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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
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       Volume 4 Issue 4, 05 December 1987 Previous Issue   Next Issue
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    ESR STUDY OF THE VO (H2O)42+ COMPLEX SUPPORTED ON Y TYPE ZEOLITES
    Xu Yuanzhi, Wang Li
    Chinese Journal of Magnetic Resonance, 1987, 4(4): 289-296.  
    Abstract     HTML ( )   PDF(4057KB)
    Two kinds of ESR spectra measured from VO2+ supported on Y-type zeolites after treatments at various roast temperatures (200~700℃) are reported. Results suggest that the VO(H20)42+ ion in the cage of zeolite has two kinds of probable structures. With the increase of roast temperature, the structure (Ⅰ) turned to structure (Ⅱ) gradually. When the roast temperature was increased over 600℃, the structure (Ⅰ) disappeared entirely, and the parameter A of structure (Ⅱ) decreased gradually. This implies that the delocalization of the unpaired electron was enhanced. At last, this unpaired electron was lost and the V4+ was oxidized to V5+. The bond parameter and reducible energy level were calculated from the spectral parameters.
    THE 13C-NMR STUDIES OF GIBBERIC ACID AND SOME DERIVATIVES
    Ling Yangzhi, J. R. Hanson
    Chinese Journal of Magnetic Resonance, 1987, 4(4): 297-302.  
    Abstract     HTML ( )   PDF(3493KB)
    The 13C-NMR spectra of some gibberic acid derivatives were assigned by using JMOD and DEPT technique in combination with deuterium labelling experiment and some chemical transformation reactions
    ESR STUDY ON ACTIVE RADICALS PRODUCED IN MICROWAVE DISCHARGE OF ALKANE
    Wang Wending, Chen Dewen, Xu Guangzhi
    Chinese Journal of Magnetic Resonance, 1987, 4(4): 303-310.  
    Abstract     HTML ( )   PDF(4242KB)
    The active radicals produced in microwave discharge of ten alkanes were studied systematically by combination of spin trapping technique with ESR. The results show that (1) R· and H· are produced in the above systems and can be trapped by PBN, (2) the ratio of [PBN-R]·/[PBN-H]· varies with the distance between PBN and the discharge cavity.
    THE STUDIES OF THE FRAMEWORK OF X-TYPE ZEOLITES BY 29SiMASNMR
    Yao Shijie, Hu Jiehah, Quo Hefu, Qiu Jianqing
    Chinese Journal of Magnetic Resonance, 1987, 4(4): 311-316.  
    Abstract     HTML ( )   PDF(3594KB)
    The 29Si NMR behaviour of the framework in divalent metal ion exchanged X-type zeolites was investigated, and the effects of exchange level, dehydration and the type of exchange ions(e.g.Cd2+,Cu2+,Co2+,Mn2+,Pb2+)on the 29SiMASNMR spectra were discussed. It was found that at the exchange level of about 85%, the zeolite remained in a special state which might be related to a special catalytic activity at this ion exchange level.
    THE NMR STUDY OF METALLIC NUCLEI Ⅱ THE 195Pt AND 31P NMR SPECTRA OF PHOSPHORUS CONTAINING PLATINUM (Ⅱ) COMPLEXES
    Yang Zhenyun, Han Xiuwen, Hu Jiehan, Liu Xiumei, Liu Zeming
    Chinese Journal of Magnetic Resonance, 1987, 4(4): 317-324.  
    Abstract     HTML ( )   PDF(4663KB)
    The 195Pt, 31P-NMR spectra were recorded for 12 platinum(Ⅱ) complexes containing phenyl cyclopentyl phosphine, phosphite and halogen ligands The influence of solvent,concentration and temperature on the 195Pt spectra were investigated Lewis base solvents cause 195Pt resonances moving upfield. For cis-Pt(PPh3)2Cl2 in CH2Cl2 solution, 195Pt concentration coefficient is -17.8ppm/mol, and temperature coefficient is 0. 43ppm/℃. It was found that the 195Pt, 31P chemical shifts of cis-isomers are less than those of trans-isomers, δcis < δtrans, and coupling constants of cis-isomers are greater than those of trans-isomers, (1Jpt-P)cis > (1Jpt-p)trans. Normal halogen dependence was observed for the complexes cis-Pt(PPh3)2X2, the order of δ(195Pt), δ(31P), 1Jpt-p values is Cl > Br > I. In 1, 2-diaminopropane solution the 195Pt satellite of 31P spectrum is the AB part of ABX system, whereas the central peak appears as a singlet.The 195Pt, 31P spectra of phosphite platinum complexes were also discussed.
    THE ESR SPECTRA OF FIVE REDUCED KEGGIN'S HETEROPOLYANIONS
    Mao Yougang, Yue Shitai, Qiu Zuwen, Wang Enbo
    Chinese Journal of Magnetic Resonance, 1987, 4(4): 325-335.  
