Synthesis, Crystal Structure and Water-induced Reversible Crystal-to-amorphous Transformation Proper

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A novel NiII complex [{Ni(IBG)(4,4’-bipy)(H2O)2}·3H2O]n 1 (H2IBG = isophthaloylbisglycine and 4,4’-bipy = 4,4’-bipyridine) has been synthesized and characterized by singlecrystal X-ray diffraction, elemental analysis, IR spectra and thermogravimetric analysis. It crystallizes in monoclinic, space group P2/c with a = 15.5420(7), b = 22.4344(1), c = 8.3455(5), β = 101.538(3)o, V = 2670.1(7)3, Z = 4, C22H32N4NiO13, Mr = 619.23, Dc = 1.443 g/cm3, F(000) = 1296.0, μ(MoKα) = 0.750 mm-1, the final R = 0.0570 and wR = 0.1445 for 2296 observed reflections with I > 2σ(I). In the structure, the NiII metal center is coordinated in an octahedral environment arranged by two water molecules, two carboxylate oxygen atoms and two nitrogen atoms from two 4,4’-bipy ligands. Thermal decomposition and powder X-ray diffraction results indicate that the transformation from the crystal form, [{Ni(IBG)(4,4’-bipy)(H2O)2}·3H2O]n, to the amorphous powder, Ni(IBG)(4,4’-bipy)(H2O)2, is reversible, so the latter form may be utilized as an absorbing agent for water and water vapor. A novel NiII complex [{Ni (IBG) (4,4’-bipy) (H2O) 2} · 3H2O] n 1 (H2IBG = isophthaloylbisglycine and 4,4’-bipy = 4,4’-bipyridine) and characterized by singlecrystal X-ray diffraction, elemental analysis, IR spectra and thermogravimetric analysis. It crystallizes in monoclinic space group P2 / c with a = 15.5420 (7), b = 22.4344 (1), c = 8.3455 , β = 101.538 (3) o, V = 2670.1 (7) 3, Z = 4, C22H32N4NiO13, Mr = 619.23, Dc = 1.443 g / cm3, F (000) = 1296.0, μ (MoKα) = 0.750 mm- 1, the final R = 0.0570 and wR = 0.1445 for 2296 observed reflections with I> 2σ (I). In the structure, the NiII metal center is coordinated in an octahedral environment arranged by two water molecules, two carboxylate oxygen atoms and two nitrogen atoms from two 4,4’-bipy ligands. Thermal decomposition and powder X-ray diffraction results indicated that the transformation from the crystal form, [{Ni (IBG) (4,4’-bipy) (H2O) 2} ] n, to the amorphous powder, Ni (IBG) (4,4’-bipy) (H2O) 2, is reversible, so th e latter form may be utilized as an absorbing agent for water and water vapor.
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