Synthesis and structural characterization of [VS_4(CuPPh_3)_4Br] centre dot CH_2Cl_2

摘要

Heating a solid mixture of (NH_4)_3 VS_4, CuCl, PPh_3, and NEt_4Br at 100 deg C for 10 h and extraction with CH_2Cl_2 yielded [VS_4(CuPPh_3)_4Br] centre dot CH_2Cl_2. Crystallographic data: Triclinic, P1-bar, a = 15.189(3), b = 20.093(6), c = 12.031(3) A, #alpha# = 102.39(2), #beta# = 100.05(2), #gamma# = 82.86(2) deg, V = 3517(3) A~3, and Z = 2. The configuration of the VS_4Cu_4Br core can be described as a distorted cubane with an additional face. The V atom has retained the tetrahedral geometry of the free[VS_4]~(3-) moiety. The four Cu atoms have three different coordination environments. strongly distorted tetrahedral, nearly trigonal planar, and strictly trigonal planar. The infrared, electronic, and ~(51)V NMR spectra have also been reported.