From the simple hydrothermal reactions of metal salts, organodicarboxylic acids and hydrazine hydrate sometimes in the presence of 1,10-phenanthroline (phen), a series of monoacylhydrazidate-containing complexes including three Pb(II) coordination polymers as 1-D chained [Pb(2)(PTH)(4)(phen)(2)].H(2)O (PTH = phthalhydrazidate) , 1-D ribboned [Pb(2,3-PDH)(2)] (2,3-PDH = pyridine-2,3-dicarboxylhydrazidate) and 3-D grid-like [Pb(3,4-PDH)(2)] (3,4-PDH = pyridine-3,4-dicarboxylhydrazidate) as well as several transition metal complexes as 2-D layered [Cu(PTH)] , mononuclear [M(2,3-PDH)(2)(H(2)O)(2)] (M = Mn , Co and Zn ) and mononuclear [Mn(H(2)O(6))] (PTH)(2).4H(2)O were obtained. The monoacylhydrazidate ligands were synthesised from hydrothermal in situ acylation reactions between organodicarboxylic acids and hydrazine hydrate. All of the title compounds were characterized by CHN analysis, IR analysis and TG analysis, and compounds were characterized by X-ray single-crystal diffraction. The fluorescence properties of compounds and with the PTH ligand were investigated. TDDFT calculations were carried out on the excited electronic states of compound in order to understand the emission mechanism.