General Syntheses of (RPPh₂)Mo(CO)₅and (RDBP)Mo(CO)₅Complexes from Ph₂PLi and DBPLiviaSingle Electron Transfer Catalysis

Solid-State95Mo NMR Studies of Some Prototypal Molybdenum Compounds: Sodium Molybdate Dihydrate, Hexacarbonylmolybdenum, and Pentacarbonyl Phosphine Molybdenum(0) Complexes

“…Therefore, it is reasonable to conclude that χ( 95 Mo) will be negative for all compounds of this type, Mo(CO) 5 PR 3 . Also, analysis of the 31 P MAS NMR spectrum confirms that 1 J ( 95 Mo, 31 P) = 130 ± 10 Hz, in excellent agreement with the value determined in solution . As in the case of Na 2 MoO 4 · 2H 2 O, the experimental spectrum was simulated using convolution with a Gaussian peak 27 Hz wide.…”

“…Sodium molybdate dihydrate and hexacarbonylmolybdenum(0) were commercially available. Pentacarbonyl-5-methyldibenzophosphole molybdenum(0), Mo(CO) 5 (MeDBP), was prepared as previously described, and pentacarbonylbis(diphenylphosphino)methanemolybdenum(0), Mo(CO) 5 (η 1 -dppm), was prepared using standard literature methods …”

Intramolecular [4+2] Diels−Alder Cycloaddition of a 2H-Phosphole to Coordinated Unsaturated Phosphines, Phospholes, and an Arsine

“…In order to explore the scope of these reactions we developed a high-yield general synthesis of the crotyl tertiary phosphine complexes ( A and B ) . The synthesis of an analogous tertiary arsine complex ( C ) is also described here (see Experimental Section).…”

“…All experiments were performed under a dry nitrogen atmosphere using standard Schlenk line techniques. (RPh 2 P)Mo(CO) 5 7 and (RDBP)Mo(CO) 5 , where R = -CH 2 CHCH 2 or -( trans )CH 2 CHCHCH 3 , and 3,4-dimethyl-1-phenylphosphole (DMPP) were prepared by literature methods. Tetrahydrofuran was distilled under nitrogen from sodium benzophenone ketyl, and diglyme was distilled under nitrogen over sodium.…”

Synthesis and Characterization of Unsymmetrical (cis-(Phosphino−arsino)ethene)tetracarbonylmolybdenum Complexes: Hydroarsination Reactions of (H3CC⋮CPPh2)Mo(CO)5 and [H2CCCH(DBP)]Mo(CO)5 and Hydrophosphination Reactions of (Ph2AsCH2C⋮CH)Mo(CO)5

“…From our several attempts to synthesize the secondary arsine complex Ph 2 AsHMo(CO) 5 by the literature procedure designed to prepare analogous secondary phosphine complexes, we found the former to be highly unstable. In contrast, we were able to synthesize the stable diphenyl tertiary arsinoalkyne complex G [(Ph 2 AsCH 2 C⋮CH)Mo(CO) 5 ] in 57% yield (see Experimental Section) by following the same synthetic route …”