Compound 3
bis(1-(2,6-diisopropylphenyl)-3,3,5,5-tetramethylpyrrolidine-2-ylidene)beryllium
From: Neutral zero-valent s-block complexes with strong multiple bonding
View in PubChem | 1H NMR | 9Be NMR | 13C NMR | UV-Vis NMR | Cyclic Voltammogram | CIF | MDL Molfile | ChemDraw
Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.
Synthesis of [Be(MeL)2], 3: A solution of 1 (170 mg, 0.5 mmol, 1.0 eq.) in Et2O (8 mL) was treated with MeL (133 mg, 0.5 mmol, 1.0 eq.) and KC8 (125 mg, 1.0 mmol, 2.0 eq.) and was stirred at room temperature for 5 h. The suspension was filtered over a pad of Celite® and the filtrate reduced in vacuo. Slow evaporation of the solution afforded 3 as purple crystalline solid (95 mg, 35%). M.p.: 195 °C. 9Be NMR (Et2O, 56 MHz): δ = 32 (s). 1H NMR (THF-d8, 400 MHz): δ = 7.21–7.16 (m, 2H, CHpara), 7.15–7.12 (m, 4H, CHmeta), 3.27 (sept., JHH = 7 Hz, 4H, C H (CH3)2), 1.81 (s, 4H, CH2), 1.40 (d, JHH = 7 Hz, 12H, CH(C H3)2), 1.23 (s, 12H, CH3), 1.18 (d, JHH = 7 Hz, 12H, CH(C H3)2), 0.76 (br s, 12H, CH3). 13C{1H} NMR (THF-d8, 125 MHz): δ = 189.4 (Cq,carbene), 150.4 (Cq), 139.9 (Cq), 128.0 (CHpara), 126.0 (CHmeta), 69.9 (Cq), 57.4 (CH2), 47.7 (Cq), 33.1 (CH3), 30.0 (CH3), 29.0 (CH( C H3)2), 28.9 (C H(CH3)2), 25.1 (CH( C H3)2). Elemental analysis calcd (%) for C40H62BeN2: C 82.84, H 10.78, N 4.83; found: C 82.46, H 10.86, N 4.85. Crystal data for 3: C52H74BeN2, Mr = 736.14, purple block, 0.29×0.22×0.18 mm3, triclinic space group P, a = 10.009(3) Å, b = 10.854(4) Å, c = 11.522(3) Å, α = 73.426(12)°, β = 71.114(8)°, γ = 78.842(11)°, V = 1128.0(6) Å3, Z = 1, ρcalcd = 1.084 g ・ cm–3, μ = 0.061 mm–1, F(000) = 404, T = 100(2) K, R1 = 0.0636, wR2= 0.1152, 4621 independent reflections [2θ≤52.744°] and 258 parameters.
