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Chinese Journal of
Magnetic Resonance
(Quarterly, Started in 1983)
Editor-in-Chief: LIU Mai-li
Sponsored by
Wuhan Institute of Physics and Mathematics, CAS
Published by Science Press, China
Distribution Code: 38-313
Pricing: ¥ 80.00 per year
Current Issue
       Volume 6 Issue 4, 05 December 1989 Previous Issue   Next Issue
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    THE STUDY ON NMR AND CONFIGURATIONS OF α-HALOCINNAMOYL PIPERIDINES
    Hua Yuxin, Zhang Jianjin, Wang Shuyu, Shen Qifeng, Jiau Ding
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 393-398.  
    Abstract     HTML ( )   PDF(364KB)
    1H-NMR and 13C NMR of six pairs of α-halocinnamoyt piperidines with substituted aromatic ring are reported. By comparing the 1H-NMR chemical shift and peak shape of α-H on piperidine ring at various temperatures, the effect of configuration and conformation arc discussed. The configurations of α-halocinnamoyl piperidines were assigned based on chemical shifts and peak shape of a-H on piperidine ring. The correctness of this deduction is also con-firmed by the coupling constants 3JCCCH of the carbon of carbonyl group and β-proton on the olefinic bond on the 13C-NMR.
    AN ESR STUDY FOR THE PHOTOCHEMICAL HYDROGEN-ABSTRACTION REACTION OF FATTY AMINES WITH NITROFLUORENONES
    Zhou Jianwei, Chen Dewen, Xu Guangzhi
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 399-406.  
    Abstract     HTML ( )   PDF(534KB)
    The active radicals produced in the photochemical hydrogen-abstraction reaction between five Tatty amines and five nitrofluorenones have been studied by means of spin trapping-ESR technique. The results show that the njtro-gen-centered free radicals arc formed in a first priority when there are N-H atoms and α-C-H atoms in amines, and the Carbon-centered free radical is founed only when there is no hydrogen linked to the nitrogen atom (N-H) in amine, as in the case of ceaction for the teitiary amines.
    DETERMINATION OF THE STRUCTURES OF SIDE PRODUCTS OF MORPHOLINE BY 2D NMR
    Yue Shufan, Ma Libin
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 407-412.  
    Abstract     HTML ( )   PDF(296KB)
    In this paper, the structures of two side products of morpholine were determined by 1H-NMR, inverted gated decoupling 13C-NMR, H-H COSY, C-H COSY, helcronuclear 2DJ. and long-range C-H COSY.
    ESR STUDY ON THE O-BENZOIC SULFIMIDE COMPLEXES OF Mn (Ⅱ) AND Cu (Ⅱ)
    Chen Deyu, Xu Yuanzhi, Wang Yongyao, Wang Shuyuan
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 413-422.  
    Abstract     HTML ( )   PDF(675KB)
    In this paper, the ESR spectra of o-Bcnzoic sulfimide complexes of Mn (Ⅱ) and Cu examined it was observed that at low temperature in pyridinc and at room,emperature after adsorbed by zeolite the ESR spectra of Mn (Ⅱ) conplex exhibit unusual doublet. These spectra may be explained in tenns of a spinhamiltonium by considering unly the M=1/2 ←→M=-1/2 transitions, and theoccurence of forbidden △m=±1 transitions. The ESR spectra of Cu (Ⅱ) complexes in various solvents and at different temperatures were also studied, the bonding characteristic of complexes and their coordinating behaviours in various solutions are discussed.
    13C-NMR STUDY OF SUBSTITUENT EFFECTS IN 3 (OR 4)-X-BENZENECARBOXIMIDATES
    Wu Meiyu, Yong Zhonggen, Shi Yaozeng, Jiang Weiping, Lu Wanfang, Hu Hongwen
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 423-430.  
    Abstract     HTML ( )   PDF(451KB)
    The 13C-NMR spectra of three ethyl 3 (or 4)-x-benzenecarboximidates (1) and eight ethyl N-cyanomethyl-3 (or 4)-x-benzenecarboximidates (2) were determined. All 13C chemical shifts were assigned. The substituent chemical shifts (SCS) of -C-OCH2CH3=NCH2CN was obtained. Correlations of the 13C chemical shifts of aromatic carbons with the appropriate substituent chemical shifts (SCS) for monosubstituted benzenes show nonadditivity at C-2, 6 in compounds lb-g and 2b-e, at C-1 in compounds 1h-j and 2f-h. Dual subslituent parameter correlations of the 13C chemical shifts were also performed in this paper.
    NMR ECHO SEQUENCE IN THE CENTRAL TRANSITION OF SPIN-3/2 QUADRUPOLAR SYSTEMS IN POWDERED SAMPLES
    Li Gengying, Wu Xuewen
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 431-438.  
    Abstract     HTML ( )   PDF(471KB)
    A pulse sequence 45x°-t1-90±y°-t2 is proposed for the spin echo of I=3/2 spin systems in powder samples, which is confirmed theoretically and experimentally. It can effectively refocuse the magnetization of the central transition in spin-3/2 quadrupole nuclear systems. And the numerical calculated excitation bandwidth of the echo sequence is also given.
