13435-10-4Relevant articles and documents
Synthesis, characterization, and X-ray crystal structures of W(VI) alkyl complexes with chelating diamide and imido co-ligands
Boncella, James M.,Wang, Shu-Yu S.,VanderLende, Daniel D.,Huff, R. Leigh,Abboud, Khalil A.,Vaughn, William M.
, p. 59 - 70 (1997)
The complex W(NPh)Cl2[o-(NSiMe3)2C6H4] 3 was synthesized from PhN=WCl4·OEt2 and N,N′-(Li2[o-(NSiMe3)2C6H4] and reacts with Lewis bases to form the adducts W(NPh)Cl2[o-(NSiMe3)2C6H4](L) (L = PMe3, THF, 3-picoline, tBuNC, MeCN) 4a-e. Crystals of 4a are triclinic, space group P1, with a = 9.562(1), b = 10.277(1), c = 14.920(2) A, α = 82.15(1), β = 80.18(1), γ = 80.41(1)°, and Z = 2. The structure was solved by the heavy atom method and refined to R = 0.0408 for 4224 observed (I > 2σ(I)) reflections. The dialkyl complexes W(NPh)R2[o-(NSiMe3)2C6H4] (R = Me, Et, CH2Ph, CH2CMe3, CH2CMe2Ph) 5-9 are formed through subsequent reactions of 3 with the corresponding Grignard reagent. Crystals of complex 5 are monoclinic, space group P2(1)/n, with a = 10.3545(2), b = 17.9669(1), c = 13.3168(1) A, β = 103.826(1)°, and Z = 4. The structure of complex 5 was solved by direct methods in SHELXTL5 and refined to R = 0.0247 for 4572 observed reflections. Compound 5 has a square pyramidal geometry in which the imido ligand occupies the apical position and reacts with PMe3 to form the adduct W(NPh)Me2[o-(NSiMe3)2C6H4](PMe3) 5a. Crystals of complex 5a are monoclinic, space group C2/m, with a = 13.5336(1), b = 14.4291(1), c = 15.3785(1) A, β = 110.365(1)°, and Z = 4. The structure of compound 5a was solved by direct methods in SHELXTL5 and refined to R = 0.0272 for 3057 observed reflections. Crystals of the bis-neopentyl complex 8 are monoclinic, space group P2(1)/n, with a= 10.6992(4), b= 18.3144(7), c = 16.0726(6) A, β = 92.042(1)°, and Z = 4. The structure of 8 was solved by direct methods in SHELXTL5 and refined to R = 0.0261 for 5881 observed reflections. Complex 8 has a trigonal bipyramidal geometry with both neopentyl groups and one amido nitrogen in the equatorial plane.
"DIBUTYLMAGNESIUM", A CONVENIENT REAGENT FOR THE SYNTHESIS OF USEFUL ORGANIC MAGNESIUM REAGENTS MgA2 INCLUDING CYCLOPENTADIENYLS, ARYLOXIDES, AND AMIDES. PREPARATION OF Zr(C5H5)Cl3. X-RAY STRUCTURE OF (SiMe3)-o>(OEt2)>2
Duff, Alan W.,Hitchcock, Peter B.,Lappert, Michael F.,Taylor, Richard G.,Segal, John A.
, p. 271 - 284 (1985)
n-Heptane-soluble "di-butylmagnesium" (I) (a commercially available material, prepared by addition of LiBus to MgBunCl, and subsequent addition of ca, 5percent MgOctn2) has been found to be a useful starting material for o
Stoichiometric Reactions of CO2 and Indium-Silylamides and Catalytic Synthesis of Ureas
Xu, Maotong,Jupp, Andrew R.,Stephan, Douglas W.
supporting information, p. 14277 - 14281 (2017/10/31)
The indium compounds In(N(SiMe3)2)2Cl?THF (2) and In(N(SiMe3)2)Cl2?(THF)n (3) were shown to react with CO2 to give [(Me3Si)2N)InX(μ-OSiMe3)]2 (X=N(SiMe3)2 4, Cl 5). 0.05–2.0 mol % of the species 3 acts as a pre-catalyst for the conversion of aryl and alkyl silylamines under CO2 (2–3 atm) to give the corresponding ureas in 70–99 % yields. A proposed mechanism is supported by experimental and computational data.
