89767-02-2Relevant academic research and scientific papers
Phosphine Substituted Chelate Ligands, IX. NMR Spectra and Crystal Structure of Diphenyl(thio)phosphoryl-N,N-dimethylthioformamide
Bruns, Andreas,Hiller, Wolfgang,Kunze, Udo
, p. 14 - 18 (2007/10/02)
The P=S and P=O derivatives 2a, b of diphenylphosphino N,N-dimethylthioformamide (1) were obtained by addition of sulfur to 1 and by Arbusov reaction of Ph2POMe with Me2NC(S)Cl, respectively.The position of the cis-P N-methyl proton signal is markedly affected by the P=X group which exerts a diamagnetic shift for X = S (2a) but a paramagnetic shift for X = O (2b) relative to 1.Unusually small 3JPC couplings are observed in the 13C NMR spectrum.The P-sulfide 2a crystallizes in the monoclinic space group C2/c with the lattice constants a = 1791.5(3) pm, b = 686.7( 2) pm, c = 2591.3(4) pm, β = 93.10(4) deg.The molecule structure is characterized by a planar thioamide unit with the P=S group forming an angle of 53.4 deg to the plane. - Keywords: Crystal Structure, NMR Spectra, Solid State NMR, Thiophosphoryl-N,N-dimethylthioformamide, Phosphoryl-N,N-dimethylthioformamide
