期刊
CRYSTALS
卷 12, 期 4, 页码 -出版社
MDPI
DOI: 10.3390/cryst12040443
关键词
molybdenum; hydrazone; solvates; complex salts; co-crystals; coordination polymer; chloranilate; o-vanillin azine
资金
- Croatian Science Foundation [IP-2016-06-4221]
Complex salts and co-crystals were synthesized by solution-based and mechanochemical methods. Stability of the complex salts could be reinforced by the incorporation of an azine compound. Solvent-mediated transformations led to different ligand replacement reactions.
Complex salts [1H]X and [1H](XA)(0.5)center dot 2MeOH, and co-crystals [1H]X center dot 0.5VA (X = chloride or bromide, XA = chloranilate or bromanilate, VA = o-vanillin azine), comprising [MoO2(HL)(MeOH)](+) ([1H](+)) cation (H2L = 3-methoxysalicylaldehyde isonicotinoyl hydrazone), were prepared either by solution-based synthesis or by mechanochemical synthesis. Whereas [1H]X salts were extremely sensitive to humidity, their stability could be reinforced by the azine incorporation into the complex network. Solvent-mediated transformations of [1H]X led to methanol co-ligand replacement and afforded complexes [MoO2(HL)X] (2Cl center dot MeOH, 2Cl, and 2Br center dot 0.5MeCN). However, solvates [1H](XA)(0.5)center dot 2MeOH, under the same conditions, gave stable complexes [1H](XA)(0.5) in which methanol remained coordinated. The differences in the assembly's behavior were attributed to the packing arrangements, the relative orientation of cations and anions, and interactions between them. Polymorph [MoO2(L)(MeOH)] (1), not attainable by other routes, was the only product when compounds [MoO2(HL)X] were treated with a weak base at low temperatures. Tetranuclear [MoO2(L)](4) and polynuclear [MoO2(L)](n) (2) supramolecular isomers, concomitantly crystallized when the reaction was conducted solvothermally. All of the complexes were characterized using X-ray diffraction methods (SCXRD and PXRD), spectroscopic methods (ATR-IR and solution-state and solid-state MAS NMR), and elemental and thermal analyses. The cytotoxicity of the different types of compounds against THP-1 and HepG2 cells was also evaluated.
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