    THE DNMR SPECTRA OF Cd、Hg、Pb AND La-DTPA COMPLEXES
    Zhang Jianbin, Song Ruifang, Qiu Zuwen
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 439-444.  
    Abstract     HTML ( )   PDF(385KB)
    Reported here arc intramolecular process DNMR spectra of some diamagnctic complexes which were synthesized by the reaction of Cd、Hg、Pb and La with DTPA (dicthylcnelriamine pentaacetate), respectively. The rate constants and other thermodynamic parameters were obtained by complete line shape analysis. The intra molecular exchange process is also discussed in this paper, it was found that the activation energies of Cd、Hg and Pb-DTPA complexes are related to the size of the metal ions. The NMR spectrum of La-DTPA shows a double AB type in room temperature, but a single coalescent AB type as the temperature increases. it indicates that the △⇌Λ conversion and the N atom inversion are slow processes within the NMR lime scale.
    ESR STUDY FOR THE INFLUENCE OF THE DISCHARGING TUBE DIAMETER AND MOISTURE CONTENT UPON THE ACTIVE RADICALS PRODUCED IN MICROWAVE DISCHARGE OF FATTY ETHER
    Wang Wending, Chen Dewen, Xu Guangzhi
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 445-451.  
    Abstract     HTML ( )   PDF(473KB)
    By means of the spin trapping-ESR technique, the influence of the tube diameters and moisture content in the sample on the radicals produced in the microwave discharge of fatty ether at low pressure has been studied systematically. The results show that:the smaller the diameter of the tube, the faster the formative speed of carbon black, as well as the shorter the lifetime of H atom. With the increase of moisture content, the extent of carbonization becomes more serious. According to the mechanism of discharge, the reasons of the carbonization are discussed.
    THE EFFECTS OF THE DIELECTRIC PROPERTY OF SAMPLES ON ST-ESR SPECTRA
    Xiang Bosong, Chen Binhuan, Wan Qian
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 453-460.  
    Abstract     HTML ( )   PDF(529KB)
    We observed the difference between the ST-ESR spectra caused by the difference of the dielectric properties of the samples directly. Then we tried to eliminate these differences and the error of the measured τC caused by them by using the "power compensation" method. We also studied the effects of the dielectric property of the sample in the whole range in which the ST-ESR spectra are sensitive to τC. The results show that the error of the measured τC is large and it is necessary to eliminate the error by using the "power compensation" method when we make use of the ST-ESR method.
    CARBON-13 CP/MAS NMR STUDY OF THE NYLON 6 POLYMORPHS AND DYNAMICS
    Dehua Wang, Jianzhi Hu, Xin Yan, Guoxi Wang, Baogong Qian
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 461-468.  
    Abstract     HTML ( )   PDF(508KB)
    C-13 CP/MAS spectra of nylon 6 were obtained on MSL-400 spectrometer. It was found that the ω carbon
    α β γ δ ω-[CO-CH2-CH2-CH2-CH2-CH2-NH]-n, nylon 6,shows two peaks in the solid state. They are designated as ω1 and ω2 which originate from different crystalline components. The two peaks coalesced in solution spectrum of the same sample. It gives the evidence of coexistence of different crystalline regions in solid nylon 6. In the solid state the ω2 peak is 2.2 ppm upfield from the ω1 peak.
    A series of CP/MAS spectra of nylon 6 was measured by varying the contact time to investigate the dynamic behavior. A SIMPLEX nonlinear least square optimization algorithm was applied to calculate the cross-polarization rates TIS and T1PH. The dynamic parameters of solid nylon 6 were calculated according to Ngai formalism.
    NMR STUDY ON DETERMINATION OF THE FOUR STEREOISOMERS OF SOMAN
    Miao Zhenchun, Du Zehan
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 469-472.  
    Abstract     HTML ( )   PDF(224KB)
    The dctermina of four of soman has been studied by NMR chiral shift reagents Eu (TFC)3 and Eu (MFC)3. It was found that the complexes of soman with Eu (HFC)3 in C6D6 show larger 19F NMR shift difference, which can been used for the simultaneous qantitaivc determination of the four stcrcoisomcrs of soman.
    THE EFFECT OF PHOTOFRIN Ⅱ ON THE PHOTOSENSITJZATION DAMAGE OF DNA 31P NMR INVESTIGATION
    Chen Fengyin
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 473-478.  
    Abstract     HTML ( )   PDF(367KB)
    The variation of conformation of DNA during its photosensitization damage rocess induced by the interaction of photofrin Ⅱ was studied by 31P NMR spectroscopy. The degree of damage and the possible mode of complexation are discussed.
    BIEXPONENTIAL CHARACTERISTIC OF THE RELAXATION PROCESS OF 13C-1H SYSTEM
    Zhao Huansui, Li Cuiping
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 479-482.  
