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Synthesis, Crystal Structure and Vibrational Spectrum of Inorganic-organic Transition Metal Borate and Vanadate

Author: LinDan
Tutor: ZhuLiXia
School: Xi'an University of Electronic Science and Technology
Course: Applied Chemistry
Keywords: inorganic-organic hybrid borate vanadate crystal structure vibrational spectrum
CLC: O611.3
Type: Master's thesis
Year: 2009
Downloads: 88
Quote: 2
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Abstract


In this paper, the synthesis of a novel hydrated transition metal tetraborate and two novel inorganic-organic hybrid borate and vanadate were studied. All these crystals have been determined by single crystal X-ray diffraction and further characterized by FT-IR spectrum and Raman spectrum.（1）A novel hydrated transition metal tetraborate NH4[Co（NH3）5（H2O）[B4O5（OH）4]2·6H2O was synthesized. It crystallizes in the orthorhombic system, space group Pnma, a=1.2901（2）nm, b=1.6817（3）nm, c=1.1368（2）nm,α=90°,β=90°,γ=90°, V=2.4742（8） nm3, Z=4, Dc=1.801g/cm3. The single-crystal X-ray diffraction analysis reveals that this compound consists of one distinct coordinated cobalt atom [Co（NH3）5（H2O）]3+, [B4O5（OH）4]2- group, NH4+ group and water molecules. All the units are further connected by hydrogen bonding interactions to form a 3-D framework structure.（2） A novel inorganic-organic hybrid borate [Cu（en）2B（OH）3][B4O5（OH）4][B（OH）3] was synthesized under hydrothermal conditions. It crystallizes in the monoclinic system, space group P2（1）/c, a=1.2779（2）nm, b=1.0166（15）nm, c=1.5019（2）nm,α=90°,β=90.301（2）°,γ=90°, V=1.9396（5）nm3, Z=4, Dc=1.708g/cm3. The single crystal X-ray diffraction analysis gives the existence of [B4O5（OH）4]2- cluster, [Cu（en）2B（OH）3]2+ cation and B（OH）3 group in the compound unit. The B（OH）3 group provides hydrogen bonds to connect all the basic units to construct an interesting framework structure.（3） A novel inorganic-organic hybrid vanadate [Ni2（py）5]V4O12（H2O）3 was prepared under hydrothermal conditions. It crystallizes in the orthorhombic system, space group, Pca2（1）, a=1.7444（3）nm, b=1.1437（16）nm, c=1.7441（3）nm,α=90°,β=90°,γ=90°,V=3.4797（9）nm3, Z=4, Dc=1.838g/cm3. The single crystal X-ray diffraction analysis reveals four [VO4] distorted tetrahedrons and two differently nickel-centered coordinated distorted octahedrons. All the units are further connected by hydrogen bonds to construct a novel framework structure.（4） The rules of synthesis of hydrated inorganic-organic hybrid borate and vanadate were studied. By analysing the experimental data and condition, a conclusion was made that the appropriate pH is between 8.0 to 9.0 and the appropriate temperature is between 130°C to 140°C when synthesizing hydrated inorganic-organic hybrid borate and vanadate.

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CLC: > Mathematical sciences and chemical > Chemistry > Inorganic Chemistry > Chemical elements and inorganic compounds > Nature
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