Fraga-Hernández, et al. Acta Crystallographica Section E: Structure Reports Online, 2011, 67(1), m31-m31.
The title compound W(NO)2Cl2(IMes)2·C4D8O was synthesized as an intermediate via the reaction of the coordination polymer dinitrosotungsten dichloro[W(NO)2Cl2]n with 1,3-bis(2,4,6-trimethylphenyl)imidazol-2-methylene (IMes). The intermolecular C-H···O interactions connect the organometallic molecules with the tetrahydrofuran-d8 solvent molecules. This intermediate can be further used to synthesize novel dinitrosotungsten hydrides and dihydrides derivatives with sterically demanding and highly donor-friendly phosphine ligands or N-heterocyclic (NHC) carbene ligands.
Synthesis of W(NO)2Cl2(IMes)2·C4D8O
A stirred suspension of [W(NO)2Cl2]n (128.4 mg, 0.408 mmol) in 15 ml of tetrahydrofuran-d8 (THF-d8) was treated with a dropwise addition of a solution of IMes (248 mg, 0.815 mmol) in THF-d8 (5 ml) over 15 minutes. The solution gradually darkened, forming a flocculent black residue. After stirring the reaction mixture at room temperature for 6 hours, a deep green solution was obtained, showing IR spectrum peaks at 1737 and 1624 cm-1, which are indicative of nitrosyl groups. The volatiles were evaporated under vacuum, and the residue was extracted with 25 ml of toluene. The resulting dark green solution was filtered through celite and dried under vacuum. The solid was recrystallized using CH2Cl2/pentane, yielding a fraction of green crystals, which were washed with pentane and dried in vacuo, resulting in 312.8 mg of [W(NO)2Cl2(IMes)2]·C4D8O (83%).
Chen, Kang, et al. Green Chemistry, 2019, 21(16), 4380-4387.