Studies on organolanthanide complexes: LXIII. Synthesis, spectroscopic and X-ray crystallographic characterization of new early organolanthanide, organoyttrium hydride and organoholmium hydroxide complexes☆

Add time:08/31/2019    Source:sciencedirect.com

Organolanthanide chloride complexes [(CH3OCH2CH2C5H4)2Ln(μ-Cl)]2 (Ln = La, Pr, Ho and Y) react with excess NaH in THF at 45°C to give the dimeric hydride complexes [(CH3OCH2CH2C5H4)2Ln(μ-H)]2, which have been characterized by IR, 1H NMR, MS and XPS spectroscopy, elemental analyses and X-ray crystallography. [(CH3OCH2CH2C5H4)2Y(μ-H)]2 crystallizes from THF/n-hexane at −30°C, in the triclinic space group P1 with a = 8.795(2) Å, b = 11.040(1) Å, c = 16.602(2) Å, α = 93.73(1)°, β = 91.82(1)°, γ = 94.21(1)°, Dc = 1.393 gcm−3 for Z = 2 dimers. However, crystals of [(CH3OCH2CH2C5H4)2Ho(μ-OH)]2 were obtained by recrystallization of holmium hydride in THF/n-hexane at −30°C, in the orthorhombic space group Pbca with a = 11.217(2) Å, b = 15.865(7) Å, c = 17.608(4) Å, Dc = 1.816 gcm−3 for Z = 4 dimers. In the complexes of yttrium and holmium, each Ln atom of the dimers is coordinated by two substituted cyclopentadienyl ligands, one oxygen atom and two hydrogen atoms (for the Y atom) or two hydroxyl groups (for the Ho atom) to form a distorted trigonal bipyramid if the C(η5)-bonded cyclopentadienyl is regarded as occupying a single polyhedral vertex.

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