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HYDROGEN BONDING INTERACTION IN COBALTIC SUPRAMOLECULAR COMPLEXES—STUDIED 59 Co NMR AND MOLECULAR MODELLING
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ZHOU Ping, AU-YANG S C F
Chinese Journal of Magnetic Resonance, 2004, 21(1): 1-15.
The hydrogen bonding interactions in a series of cobaltic supramolecular complexes [12] aneN4 [Co(CN)6 ], [18] aneN6 [Co(CN)6 ], [24]aneN8 [Co(CN)6 ], [16] aneN4 [Co(CN)6 ], [24] aneN6[ Co(CN)6 ] and [32] aneN8 [Co(CN)6] were studies and found to be closely related to the molecular conformations in the aqueous solution. Such interactions caused the 59 Co chemical shifts to move towards upfield, and the quadrupolar interaction to change as well. It was observed in this study that stronger hydrogen bonding resulted in larger upfield shift of the 59 Co chemical shifts and higher quadrupolar interaction in the cobaltic supramolecular complexes. On the other hand, larger supramolecular sizes resulted in longer molecular rotational correlation time τc and shorter 59 Co longitudinal relaxation time (T 1 ). In summary, 59 Co NMR proves to be an ideal probe to investigate the second sphere or weak interaction in the cobaltic supramolecular complexes in addition to the small molecules.
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L-BAND THREE DIMENSIONAL ESR IMAGING SYSTEM(Ⅳ)——System Configuration and Performance Features
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WU Ke, CONG Jian-Bo, ZHANG Qing-Jun, XIAN Hong, WANG Chang-Zhen, SUN Cun-Pu, ZHENG Ying-Guang, XU Jing, DONG Feng-Xia, CHEN Er-Zhong, XU Yu-Shu
Chinese Journal of Magnetic Resonance, 2004, 21(1): 33-40.
Configuration and performance features of the newly developed L-band three-dimensional ESR imaging system were introduced. The main components of the ESRI system include a set of L-band ESR spectrometer, the three dimensional gradient magnetic field system and the imaging reconstruction software. The microwave system worked at the frequency of 1.05 GHz with more than 500 mW microwave power. The phase-locking receiver was set to work at 100 kHz modulation frequency with a modulation amplitude of more than 0.5 mT. Receiver gain could be set up to 1×10+6 and time constant was adjustable from 0.02 ms to 1 s. The sample cavity was a threelooptwogap reentrance one which had an unloaded Q- value of more than 1 000 and had a cylindrical sensitive volume of 2 cm in diameter and 3 cm in length. The maximum gradient strength could be 2 mT/cm with spatial linearity of better than 5% in all three dimensions. Field stability was about 10-5 . Main magnet strength and the scanning range of the magnetic field were 1.6~96 mT and 0.2~16 mT respectively. Data system worked on a 12-bit A/D card for data acquisition. Three channels of 8-bit D/A converter were used for gradient control. Spectrum processing functions included integration, base line correction, resolution enhancement, spectrum deconvolution and noise filtering. Imaging functions included two and three dimensional imaging reconstruction, 2D image display of spin intensity isograms, 3D image display of contour and computed tomography. The preliminary results of imaging of biological equivalent samples, such as large volume solution phantoms, suggested that the present ESRI system was capable of imaging biological samples in combination with spin labeling techniques.
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INTERACTIONS OF WATER-SOLUBLE POLYMERS WITH SODIUM DODECYL SULFATE IN AQUEOUS SOLUTION STUDIED BY 1 H NMR
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FENG Yang, FANG Xiao-Wen, MAO Shi-Zhen, ZHAO Sui, YUAN Han-Zhen, YU Jia-Yong, DU You-Ru
Chinese Journal of Magnetic Resonance, 2004, 21(1): 49-55.
Aqueous solutions of sodium dodecyl sulfate (SDS) at various concentrations in 2 g/L polyvinylpyrrolidone (PVP) and 2 g/L polyvinyl alcohol (PVA), respectively, were studied by 1 H NMR. Two-dimensional nuclear Overhauser enhancement spectroscopy (NOESY) experiments show that SDS starts to micellize at a concentration of 2.5 mmol/L, with PVP solubilized in the interior of the micelles. At
SDS concentrations lower than 2.5 mmol/L, no significant interaction could be detected. Spin-spin relaxation measurements support this conclusion. The interaction between PVA and SDS was hardly detected.
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SYNTHESIS OF PHOSPHORYLATED AMINOPHENOLS AND DIHYDROXYBENZENES BY THE ATHERON-TODD REACTION AND THEIR NMR CHARACTERIZATION
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CHEN Xiao-Lan, YU You-Zhu, LU Jian-Sha, CHEN-Li, QU Ling-Bo, LIAO Xin-Cheng, ZhAO Yu-Fen
Chinese Journal of Magnetic Resonance, 2004, 21(1): 87-91.
The Atheron-Todd reaction has been applied extensively to the synthesis of phosphates and phosphoroamidates. In this study, aminophenols and dihydroxybenzenes were phosphoylated by a modified Atheron-Todd procedure, in which DEPH and etrachloromethane were added to the mixed solution of phenol, triethylamine and dioxane and the mixed solution of phenols, triethylamine and dioxane, respectively. The target phosphates were obtained with good yields. Their structures were elucidated by NMR and ESI-MS.
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A NMR STUDY OF METOLAZONE
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DONG Jian-Jun, WU Ming-Jian, ZHANG Hai-Yan, FU Jing-Guo, CHEN Tao, ZHAO Tian-Zeng
Chinese Journal of Magnetic Resonance, 2004, 21(1): 93-97.
Metolazone is a well-known quinazolinone diuretic widely used for the treatment of congestive heart failure and high blood pressure. Metolazone was first synthesized in 1967 with its first detailed pharmacological evaluation done in 1969. Previous results only reported part of its 1 H NMR data, and the detailed elucidation is yet to be performed. In this paper, using a combination of 1D and 2D NMR
techniques, the 1 H and 13 C NMR spectra of metolazone were completely assigned and analyzed. The characteristics of its NMR data were also discussed.