Hydrothermal Synthesis And Characterization Of Structure Of Organic-inorganic Hybrid Compounds Containing Polyoxotungstates And Metal-oxalate

This thesis reported two unprecedented polyoxotungstates and a new organic-inorganichybrid compound containing metal-oxalate by hydrothermal techniques, namely changingreaction conditions and reaction materials:Compound [Fe(phen)3]2[P W9V3O40]·4H2O(1)crystallizes in the triclinic space group P-1with a = 12.173(5)?, b = 13.623(5) ?, c = 14.609(5) ?, α = 104.854(5) o, β = 109.553(5) o,γ = 93.477(5) o, V = 2177.9(14) ?3 , Z = 1.Compound [Fe(phen)3]2 [PWⅥ8VⅤ3VⅣ3O43]·4.5H20(2) crystallizes in the monoclinicspace group C2/c with a = 30.1709(15) ? , b = 13.9783(6) ?, c = 24.7535(14) ?, β =99.967(2) o,V = 10281.9(9) ?3, Z = 4.Compound Fe2(phen)2(C2O4) 2(3)crystallizes in the monoclinic space group P2(1) with a= 9.248(5) ?, b = 13.580(5) ?, c = 10.207(5)?, β = 94.357(5) o , V = 1278.2(10) ?3,Z = 2.The structures of the three compounds were determined by single crystal X-raydiffraction, and we groped for the factor of influencing their structure.The single crystal X-ray diffraction analysis reveals that compound 1 consists ofpolyoxotungstate anion [P W9V3O40]6-and two coordinated cations [Fe(phen)3]3+.view along a,b and c, anions and cations arrayed in linetype, there are six cations around every anion. Thereexist weak π-π packing interactions between neighboring two cations.Compound 2 consists of polyoxotungstate anion[PWⅥ8VⅤ3VⅣ3O43]6-containing two Vcapped and two coordinated cations [Fe(phen)3]3+. Cations arrange in line and pack into 1Dchain via weak π-π interactions, and anions link into 1D chain via H-bonding interactions.View along a, anions in bc plane link into anionic layer via H-bonding interactions. Namelysupramolecular compound was formed by π-π and H-bonding interactions.Compound 3 is supramolecular coordination polymer, Fe(II) ions were coordinatedwith phen and oxalic, and bridged into 1D zigzag chain via oxalic, such 1D chain werefurther linked into 2D layer by π-π interaction of phen, oxalic chains among layers bend alongdifferent directions, and supramolecular compound was formed via hydrogen bondingamong layers, namely hydrogen atoms of phen and oxygen atoms of oxalic.In these experiment, we found that the ratio of materials, reaction temperature, reactiontimes and pH value have importantly influenced on the final product, and pH is the crucialfactor. Three compounds were characterized by elemental analysis, IR, TGA-DTA.