| As the novel functional molecular materials, the design and assembly of coordination polymers have been of great interests due to their interesting topologies and potential applications in separation, gas storage, optical, magnetics, molecule identification and catalyst fields. The synthesis of coordination polymers have obtained great success for the past several decades. Large numbers of coordination polymers, which have novel architecture and particular properties, emerge in endlessly. Especially the detection and study of in situ ligand synthesis bring more mulriple synthesis methods and more abundant structure aboat coordination compounds. Hydro(solvo) in situ ligand synthesis is of great interests in coordination chemistry as an effective strategy in synthesizing coordination compounds. Lots of novel coordination complexes involving hydro(solvo)thermal in situ synthesized ligands were synthesized successfully,which could not be easy or be prepared by ordinary methods. In this paper, we have synthesized seven coordination compounds and one organic compound through hydrothermal in situ acylation reaction. We aslo try our best to study the synthesis, structure and properties of these compounds.1. The coordination polymer [Cu(PTH)](1) with H2ph(=phthalic acid), hydrazine hydrate, and CuBr have been synthesized through hydrothermal syntheses method by in situ acylation reaction. constructed from the dinuclear Cu(I) units by PTH The new coordination polymer 1 is 2-dimension layer structure with the briging(μ3-) ligand PTH(=phthalhydrazidate). In the compound 1, the crystallographically unique Cu(I) center exhibits a special T-type geometry. Finally, all the 2-D layers are self-assembled together via the offset face-to-faceπ···πstacking interactions between the PTHs, forming a 3-D supramolecular network. The compound 2, deriving from in situ reaction of phthalic aicd and hydrazine hydrate directly, shows some characteristics in participating in compound. We sum up its characteristics from the compounds we obtained. We have characterized them by elemental analysis, IR spectroscopy, UV-Vis-spectroscopy, TG, powder-XRD, XPS and 1H-NMR ect. We studied their fluorescence, especially for polymer 1, the time-dependent density functional theory (TD-DFT) calculations were carried out on the excited electronic states.2. We synthesized three compound(3-5) through in situ acylate reaction in hydrothermal condition. The polymer [Pb2(PTH)4(phen)2]·H2O(3) was obtained by the in situ acylate reaction of phthalic acid and hydrazine hydrate self-assembling with plumbum acetate. The compound 3 is 1-dimention chian with Pb-O bonds(2.965, 2.985?). The 1-dimentionnal ribboned compound [Pb(2,3-PDH)2](4) (2,3-PDH=2,3-pyridine hydrazidate) was synthesized through in situ acylate reaction of 2,3-pyridine dicarboxylic acid and hydrazine hydrate self-assembling with plumbum hydroxide.The The 1-dimention ribbons are linked into 3-D supramolecular network by hydrogen bonds. The compound [Pb(3,4-PDH)2](5)(3,4-PDH=3,4-pyridine hydrazidate), which are generated through the in situ hydrothermal acylate reaction of 3,4-pyridine dicarboxylic acid and hydrazine hydrate, with plumbum hydroxide has been investigated. The compound 5 is 3-dimention network with bridging ligand(μ3-) 3,4-PDH, and the hydrogen bonds andπ···πstacking interactions enable the network more stable. We aslo sum up the modes of ligands in componds 4 and 5, and study on the effect factors influencing the structure of the coordination polymers 3-5, such as pH and ligands etc. All of them were characterized by IR, UV-Vis-spectroscopy, TG, elemental and fluorescence analysis.3. The coordination chemistry of the organic ligand 2,3-PDH(=2,3-pyridine hydrazidate), which is generated through the in situ hydrothermal acylate reaction of 2,3-pyridine dicarboxylic acid and hydrazine hydrate, with manganese, cobalt and zinc salt has been investigated. Three new coordination compounds [Mn(2,3-PDH)2(H2O)2](6), [Co(2,3-PDH)2(H2O)2] (7) and [Zn(2,3-PDH)2(H2O)2] (8) have been synthesized with different metal salts under the same experimentation conditions through hydrothermal reaction. Despite that the single-crystals of compounds 7 and 8 are unsuitable for X-ray diffraction analysis, the IR spectrum, TG and UV-Vis spectrum indicate the compounds 7 and 8 are isomorphic with compound 6. The compound[Mn(2,3-PDH)2(H2O)2](6) shows mononuclear structure, which extends 3-dimentional supramolecular network by hydrogen bonds andπ···πstacking interactions. The coordination mode of 2,3-PDH in compound 6 is different from in compound 4. We characterized them with IR, UV-Vis-spectroscopy, TG, elemental and fluorescence analysis.In conclusion, comparing the syntheses and the structure of all the compounds, the nature of metal ion, the kind of ligands and pH value all effect on the finally products, while the definitive effect factor for different reaction is dissimilar.
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