MIXED-LIGAND COMPLEXES OF RHENIUM .7. SYNTHESIS, CHARACTERIZATION AND X-RAY CRYSTAL STRUCTURE OF BIS(DIETHYLDITHIOCARBAMATO)(DIMETHYLPHENYLPHOSPHINE)-(TRIPHENYLBORYLIMIDO) RHENIUM(V), [RE(NBPH(3))(ME(2)PHP)(ET(2)DTC)(2)]

摘要

The novel borylimido rhenium(V) complex bis(diethyldithiocarbamato)(dimethylphenylphosphine)(triphenylborylimido)- rhenium(V), [Re(NBPh(3))(Me(2)PhP)(Et(2)dtc)(2)], has been synthesized from [ReN(Me(2)PhP)(Et(2)dtc)(2)] and NaBPh(4) via the intermediate complex [Re{NC(CH3)(2)CH2C(O)CH3}(Me(2)PhP)(Et(2)dtc)(2)](+) which is primarily formed in an acetone/HCl mixture. [Re{NC(CH3)(2)CH2C(O)CH3}(Me(2)PhP)(Et(2)dtc)(2)] and the final product were characterized by IR and NMR spectroscopy and mass spectrometry. [Re(NBPh(3))(Me(2)PhP)(Et(2)dtc)(2)] crystallizes monoclinic in the space group P2(1), Z = 4, R = 0.0479 for 5899 observed independent reflections. The lattice dimensions are a = 10.313(2), b =24.357(4), c = 15.857(3) Angstrom, beta = 106.35(1)degrees. The bond lengths in the linear Re=N-B bridge are Re-N 1.653(12) and N-B 1.64(3) Angstrom, respectively. [References: 10]