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Two new hybrid materials, (C4H14N2)[MII(H2O)6](SO4)2·4H2O (MII: Co (I), Ni (II)), have been synthesised by slow evaporation method at room temperature and crystallographically characterized. They crystallise isotypically in the monoclinic system, space group P21/n, with the following unit-cell parameters a = 9.2285(3), b = 11.3333(4), c = 10.6693(4) Å, β = 109.004(2)°, Z = 2 and V = 1055.07(6) Å3 for I and a = 9.2127(2), b = 11.3182(2), c = 10.6434(2) Å, β = 109.094(1)°, Z = 2 and V = 1048.74(4) Å3 for II. The structure of the two supramolecular compounds consists of metallic cation octahedrally coordinated to six water molecules, sulfate anions, 1,4-butanediammonium cation and water molecules linked together via two types of hydrogen bonds, O–H?O and N–H?O. The two compounds are not stable at room temperature and their partial dehydration depends on the humidity of the environment. The thermal decomposition of precursors, studied by thermogravimetric analysis (TG) and temperature-dependent X-ray diffraction (TDXD), shows successive intermediate hydrates and crystalline anhydrous compounds upon dehydration. 相似文献