Based on a new family of NiII cubane-like clusters, this work addresses current challenges in synthesis, analysis and dynamics of single-molecule-magnet (SMM) systems. Investigation of various synthetic routes and desorption-sorption processes yielded series of isomorphous compounds: [Ni4L4(CH3OH)4]·xsolv, [Ni4L4(CH3OH)4] and [Ni4L4]. In order to analyze these deceivingly simple materials, several analytical and quantum mechanical methods had to be used. This revealed materials with mixed lattice solvents, statistical disorder of the solvent, and disordered [Ni4L4] cores, what offered an insight into risks of the self-assembly process and interconversion dynamics of the investigated NiII family. These findings also allowed structural-magnetic relationships to be established, and the outcomes were exploited in two turns: in first, effect of the coordinated and lattice solvent on the magnetic properties was examined, and in second, magnetic properties were used to facilitate crystal structure determination.
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