Synthesis under self-controlled reaction conditions: Reaction of tetraamminezinc(II) chloride with 3,5-dimethyl-1-thiocarboxamide pyrazole
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The trinuclear [Zn-3(Hdmpz)(2)(dmpz)(4)(NCS)(2)] complex (Hdmpz: 3,5-dimethylpyrazole) has been synthesized by the reaction of tetraamminezinc(II) chloride with 3,5-dimethyl-1-thiocarboxamidepyrazole. The ammonia evolving gradually from [Zn(NH3)(4)]Cl-2 ensured a mild gradually increasing basic pH during the synthesis which caused a cleavage of the 1-N-substituent. Moreover, the changing pH controlled the pyrazolate anion-neutral ligand equilibrium, and in this way the formation of the precipitate complex. The structure of the complex was investigated by X-ray diffraction and quantum chemical computations. The complex was characterized in detail by FT-IR-spectroscopy and thermal analysis. The bonding interactions between Zn2+ and the ligands were analysed on the basis of the computed data. (c) 2007 Elsevier B.V. All rights reserved.
Кључне речи:crystal growth / XRD / FT-IR / thermal analysis / DFT computations
Извор:Journal of Organometallic Chemistry, 2007, 692, 12, 2582-2592
ISSN: 0022-328X (print)