- 作者: 廖芬鈴 ; 王素蘭 ; 林正憲 等
- 作者服務機構: 清華大學化學系
- 中文摘要: The preparation of benzoyl-protected N,N'- ethylenebis(2-mercaptopropanamide) (H/sub 4/emp) and its ligand-exchange reaction with ReO/sub 2/(en)/sub 2/Cl are described. Three diastereomers, [ syn-ReO(meso-emp) ]/sup -1/, [ anti-ReO(meso-emp) ] /sup - 1/, and a pair of enantiomers, [ ReO(rac-emp) ] /sup -1/, were formed due to syn and anti orientation of the two methyl groups of the ligand relative to the ReO core. The diastereomers were separated by reverse phase C/sub 18/ semipreparative HPLC and isolated as salts of [ Ph/sub 4/As ] [ ReO-(emp) ] . The structures of [ Ph/sub 4/As ] [ ReO(meso-emp) ] were determined by single-crystal X-ray analyses. [ Ph/sub 4/As ] [ syn-ReO(meso-emp) ] .bcdot.H/sub 2/O crystallizes in triclinic space group P.1bar. with a=10.326(3).ANG., b=13.672(4).ANG., c=14.023(5).ANG., .alpha.=61.20(2).degree., .beta.=74.74(3).degree., .gamma.=75.68(2).degree., V=1656.6(8).ANG./sup 3/, Z=2, Dc=1.676gm/L, F(000)=824 and R=0.0329 for 5877 unique reflections. For the complex [ Ph/sub 4/As ] [ anti-ReO(meso-emp) ] , the crystal data are: monoclinic, space group P2/sub 1//n, a=9.128(2).ANG., b=24.284(7).ANG., c=14.112(4).ANG.,.beta.=93.41(2).degree., V=3122.5(15).ANG./sup 3/, Z=4, Dc=1.740gm/L, F(000)=1608 and R=0.0361 for 5487 unique reflections. In both structures the rhenium atom is penta-coordinated and in an approximately square pyramidal environment.
- 英文摘要: --
- 中文關鍵字: Rhenium; Complex; Synthesis; Characterization; X-Ray Crystal Structure
- 英文關鍵字: 錸;錯合物;合成;特性;X射線晶體結構