261623-95-4Relevant academic research and scientific papers
The reaction of ytterbium with N-iodo-triphenylphosphaneimine. Crystal structures of Yb2I(THF)2(NPPh3) · 2 THF, [YbI2(HNPPh3)(DME)2], and [{YbI2(DME)2}2(μ-DME)]
Groeb, Thorsten,Seybert, Gerd,Massa, Werner,Dehnicke, Kurt
, p. 349 - 353 (2000)
When treated with ultrasound, the reaction of ytterbium powder with INPPh3 in tetrahydrofuran leads to [YbI2(THF)4] and to the mixed-valence phosphoraneiminato complex [Yb2I(THF)2(NPPh3)4] · 2 THF (1), which forms red single-crystals. In the analogous reaction in 1,2-dimethoxyethane (DME) only the ytterbium(II) iodide solvates [YbI2(HNPPh3)(DME)2] (2) and [{YbI2(DME)2}2 · (μ-DME)] (3) can be isolated, which form yellow single crystals. All compounds were characterized by crystal structure analyses. 1: Space group P1, Z = 2, lattice dimensions at -80 °C: a = 1337.6(5), b = 1389.6(5), c = 2244.2(17) pm; α = 86.11(7)°, β = 88.06(7)°, γ = 88.63(4)°; R = 0.0759. In 1 the two ytterbium atoms are connected via the N atoms of two phosphoraneiminato groups (NPPh3-) to form a planar Yb2N2 fourmembered ring. The structure can also be described as an ion pair consisting of [YbI(THF)2]+ and [Yb(NPPh3)4]-· 2: Space group P21 Z = 2, lattice dimensions at -80 °C: a = 811.9(1), b = 1114.0(1), c = 1741.3(1) pm; β = 95.458(5)°; R = 0.0246. 2 forms molecules in which the ytterbium atom is coordinated in a pentagonal-bipyramidal fashion with the iodine atoms in the axial positions. The O atoms of the two DME-chelates and the N atom of the phosphaneimine ligand HNPPh3 are in the equatorial positions. 3: Space group P1, Z = 2, lattice dimensions at -70 °C: a = 817.5(1), b = 1047.7(1), c = 1115.5(2) pm; α = 90.179(10)°, β = 97.543(15)°, γ = 91.087(12)°; R = 0.0317. 3 has a dimeric molecular structure, in which the two fragments {YbI2(DME)2} are connected centrosymmetrically via a μ-DME bridge. As in 2, the ytterbium atoms are coordinated in a pentagonal-bipyramidal fashion with the iodine atoms in the axial positions, as well as with the two DME chelates and with one O atom each of the μ-DME ligand in the equatorial positions.
