Structural and solid-state 31P N.M.R. studies on a novel fluorotris(triphenylphosphine)copper(I) adduct
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The synthesis of the title compound as its triphenylphosphine /methanol solvate, [(PPh3)3CuF].- 4PPh3.4MeOH, is reported together with characterization by solid-state 31P CP-MAS n.m.r. and single-crystal X-ray diffraction. Crystals are trigonal, space group P3, with a 14.453(5), c 15.388(6)?. The structure refined to a final R value of 0.049 for 1926 'observed' [I> 3s(I)] reflections. The (PPh3)3CuF molecule lies on a crystallographic threefold axis. Cu-F is 2.115(9)?, and Cu-P 2.323(3)?. The solid-state 31P n.m.r. spectrum is dominated by peaks from each of the four solvated PPh3 molecules at -1.6, -5.4, -10.6 and -14.2 ppm with respect to 85% H3PO4. The quartet of lines arising from the ligands coordinated to the copper atom shows an average chemical shift of -5 ppm and approximately equal line spacings of 1.0 kHz.
Australian Journal of Chemistry