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 H4bbh (=benzene-1,2,4,5-bihydrazide) and H3bcbh (=benzene-4-carboxylate-1,2-bihydrazide) generated through the in situ hydrothermal acylate reaction of H4bta (=benzene-1,2,4,5-tetracarboxylic acid) and H3btc (=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(μ3-H2bbh)(phen)]n (1) (triclinic space group P1 with a = 9.762(4) A, b = 10.169(4) A, c = 11.143(4) A, α = 80.96(3)°, β = 64.49(3)°, γ = 71.88(3)°, Z = 2) was synthesized from the reaction of CoCl2·6H2O, H4bta (=benzene-1,2,4,5-tetracarboxylic acid), N2H4·H2O, phen (=1,10-phenanthroline) and H2O, and consists of one-dimensional double-chains. [Co(μ4-H2bbh)(H2O)2]n (2) (monoclinic space group P2(1)/c with a = 6.8687(5) A, b = 7.5943(6) A, c = 10.0401(6) A, β = 95....