A series of rationally designed pentanuclear clusters with D3 symmetry have been synthesized and structurally characterized. The complexes were of formula [Ni5L6]XnY4−n·mH2O [2–431, X = NO3, Y = OH, n = 1, m = 3 (5); X = Br, n = 4, m= 4 (6); X = I, n = 4, m= 0 (7)], where the ligand [L, (Z)-1,2-di(1H-benzoimidazol-2-yl)ethenol] was produced in situ under hydrothermal conditions. SEM images proved that the crystals of compounds 2–4, 6 and 7 were hollow tetragonal or hexagonal prisms, and a nucleation–dissolution–recrystallization mechanism was investigated. Complexes 3 and 4 demonstrated chirality from CD spectra. Magnetic susceptibility measurements of 4–7 showed the occurrence of antiferromagnetic interactions, and the all negative J values fitted of the variable-temperature magnetic susceptibility data applying the spin matrix method confirmed the overall antiferromagnetic exchange in the clusters.
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