-PAC-2-A (A = PF6, BF4, CF3SO3, and CH3SO3); py = pyridine), γ-{[Cu(PF6)2(py)4]·2guest} (γ-PAC-2-PF6 ⊃ 2guest (guest = acetone and py)), γ-{[Cu(BF4)2(py)4]·2acetone} (γ-PAC-2-BF4 ⊃ 2acetone), and β-{[Cu(CH3SO3)2(py)4]·2.67H2O} (β-PAC-2-CH3SO3 ⊃ 2.67H2O). The single-crystal X-ray diffraction analyses of α-PAC-2-A show that α-PAC-2-A have dense packing structures, in which anions of the discrete coordination complexes form weak hydrogen-bonding and anion–π interactions. In contrast, γ-PAC-2-PF6 ⊃ 2guest, γ-PAC-2-BF4 ⊃ 2acetone, and β-PAC-2-CH3SO3 ⊃ 2.67H2O form guest-including structures with coordination environments around the CuII atoms similar to the α-forms. The vapour adsorption measurements for MeCN and acetone in α-PAC-2-A suggest that the adsorption associated with structural transformations is induced by weak Lewis-base PF6− and BF4− anions covered only with fluorine atoms, which weaken the host–host interactions.
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