| The chemistry of organoantimony compounds derived from carboxylates have been an active area of research for more than two decades, not only for the striking structural possibilities ranging from discrete monomeric structures to supramolecular assemblies, but also for the biological importance in antimicrobial properties as well as antitumor activities. As a result of the deep research of organoantimony compounds, some can well inhibit the growth of cancer cell, even more active one hundred times than cis-platinum derivatives in antitumour activity. So it becomes a research hotspot on the relationship of the structure-effect of organoantimony compounds. With the development of X-diffraction technique and its application in structure chemistry, organoantimony chemistry boomed unprecedentedly. Based on these X-ray diffraction data, scientists are able to have a more intuitionistic observation and deeper perspective of the organoantimony compounds as well as to find more potential applications of the organoantimony compounds.Therefore studying these compounds has more meanings in synthesis, characterization, pharmaceutics and other theory and application researches other than in structure. Out of above considerations, we carried out a series of research on syntheses and characterization of organoantimony derivatives from carboxylate ligands. The structures and formations of compounds were determined by elemental analysis, IR, 1H NMR spectra and X-ray single crystal diffraction,and the processes and mechanisms of the reactions were presumed. The main contributions of the thesis are as follows:1. Preparations of a series of organoantimony halides: triphenylantimony dichloride, triphenylantimony dibromide,μ-O-chlorotriphenylantimony and they have been determined by X-ray single crystal diffraction.2. Synthesize a series of organoantimony compounds by reaction of triphenylantimony dichloride with mono-carboxylic acid in different stoichiometry. And eleven compounds have been obtained. Their spectral properties and molecular structures have been studied carefully with elemental, IR analyses, NMR (1H, 13C) spectroscopy and single crystal X-ray diffraction. The results show that mono-carboxylic acid, especially with electronegative atom, easily reacts with triphenylantimony dichloride to give mono-organoantimony compounds. Interestingly, hydrogen atoms on phenyl ring of compounds and hetero atoms can easily form hydrogen bonds as C-H…Cl, C-H…F, C-H…Br, C-H…O, C-H…πand so on, and through these hydrogen bonds dimer, 1D chain, 2D net and 3D framework supermolecules are formed.3. Synthesize a series of organoantimony compounds by reaction of triphenylantimony dibromide with mono-carboxylic acid. And four compounds have been obtained. Their spectral properties and molecular structures have been studied carefully with elemental, IR analyses, NMR (1H, 13C) spectroscopy and single crystal X-ray diffraction. The results show that it is difficult for carboxylic oxygen atoms to coordinate to antimony atoms, because of existence of four phenyl rings to make space crowded. But mono-carboxylic acid with stronger acidity coordinating to antimony atoms gives most mono-organoantimony compounds and few compounds with cheliform coordination modes.4. Synthesize a series of organoantimony compounds by reaction ofμ-O-chlorotriphenylantimony with mono-carboxylic acid. And two compounds have been obtained. Their spectral properties and molecular structures have been studied carefully with elemental, IR analyses, NMR (1H, 13C) spectroscopy and single crystal X-ray diffraction. The results show that mono-carboxylic acid with stronger acidity easily reacts withμ-O-chlorotriphenylantimony. Through hydrogen bonds C-H…Cl, C-H…O and so on, 1D chain is formed.5. Investigations on the reactions of phenylantimony halide with dualistic carboxylic acid. And nine compounds have been obtained. Their spectral properties and molecular structures have been studied carefully with elemental, IR analyses, NMR (1H, 13C) spectroscopy and four of them have been determined by X-ray single crystal diffraction. The results show that multi-antimony nuclears compounds couldn't be obtained easily, but di-antimony nuclears triphenyl organoantimony compounds, mono-antimony nuclear tetraphenyl organoantimony compounds and di-antimony nuclears, with different coordination modes, tetraphenyl organoantimony compounds have been obtained, and the results wouldn't change along with the change of molar rate.6. We synthesized two kinds of oxime and do investigations on the reactions of triphenylantimony dichloride with oxime. And eight compounds have been obtained. Their spectral properties and molecular structures have been studied carefully with elemental, IR analyses, NMR (1H, 13C) spectroscopy and two of them have been determined by X-ray single crystal diffraction. The results show that oxime exhibits mono-coordiantion to react with thiphenylantimony dichloride to give mono-nuclear organoantimony compounds with five coordinated antomony.7. The antitumor activity was assayed after X-ray single crystal diffraction. Inhibition ratio for human hepatocellular carcinoma cells (Bel-7402), human gastric carcinoma cells (BGC-823), human immature granulocyte leukemia cells (HL-60), human nasopharyngeal carcinoma cells (KB) of the compounds have been tested at 1.25μM/L, 2.5μM/L, 5μM/L, 10μM/L, 20μM/L. The results show that the antitumor activity was affected by the concentration of the compounds, but not on multiple. Simultaneously, most coumpounds hardly exhibit inhibition for human immature granulocyte leukemia cells (HL-60) even facilitate the growth of them.It is worth noting that through these structural characterizations, we found that weak interaction, hydrogen bonding may benefit the construction of 1D chain, 2D layer or 3D structures of the organoantimony compounds. And under a certain condition, some structure can recognize special molecules and processed self-assemblement to form supramolecules. The structural information may throw new light in the structure-effect relationship of the organoantimony compounds.
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