    Abstract     HTML ( )   PDF(254KB)
    In this paper, the mutual effect of relaxation processes of 13C and 1H in a CHn group is studied theoretically and experimentally.
    THE STUDY ON 1H NMR, UV AND CIS-TRANS CONFIGURATION OF α-SUBSTITUTED CINNAMAMIDES
    Li Anliang, Liu Weiqin, Chen Suming
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 483-488.  
    Abstract     HTML ( )   PDF(361KB)
    The 1H NMR and UV spectral data of 24 cinnamamides whose α-position was substituted with 13 types of groups are reported. The chemical shifts of β-H were calculated with empirical equation. The result shows that comparison of experimental values with calculated values can be used for concluding cis-or trans-configuration of these compounds. The chemical shifts of phenyl pretons can also give evidence for configuration. For the pairs of these compounds, the chemical shifts of protons on amide nitrogen and the UV spectra arc helpful for assigning configuration.
    THE 13C-NMR STUDIES OF ALKYL、PHENYL AND FIVE-MEMBERED HETERORING TIN COMPOUNDS
    Yang Zhenyun, Wang Shihuo, Liu Xiumei, Yan Shenggang
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 489-494.  
    Abstract     HTML ( )   PDF(354KB)
    The 13C NMR spectra were recorded for eighteen organotin (Ⅳ) compounds containing alkyl, phenyl, atyl, five-membercd hclcrorings and other polar groups. All the 13C spectral lines were asslgned. The Sn-C bond property in alkyl and phenyl us cempouds, and the influcncc of polar substitucnts on C-1 δ values are Jiscassed.The magntudes and orders of carbon-tin coupling constants nJC-Sn and the ationship between nJC-Sn and nJC-Sn were also investigated.
    STUDIES ON CARBON-13 NUCLEAR MAGNETIC ROSONANCE SPECTRA OF 1-NICOTINYL-4-ARYLTHIOSEMICARBAZIDES AND 3-(3-PYRIDYL)-4-ARYL-l, 2, 4-TRIAZOLINE-5-THIONES
    Zhang Ziyi, Liu Peiqi, Zhang Lixue
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 495-500.  
    Abstract     HTML ( )   PDF(386KB)
    The carbon-13 nuclear magnetic resonance spectra of eight new compounds including 1-nicotinyl-4-phenylthiosemicarbazide and 3-(3-pyridyl)-4-phcnyl-1, 2, 4-triazoline-5-thione were recorded. The chemical shifts of various carbon resonances have been assigned on the basis of the application of proton broad band decoupling and off resonance decoupling techniques, the comparison of signal intensity, the calculation based on substituent effect, and comparison with the chemical shifts of the model compounds. The difference between thiosemicarbazides and 1, 2, 4-triazoline-5-thiones in 13C NMR was discussed. In addition, the data of the effect of substituent of hydrazide on the C-13 chemical shifts in 3-monosubstituted pyridines were obtained.
    NMR STUDY OF TERT-BUTYL PHENOL COMPOUNDS
    Chen Xingcai, Liu Ning
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 501-508.  
    Abstract     HTML ( )   PDF(451KB)
    1H and 13C chemical shifts of tert-butyl phenol compounds were determined by NMR. 13C-1H one bond and long-range coupling constants (nJCOH). 13C-1H gcminal coupling constants over the C-OH chain (2JCOH) and 13C-31P coupling constants (nJCP) in It tert-butyl phenol compounds were obtained.
    The coupling constants between aromatic hydrogen and aromatic carbon and the coupling constants between aromatic hydrogen (carbon) and aliphatic carbon (hydrogen) directly attached to aromatic are discussed. Induced and stcric effects on the coupling constants are also discussed.
    THE MECHANISM OF COORDINATION OF ISOPROPYL (DIALKOXY PHOSPHOROYL) ACETATE WITH LANTHANUM NITRATE BY NMR STUDY
    Chen Chaohuan, Shi Liping, Ye Weizhun, Yan Jinying
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 509-512.  
    Abstract     HTML ( )   PDF(266KB)
    The mechanism of coordination of isopropyl (diisopropoxy phosphoroyl) acetate (Ⅰ) and isopropyi (dibutoxy phosphoroyl) acetate (Ⅱ) with lanthanum nitrate has been investigated. Results show that the La3+ ion coordinates at P=O and C=O for the coordination compound Ⅰ and at P=O for the Ⅱ. Their coordination constants K were determined in CDCl3 solvent, they are K=0.4 for Ⅰ and K=0.04 for Ⅱ.
    WATER SUPPRESSION IN in VIVO 1H NMR SPECTROSCOPY
    Zhang Weiguo
    Chinese Journal of Magnetic Resonance, 1989, 6(4): 513-516.  
    Abstract     HTML ( )   PDF(257KB)
    Water-suppression is introduced into OSIRIS localized in Vivo spectroscopic technique. By combining presaturation and selective detection episodes, a suppression factor of > 1000 could be readily obtained. The technique could therefore be used to detect and study metabolites in Vivo.