DOI: 10.14469/hpc/11408 Metadata

Created: 2022-10-12 10:21

Last modified: 2024-06-25 09:37

Author: Henry Rzepa

License: Creative Commons: Public Domain Dedication 1.0

Funding: (none given)

Description

Crystal structure, IRl data for Sodium(I) tetrakis((4-(ethoxycarbonyl)-1-(4-methoxybenzyl)-1H-pyrazol-5-yl)oxy)dysprosium (65): DyCl3•6H2O (95.0 mg, 0.252 mmol, 1.00 equiv) was added with stirring to pyrazolone 8 (209 mg, 0.757 mmol, 3.00 equiv) in EtOH (4.5 mL) at 79 °C. Aqueous NaOH (2 M; 0.38 mL, 0.757 mmol, 3.00 equiv) was added with stirring and the mixture was heated at reflux for 20 h. H2O was added (20 mL), the mixture was cooled to room temperature, and the resultant precipitate was collected by filtration, washed with H2O (3 x 10 mL) and dried in vacuo. Dy-pyrazolone complex 65 (165 mg, 0.128 mmol, 51%) was obtained as a yellow-white solid. Crystals suitable for X-ray crystallography were obtained by slow evaporation from an EtOH solution of complex 65. Repeating the reaction with Dy(OTf)3 (200 mg, 0.328 mmol, 1.00 equiv), pyrazolone 8 (272 mg, 0.984 mmol, 3.00 equiv) and aqueous NaOH (2M, 0.49 mL, 0.984 mmol, 3.00 equiv) according to the above procedure resulted in an improved yield of Dy-pyrazolone complex 65 (285 mg, 0.222 mmol, 68%). IR (Diamond-ATR, neat) νmax (cm-1) = 1616, 1510, 1430, 1318, 1243, 1215, 1175, 1090, 1027, 782. HRMS (ESI) m/z: [M – L + H]+ calc. for (C42H46DyN6O12)+: 990.2460, found: 990.2491. m.p.: 170 – 173°C (EtOH). Anal. Calcd for C56H60DyN8NaO16 ∙ H2O ∙ 2 EtOH: C, 51.59; H, 5.34; N, 8.02. Found: C, 51.84; H, 4.70; N, 7.81.

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/11495	IR Data for Compound 65.
10.14469/hpc/11435	Primary crystal structure data for Compound 65. Sodium(I) tetrakis((4-(ethoxycarbonyl)-1-(4-methoxybenzyl)-1H-pyrazol-5-yl)oxy)dysprosium

Edit