    Abstract     HTML ( )   PDF(6219KB)
    The ESR spectra of five reduced heteropolyanions belonging to the Keggin structure are reported in this paper. They are SiV2Mo10O406-, SiV3Mo9O407-, PV3MO9O406-, PV3W9O406- and VV3W9O406-. At room temperature and pH≤ 3, their spectra contained 8 hfs lines, while at pH=7-8, 8+15 hyperfine lines. Their shape change gradually and finally turned to 8-lines spectrum after a long period of time. The frozen spectra at - 150℃ exhibited complicated 8 line spectra which were successfully simulated based on slightly modified Bleaney's theory.The ESR parameters g g A A were determined and the approximate K, α values were calculated based on DeArmond's theory. The physical meaning of the results are discussed and the failure of observing the 22 hfs lines of Vs species are primarily explained according to the number and degeneracy of the isomers present in the V3 species.
    NMR INVESTIGATIONS AND SEPARATIONS OF COMPONENTS OF CHINESE LACQUER'S URUSHIOL
    Qiu Feng, Li Liyun, Huang Zhaogeng, You Jiang, Qian Baogong
    Chinese Journal of Magnetic Resonance, 1987, 4(4): 337-343.  
    Abstract     HTML ( )   PDF(3363KB)
    The urushiol diacetate derived from urushiol have been successfully separated using centrifugal rotational TLC with preparative silica gel thin layer coated by silver nitrate. The method gave rapid separation of a large amount of different kinds of urushiol diacetatcs. Because the silver ion is very sensitive to the degree of unsaturation and configuration of the unsaturated bonds, urushiol di-acetates were well separated. We are satisfied that the five main components were good enough in purity and quantity for NMR study.
    The structure and configuration of key components of urushiol were determined successfully by 1H and 13C-NMR. The assignment of resonances for 1H and 13C were defined. In addition, they were confirmed by MS.
    ESR STUDY OF ACTIVE RADICALS PRODUCED IN THE PHOTOCHEMICAL HYDROGEN ABSTRACTION REACTIONS BETWEEN BENZOPHENONE AND 2-ARYL-1,3-DITHIOLAN
    Ji Haixing, Xu Guangzhi, Sun Lijun, Shi Shujian
    Chinese Journal of Magnetic Resonance, 1987, 4(4): 345-354.  
    Abstract     HTML ( )   PDF(5067KB)
    The active radicals produced in the photochemical hydrogen abstraction reactions between benzophenone and 2-ary1-1, 3-dithiolan were studied by combination of spin trapping technique with ESR specroscopy. Results show that the homolytic cleavage of C-H on the 2-C (or 4-C, 6-C) could take place, the produced active radicals  CH2 werestabilized by the conjugation of adjacent sulphur atoms and could be trapped by nitrosodurene (ND) (or 2,4,6-tri-t-butylnitrosobenzene(TBN)) to form two spin adducts the concentration ratio of which was about 1:1.
    THE STUDY ON UV,1H NMR AND CONFIGURATION OF α-HALOCINNAMAMIDES
    Wang Shuyu, Wang Dong, Qiao Liang, Wang Yingfen, Pang Jihai, Liu Weichin, Li Renli
    Chinese Journal of Magnetic Resonance, 1987, 4(4): 355-363.  
    Abstract     HTML ( )   PDF(4770KB)
    UV and 1H NMR of twelve pairs of α-halocinnamamides substituted by aromatic ring are reported. A structure-activity relationship study of a series of(Z) and(E)-N-alkyl-α-halocinnamamides showed that geometrical isomers act differently in the anticonvulsant activty; generally, (Z) derivatives are several times more potent than (E) isomers in the anticonvulsant activity. Their configurations were assigned by their UV γmax and 1H chemical shifts of protons on the amide group and olefinic bond. The configuration was confirmed by the X-ray diffraction results of one pair of these geometric isomers.
    2D NMR STUDY OF CLAVULACTONE
    Wang Qiwen, Wu Yuling
    Chinese Journal of Magnetic Resonance, 1987, 4(4): 365-368.  
    Abstract     HTML ( )   PDF(2136KB)
    This paper reports the study of DEPT, 2D H-H COSY, C-H COSY and long-range C-H COSY spectra of Clavulactone,a Dolabellane type diterpene.The long-range C-H COSY plays a very important role in the elucidation of H-C-C, H-C-C-C connectivities,therefore it is to some extent an alternative to the insensitive inadequate.
    NMR IMAGING THE LATEST PROGRESS AND REVIEW
    Feng Yilian
    Chinese Journal of Magnetic Resonance, 1987, 4(4): 369-379.  
    Abstract     HTML ( )   PDF(0KB)
    The fundamental principle of MRI is introduced briefly, and Compared with the traditional NMR spectroscopy. The recent research works of MRI are listed, and a diagram of research works system is made by the author. Particular emphases are placed on problems of fast imaging, high spacial resolution and contrast enhancement, etc. The problems of developing the chemical shift imaging and spectroscopic imaging are reviewed in detail. A new field of "Spacial Localized Spectroscopy" is discussed with the author's viewpoint in detail, also.