화학공학소재연구정보센터
Inorganic Chemistry, Vol.43, No.7, 2261-2266, 2004
A new route for preparing coordination polymers from hydrothermal reactions involving in situ ligand synthesis
The coordination chemistry of inorganic cobalt salt and the organic ligands H(4)bbh (=benzene-1,2,4,5-bihydrazide) and H(3)bcbh (=benzene-4-carboxylate-1,2-bihydrazide) generated through the in situ hydrothermal acylate reaction of H(4)bta (=benzene-1,2,4,5-tetracarboxylic acid) and H(3)btc (=benzene-1,2,4-tricarboxylic acid) with hydrazine hydrate, respectively, has been investigated. Three new coordination polymers were prepared and fully characterized by infrared spectroscopy, elemental analysis, and single-crystal X-ray diffraction, The compound [Co(mu(3)-H(2)bbh)(phen)](n) (1) (triclinic space group P(1) over bar with a = 9.762(4) Angstrom, b = 10.169(4) Angstrom, c = 11.143(4) Angstrom, alpha = 80.96(3)degrees, beta = 64.49(3)degrees, gamma = 71.88(3)degrees, Z= 2) was synthesized from the reaction of CoCl2.6H(2)O, H(4)bta (=benzene-1,2,4,5-tetracarboxylic acid), N2H4.H2O, phen (=1,10-phenanthroline) and H2O, and consists of one-dimensional doublechains. [CO(mu(4)-H(2)bbh)(H2O)(2)](n) (2) (monoclinic space group P2(1)/c with a = 6.8687(5) Angstrom, b = 7.5943(6) Angstrom, c = 10.0401(6) Angstrom, beta = 95.250(4)degrees, Z = 2) was generated by the combination of CoCl2.6H(2)O, H(4)bta, N2H4.H2O, and H2O. It adopts a three-dimensional structural motif in the solid state with channels consisting of 20-numbered rings. [Co(mu(3)-Hbcbh)(bpy)](n) (3) (monoclinic space group Cc with a = 9,9464(13) Angstrom, b = 23.685(5) Angstrom, c = 7.9491 (16) Angstrom, beta = 117.677(13)degrees, Z = 4) was obtained from the mixture of CoCl2.6H(2)O, N2H4.H2O, H(3)btc (=benzene-1,2,4-tricarboxylic acid), bpy (=2,2'-dipyridyl), and H2O, and features a two-dimensional plane, The results of magnetic research indicate that there exist antiferromagnetic interactions between Co centers in both compounds 1 and 2.