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NMR STUDIES OF METALLIC NUCLEI Ⅲ THE 119 Sn,117 Sn-NMR SPECTRA OF ORGANO-TIN (Ⅳ) COMPOUNDS AND THE COMPLEX FORMATION WITH DONOR SOLVENT
Yang Zhenyun, Wang Shihua, Liu Xiumei, Pan Hongcheng
Chinese Journal of Magnetic Resonance, 1990, 7(2): 147-152.
The 119 Sn,117 Sn-NMR spectra were recorded for twenty organo-tin (IV) compounds containing alkyl, phenyl, allyl, five-membered heterocyclcs and other polar groups. The substituent influence on tin electron density and magnetic shielding were discussed. The effects of solvents, concentration and temperature on 119 Sn resonances were investigated. The complex formation of Ph3 SnCl with DMSO was studied and the equilibrium constant K and △G were calculated.
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13 C-NMR STUDY ON CARBONYLATION OF TOLUENE (Ⅱ)
Wu Daxu, Zheng Yu, Chen Zhengming
Chinese Journal of Magnetic Resonance, 1990, 7(2): 153-159.
The tracer experiments of the passing CO-HCl mixture through Toluene-Aluminum Chloride-Hydrogen Chloride system were described by
13 C-NMR.The results suggest that the intermidiate complex of thecarbonylation of Toluene is
AlCl
4 - , the reaction mechanism is also discussed.
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SEPARATION OF DIPOLE-DIPOLE RELAXATION FOR QUATERNARY CARBONS-NMR RELAXATION STUDY OF TESTOSTERONE PROPIONATE IN SOLUTION
Zheng Douhuan, Hideaki Fujiwara, Dan Yongzhong, Masayuki Watanabe, Yoshio sasaki
Chinese Journal of Magnetic Resonance, 1990, 7(2): 161-170.
In this paper, a new method was suggested to separate Dipole-Dipole relaxation, that is called parameter separation method. For a stable rigid molecule, the diffusion coefficient could be calculated from measurement values of secondry and tertiary carbons, which is usually not only for a kinematic research, but also for evaluation of Dipole-Dipole relaxation of quaternary carbons. This procedure shows higher reliability. The result of relaxation study on title mentioned compound shows that parameter separation method is quite efficient for the study of relaxation mechanism for a stable rigid molecule, especially for quaternary carbons.
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ESR STUDIES OF POLYACENIC ELECTRICAL CONDUCTIVITY MATERIALS
Wang Rongshun, Xie Demin, Wang Yusong, Zhang Xiyan, Fu Yujie, Zhao Chengda, Zhan Ruiyun, Liu Guizhen
Chinese Journal of Magnetic Resonance, 1990, 7(2): 195-200.
ESR measurements have been performed on polyacenic material prepared by the pyrolytic treatment of phenol-formaldehyde resin. Five pyrolysis temperatures in the range of 500-1100℃ were selected. The ESR line width, spin concentration, the ratio of Dysonian lineshape's A and B etc. of the pristine samples strongly depend on the pyrolysis temperatures, reflecting the structureal characteristics in each samples.
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ASSIGNMENT OF THE INDIVIDUAL SHIFTS OF CROWN ETHER DERIVATIVES OF EDTA AND 4'-DANSYLAMINO BENZO CROWN ETHERS' 1 H AND 13 C NMR SPECTRA
Zhang Anjiang, Wang Shumei, Huang Su, Qing Shenying
Chinese Journal of Magnetic Resonance, 1990, 7(2): 225-230.
1 H and 13 C NMR spectra of N (,N')-(di) tosyl macro-cyclic ether-bislactones (1-6), N,N'-dicarboxymethyl macrocyclic ether-bislactones and amine-bislactame (8-12) and 4'-dansylamino benzo crown ethers (13-16) etc. eighteen crown ethers were recorded and assigned by consideration of known substitute effects. The 1 H chemical shifts obtained indicate that the larger the crown ether, the larger the proton chemical shift for methylene b in Crown 1-6 and for methylene a, b, c in Crown 8-11. These shifts approach a limit when the number of macrocyclic atoms arrives at 21-24. Solvents show considerable effect on the 1 H chemical shifts of methylenes a, b, c in Crown 8-11 which increase with the solvent polarity, the order is as follows:CD3 COOD > PY-d3 ≥ D2 O > CD3 OD > CD3 CD2 OD > DMF-d7 > DMSO-d6 .