ONE STEP CONVERSION OF PERRHENATE INTO AN RE(IV) COMPLEX - SYNTHESIS AND MOLECULAR STRUCTURE OF TRANS-[RECL4(PMEPH2)(2)]

摘要

KReO4 reacts in a one-pot reaction with 4 mole of diphenylmethylphosphine and aqueous hydrochloric acid in boiling ethanol to yield trans-tetrachloro-bis (diphenylmethylphosphine) rhenium (1) in high yield. The almost quantitative, direct reduction of perrhenate to Re(IV) by PPh2Me/HCl has been observed for the first time. Bright red 1 can be crystallized from chloroform/hexane to give bright red plates. Crystals of 1 are triclinic with a=8.898(6), b=9.543(4), c=9.713(3) Angstrom, alpha=66.68(2), beta=88.54(4), gamma=63.10(3)degrees, Z=1 and D-obs=1.83 g cm(-3). The structure was solved from 2327 diffraction data (F-o(2) greater than or equal to 3 sigma(F-o(2))) collected at 20(2)degrees and refined to R=0.029 (R-w=0.039). [References: 13]