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Hafnium(IV) Chloride Complexes With Chelating β-ketiminate Ligands: Synthesis, Spectroscopic Characterization and Volatility Study

Hafnium(IV) Chloride Complexes With Chelating β-ketiminate Ligands: Synthesis, Spectroscopic Characterization and Volatility Study

Siddappa A Patil, Phillip A Medina, Aleks Antic, Joseph W Ziller, Jason K Vohs, Bradley D Fahlman

Spectrochim Acta A Mol Biomol Spectrosc. 2015 Sep 5;148:223-31.

PMID: 25897715

Abstract:

The synthesis and characterization of four new β-ketiminate hafnium(IV) chloride complexes dichloro-bis[4-(phenylamido)pent-3-en-2-one]-hafnium (4a), dichloro-bis[4-(4-methylphenylamido)pent-3-en-2-one]-hafnium (4b), dichloro-bis[4-(4-methoxyphenylamido)pent-3-en-2-one]-hafnium (4c), and dichloro-bis[4-(4-chlorophenylamido)pent-3-en-2-one]-hafnium (4d) are reported. All the complexes (4a-d) were characterized by spectroscopic methods ((1)H NMR, (13)C NMR, IR), and elemental analysis while the compound 4c was further examined by single-crystal X-ray diffraction, revealing that the complex is monomer with the hafnium center in octahedral coordination environment and oxygens of the chelating N-O ligands are trans to each other and the chloride ligands are in a cis arrangement. Volatile trends are established for four new β-ketiminate hafnium(IV) chloride complexes (4a-d). Sublimation enthalpies (ΔHsub) were calculated from thermogravimetric analysis (TGA) data, which show that, the dependence of ΔHsub on the molecular weight (4a-c) and inductive effects from chlorine (4d).

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP13499053	Hafnium(IV) chloride		13499-05-3	Price

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