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In this thesis, classic Keggin type polyoxometalate inorganic component and organic amine rigid ligands for organic components, design, synthesis and characterization of a series of organic - inorganic supramolecular assembly of such multi-metal polyoxometalate synthesis process conditions, reaction law and main influencing factors, and to study the relationship between the structure and properties of the compounds. Synthesized by the hydrothermal method, by controlling the reaction conditions and the conversion reaction of the kind of raw materials and the reaction amount, synthetic three Keggin type polyoxometallate as the main organic - inorganic supramolecular compound. And by means of single crystal X-ray diffraction pattern, TGA, electrochemical thorough study of the structural characteristics of the compound. Under hydrothermal conditions, classic Keggin type polyoxometalate basic building unit V atom as a central heteroatom, by introducing rigid organic molecules, design, synthetic rare supramolecular compound (C 3 N 2 H 5 ) 3 (VMo 12 O 40 ) · 2.5H 2 O (1), belong to the triclinic P-1 space group, unit cell parameters a = 12.337 (5) (A | °), b = 12.346 (5) (A | °), c = 17.937 (5) (A | °), α = 105.67 (5) °, β = 91.865 (5) °, γ = 114.15 (5) °, V = 2368.2 (15 ) (A | °) from 3 sup> and Z = 1. Compound 1, Keggin VMo 12 O 40 ] 3 - sup> through molecular bonding interaction between the anion are connected together through more connected to the strong hydrogen bonding interactions with the organic molecules and the water molecules to form a multidimensional supramolecular compound. 2 classic Keggin type polyoxometallate in hot water under the conditions for the synthesis of the main body, by introducing the rigidity of the 2,2 '-bipy organic molecule for the modification unit, the design, synthesis interesting supramolecular compound (2 , 2'-bipy) [H 2 PMo 12 O 40 ] · H 2 O (2), belongs to the monoclinic system, P2 (1) / n space group, unit cell parameters a = 11.504 (A | °), b = 12.089 (A | °), c = 17.258 (A | °), α = 90 ( 5) °, β = 103.183 (5) °, γ = 90 (5) °, V = 2336.9 (16) (A | °) 3 sup> and Z = 4. In compound 2, the Keggin type heteropoly anion and an organic ligand by hydrogen bonding, the formation of the supramolecular clusters ,2,2-bipy molecular bond force and the role of hydrogen bonds showing a distorted shape. Under hydrothermal conditions, with a compound similar to the basic building unit is also based on the classic Keggin type polyoxometalate, 4,4 '-bipy by changing rigid introduced body as an organic component, design, synthetic the the interesting supramolecular compound (4,4 '-bipy) 2 [HPMo 12 from O 40 ] (3), belong to the triclinic Department, P-1 space group, unit cell parameters a = 11.504 (A | °), b = 12.089 (A | °), c = 17.258 (A | °), α = 90 (5) °, β = 103.183 (5) °, γ = 90 (5) °, V = 2336.9 (16) (A | °) 3 sup> and Z = 4. In compound 3, Keggin [the PMo 12 O 40 ] 3 - sup> anion clusters connected by intermolecular forces together with the are connected by hydrogen bonds between the organic molecules, forming a supramolecular assembly.
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