114860-65-0Relevant academic research and scientific papers
Anionic perphosphido and perarsenido complexes of gallium and indium
Carrano, Carl J.,Cowley, Alan H.,Giolando, Dean M.,Jones, Richard A.,Nunn, Christine M.,Power, John M.
, p. 2709 - 2714 (2008/10/08)
Reaction of 4 equiv of LiEPh2 with MCl3 in THF at -78°C yields the anionic perphosphido and perarsenido complexes [Li-(THF)4] [M(EPh2)4] (1, M = Ga, E = P; 2, M = In, E = P; 3, M = Ga, E = As) in 70-80% yields. The air-sensitive complexes are yellow and crystalline and can be recrystallized from THF/toluene mixtures. The X-ray structures of 1-3 have been determined. The anionic moieties of 1-3 are very similar. The M-E bond lengths, EPh2 geometries, and M(EC2)4 conformations are indicative of M-E single bonding in each case. Crystal data for 1: C64H72GaLiO4P4, Mr = 1105.84, orthorhombic, P212121 (No. 19), a = 13 945 (7) A?, b = 18.332 (5) A?, c = 23.671 (4) A?, V = 6051.7 (3) A?3, Dcalcd = 1.214 g cm-3, Z = 4, μ(Mo Kα) = 5.99 cm-1. Refinement of 4127 reflections (I > 3σ(I)) out of 4155 unique observed reflections (3° ≤ 2θ ≤ 44°) gave R and Rw values of 0.0688 and 0.0747, respectivelv. Crystal data for 2: C64H72InLiO4P4, orthorhombic, P212121 (No. 19), a = 14.017 (4) A?, b = 18.402 (9) A?, c = 23.696 (5) A?, V = 6112.6 (9) A?3, Dcalcd = 1.251 g cm-3, Z = 4, μ(Mo Kα) = 5.25 cm-1. Refinement of 4163 reflections (I > 3σ(I)) out of 4189 unique observed reflections (3° ≤ 2θ ≤ 44°) gave R and Rw values of 0.0558 and 0.0644, respectively. Crystal data for 3: C68H80As4GaLiO5, triclinic, P1 (No. 2), a = 13.392 (7) A?, b = 13.521 (5) A?, c = 19.025 (7) A?, α = 87.92 (3)°, β = 76.19 (4)°, γ = 83.16 (3)°, V = 3321.1 (7) A?3, Dcalcd = 1.354 g cm-3, Z = 2, μ(Mo Kα) = 24.30 cm-1. Refinement of 8132 reflections (3° ≤ 2θ ≤ 44°) gave R and Rw values of 0.0626 and 0.0707, respectively. There is a disordered THF molecule not bound to Li in the structure of 3.
