The title compound, 1,2-bis-(p-nitro-phenylsulfonamido)-4,5-dinitrobenzene, was synthesized and characterized by elemental analysis, IR and 1H NMR. A pale yellow prism crystal of C23H26N8O13S2 (Mr = 686.64) was obtained in DMF solution and determined by single-crystal X-ray diffraction method. It crystallizes in triclinic system, space group P1 with a = 10.346(4), b = 12.210(5), c = 12.976(5) , α = 108.220(8), β = 99.482(4), γ = 95.490(4)°, V = 1516.7(10) 3, Z = 2, Dc = 1.504 g/cm3, F(000) = 712, μ = 0.254, Mr = 686.64, the final R = 0.0561 and wR = 0.1487. One sulfonamido group of the title compound is deprotoned and forms N(3)=C(13). The crystal involves N,N-dimethylamine from the decomposition of DMF and the proton is transferred to N,N- dimethylamine. It is a strong proof for the characterization of deprotoned recognition compound by X-ray single-crystal structure.
A Maleamide bridged carbazole receptor was designed and synthesized, the interactions between the receptor and anions, such as Ac-, H2PO4-, OH-, F-, Cl-, Br- and I- in DMSO were investigated by UV-Vis spectroscopy and 1H NMR titration. The results of UV-Vis spectral studies indicate that interactions existed between receptor and anions, which induced remarkable color changes. The 1H NMR titration indicated amide moiety of the receptor was deprontonated first when a small quantity of anions such as Ac-, H2PO4-, F- were added; however, the carbazole N―H was gradually deprontonated upon the addition of anions.
The title compound, N-(1?-H-pyrrol-2?-ylcarbonyl)-5-amino-1,10-phenanthroline, was synthesized by the reaction of α-pyrrolyl carbonyl chloride and 5-amino-1,10-phenanthroline in pyridine. Determined by X-ray structure analysis, it crystallizes in triclinic system, space group P 1 with the following crystallographic data: C20H21N5O3, Mr = 379.42, a = 7.8559(4), b = 9.1681(6), c = 14.6818(9), α = 73.254(10), β = 88.938(15), γ = 68.080(10)o, V = 934.66(10) 3, Z = 2, F(000) = 400, Dc = 1.348 g/cm3 and μ = 0.094 mm-1. The final R = 0.0680 and wR = 0.1419 for 2142 observed reflections with I > 2σ(I), and R = 0.1084 and wR = 0.1643 for all reflections. Two aromatic ring planes (pyrrole and phenanthroline rings) are connected by the amide plane. Two different types of intermolecular hydrogen bonds, O-H…N and N-H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 3-D supramolecule.
A simple colorimetric acetate ion receptor based on 3-methoxysalicylaldehyde-4'-nitrophenyl-hydrazone was synthesized in an ethanol solution through one step,and characterized by 1H NMR and elemental analyses.Its anion-binding ability was examined by UV-Vis absorption spectroscopy in DMSO(dimethyl sulfoxide).The result shows that the compound has a high affinity for and a high selectivity toward acetate ions,and also an advantage of 'naked-eye' recognition of color changing from yellow to purple.
Two multidentate ligands 2,9-di[6'-(2″-hydroxyl-3″-methoxyphenyl)-n-2',5'-diazahexyl]-1,10-phenanthroline(LA)and 2,9-di(6'-α-phenol-n-2',5'-diazahexyl)-1,10-phenanthroline(LB)were synthesized and fully characterized.Protonation of the ligands and the stability of the complexes of the ligands with divalent metal ions were investigated.The trinuclear metal complexes [Cu(Ⅱ)and Zn(Ⅱ)] of the ligands were studied,as catalysts,for the transphosphorylation of the RNA-model substrate 2-hydroxypropyl-p-nitrophenyl phosphate(HPNP).The second-order rate constants of HPNP-hydrolysis catalyzed by M3L and M3LH-1 were obtained,which indicated that Zn3LBH-1 was the most efficient catalyst among them.The proposed mechanisms included the activation of the substrate via binding to the metal ions and intramolecular nucleophilic attack by the deprotonated C2-hydroxyl of HPNP.
