90968-01-7Relevant academic research and scientific papers
Preparation, properties, and structural studies of molybdenum and tungsten complexes with [Ph2P(S)C(S)NR]- (R = Me, Ph) or Ph2PS- ligands. X-ray structure analysis of Mo(CO)2(η5-C5H5)[Ph 2P(S)C(S)NPh]
Ambrosius,Van Hemert,Bosman,Noordik,Ariaans
, p. 2678 - 2685 (2008/10/08)
M(CO)3(η5-C5H5)Cl (M = Mo, W) reacts with Ph2P(S)C(S)N(H)R (R = Ph, Me) and a base to yield three different products depending on reaction time and temperature. At room temperature complexes of composition M(CO)2(η5-C5H5)[Ph 2P(S)C(S)NR] are obtained, in which the ligands are coordinated by both sulfur atoms. At higher temperature mixtures are obtained of M(CO)2(η5-C5H5)[Ph 2P(S)C(S)NR] (M = Mo, R = Ph, Me; M = W, R = Me), in which the ligand is coordinated through S(C) and N, and M(CO)2(η5-C5H5)(η 2-SPPh2) (M = Mo, W). The last complexes can also be prepared from M(CO)3(η5-C5H5)Cl in a direct reaction with SPPh2H and Et3N. M(CO)3(PPh3)2Cl2 (M = Mo, W) reacts with 2 equiv of Ph2P(S)C(S)N(H)Ph in the presence of a base to form M(CO)2(PPh3)[Ph2P(S)C(S)NPh]2, in which the ligands show a dynamic behavior with respect to the coordinating mode. The starting complexes react with SPPh2H and Et3N to M(CO)2(PPh3)(η2-SPPh2) 2. Under similar conditions Mo(CO)4Cl2 gives Mo(CO)3(η2-SPPh2)2. The complexes are characterized by means of elemental analyses, infrared spectroscopy, and 1H and 31P NMR spectroscopy. The X-ray structure analysis of Mo(CO)2(η5-C5H5) [Ph2P(S)C(S)NPh] is presented: a = 10.390 (4) A?, b = 14.328 (5) A?, c = 9.602 (3) A?, a = 73.02 (2)°, β = 108.49 (2)°, and γ = 112.39 (2)° in space group P1 and Z = 2.
