DOI: 10.14469/hpc/11410 Metadata

Created: 2022-10-12 10:24

Last modified: 2024-06-25 09:40

Author: Henry Rzepa

License: Creative Commons: Public Domain Dedication 1.0

Funding: (none given)

Description

Crystal structure, NMR and IR data for Tris((4-(ethoxycarbonyl)-1-phenyl-1H-pyrazol-5-yl)oxy)ytterbium (70): Yb(OTf)3 (166 mg, 0.267 mmol, 1.00 equiv) was added with stirring to pyrazolone 6 (186 mg, 0.801 mmol, 3.00 equiv) in EtOH (4.0 mL) at 79 °C. Aqueous NaOH (2 M; 0.40 mL, 0.801 mmol, 3.00 equiv) was added with stirring and the mixture was heated at reflux for 4 h, after which the mixture was cooled to room temperature, H2O (20 mL) was added, and the resultant precipitate was collected by filtration, washed with H2O (3 x 10 mL) and dried in vacuo. Yb-pyrazolone complex 70 (211 mg, 0.227 mmol, 85%) was obtained as a white solid. Crystals suitable for X-ray crystallography were obtained by slow evaporation from an EtOH solution of complex 70. IR (Diamond-ATR, neat) νmax (cm-1) = 1647, 1598, 1555, 1531, 1500, 1433, 1256, 1232, 1171, 1120, 1085, 1036, 952, 785, 754, 632. m.p.: >140 °C (EtOH) (decomp.); 208 – 210 °C. Anal. Calcd for C36H33N6O9Yb ∙ H2O ∙ EtOH ∙ 1.3 Yb2O3: C, 31.84; H, 2.88; N, 5.86. Found: C, 31.69; H, 2.78; N, 5.46.

Member of collection / collaboration

DOI	Description
10.14469/hpc/10386	Syntheses and Characterization of Main Group, Transition Metal, Lanthanide and Actinide Complexes of Bidentate Acylpyrazolone Ligands

Members

DOI	Description
10.14469/hpc/11506	IR Data for Compound 70.
10.14469/hpc/11437	Primary crystal structure data for Compound 70. Tris((4-(ethoxycarbonyl)-1-phenyl-1H-pyrazol-5-yl)oxy)ytterbium

Edit