Three compounds have been isolated from solvothermal reactions of a transition metal(II) (Ni(II), Co(II)) with N,N-bis(phosphonomethyl)aminoacetic acid [(HO2CCH2)N(CH2PO3H2)2] (H5L), namely [NH3(CH2)3NH3](NH4)4[Ni(L)(H2O)]2 (1), (H3O)3[Ni(L)(H2O)2]·4H2O (2) and (H3O)[Co(H2L)(H2O)2]·2H2O (3). These compounds were characterized by single crystal and powder X-ray diffraction, infrared spectroscopy, thermal analysis, elemental analysis, fluorescent spectroscopy and magnetic measurements. The structure of compound 1 is composed of binuclear [Ni2O6N2]n4− units, which are further interconnected into a 3D supramolecular network by hydrogen bonds. Compounds 2 and 3 are both mononuclear and consist of similar octahedral [MO5N] units. A 1D dendritic water chain is formed by hydrogen bond interactions in the supramolecular network of compound 2. Compounds 1 and 2 show ferromagnetic properties, while weak antiferromagnetic properties are observed in compound 3. Compounds 1 and 2 also display fluorescent emission excited at 235 nm.
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