Dissertation
Dissertation > Mathematical sciences and chemical > Chemistry > Organic Chemistry > Elements in organic compounds > The first III group elements, organic compounds > Boron compounds, aluminum organic compounds

Synthesis, characterization and crystal structure of two hydroxy benzoic acid esters

Author ZhangJing
Tutor LiuZhiHong
School Shaanxi Normal University
Course Inorganic Chemistry
Keywords Borates Inorganic-organic hybrid Synthesis Crystal structure Photoluminescent properties
CLC O627.31
Type Master's thesis
Year 2011
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Borate materials have been a research field with rapid expansion in the past decades, mainly because of their rich structural chemistry and important practical applications. However, in comparison with inorganic borates, relatively less work has been carried out on the synthesis, crystal structure and application of inorganic-organic hybrid borates.In this thesis, eight new inorginic-organic hybrid boric acid esters have been synthesized by using the hydrothermal and solution methods with the use of the boric acid, dihydroxybenzoic acid, and alkali metal salts/organic amine/and transition metal complex as the materials. They were further characterized by elemental analysis, FT-IR, PXRD and TG-DTA. The crystal structures of four compounds have been determined by single X-ray diffractometer. The photoluminescent properties have also investigated. This study is of significance to enrich the types and structure chemistry of inorginic-organic hybrid compounds containing boron.Six alkali metal dihydroxybenzoic acid borates, Li[BO4(C7H4O)2], Na[BO4(C7H4O)2], K[BO4(C7H4O)2](2,3- and 2,4-), Rb[BO4(C7H4O)2] and Cs[BO4(C7H4O)2], were synthesized by using aqueous solution methods. The bis(2,3-dihydroxy benzoic acid) potassium borate crystallizes in the orthorhombic space group Pbcn (60) with unit cell dimensions a=12.3740(13) A, b=13.1903(12) A, c=16.0476(18) A, a=90°,β=90°,γ=90°, Z=8, V=2619.24(47) A3. The bis(2, 4-dihydroxy benzoic acid) potassium borate crystallizes in the orthorhombic space group Pbca with unit cell dimensions a=9.210(3) A, b=15.866(5) A, c=19.853(7) A,α=90°,β=90°,γ=90°, Z=8, V= 2901.2(17) A3.Two new inorginic-organic hybrid boric acid esters, [CH3CH2OH]0.5[CH3NH3][B04(C7H402)2]·1.5H20 and [Fe(C12H8N2)3][BO4(C7H4O2)2]2-2H2O, have been synthesised by using aqueous solution methods. The [CH3CH2OH]o5[CH3NH3][B04(C7H4O2)2]·1.5H20 belongs to the P2(l)/c monoclinic space group, with the following unit cell parameter:a= 15.1705(6) A, b=8.0996(3) A, c= 15.9099(5) A, a=90°,β=98.017(3)°,γ=90°, Z=4, V=1935.82(12) A3. The [Fe(C12H8N2)3][BO4(C7H4O2)2]2·2H2O belongs to the C2/c monoclinic space group, with the following unit cell parameter:a=25.4508(13) A, b=15.3060(5) A, c=18.0048(10) A,α=90°,β=127.56(1)°,γ=90°, Z=4, V= 5559.77(3421) A3.Three other types of crystals, Zn(C3H3N2)2, (C6H6O2)8·(C6H12N2)8 and Cd3(C10H8N2)2(C9H3O6)2·H2O, have been synthesised by using the hydrothermal and solution methods. The Zn(C3H3N2)2 belongs to the I41cd tetragonal space group, with the following unit cell parameter:a=23.48827(15) A, b=23.48827(15) A, c=12.44821(15) A,α=90°,β=90°,β=90°, Z=16, V=6867.67(11) A3. The Cd3(C10H8N2)2(C9H3O6)2·H2O belongs to the C2/c monoclinic space group, with the following unit cell parameter:a=23.700(5) A, b=11.6876(11) A, c=20.563(5) A,α=90°,β=135.16(4)°,γ=90°, Z=4, V=4016.5(14) A3. The (C6H6O2)8·(C6H12N2)8 belongs to the P21/c monoclinic space group, with the following unit cell parameter:a=9.4882(5) A, b=23.7390(11) A, c=11.2532(6) A,α=90°,β=113.335(6)°,γ=90°, Z=4, V=2327.3(2) A3.

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