A pyridine adduct of bis(di-iso-butyldithiocarbamato-S,S ')cadmium(II): Multinuclear (C-13, N-15, Cd-113) CP/MAS NMR spectroscopy, crystal and molecular structure, and thermal behaviour

作者：Rodina Tatyana A; Ivanov Alexander V^*; Gerasimenko Andrey V; Ivanov Maxim A; Zaeva Anna S; Philippova Tatyana S; Antzutkin Oleg N

来源：Inorganica Chimica Acta, 2011, 368(1): 263-270.

DOI：10.1016/j.ica.2011.01.006

• N,N-dialkyldithiocarbamate cadmium(II) adducts
• Supramolecular compounds
• Molecular structures
• Multinuclear C-13, N-15
• Cd-113 CP/MAS NMR spectroscopy
• Cd-113 chemical shift anisotropy
• Simultaneous thermal analysis

Crystalline bis(N, N-di-iso-butyldithiocarbamato-S,S')(pyridine)cadmium(II) - adduct 1 was prepared and studied by means of multinuclear C-13, N-15, Cd-113 CP/MAS NMR spectroscopy, single-crystal X-ray diffraction and simultaneous thermal analysis (STA). In molecular structure 1, the cadmium atom coordinates with four sulphur atoms and one nitrogen atom of pyridine, forming a coordination polyhedron [CdS4N], whose geometry is an almost ideal tetragonal pyramidal (C-4v). The coordinated py molecule is in the apical position, while two structurally non-equivalent di-iso-butyldithiocarbamate ligands, playing the same terminal S,S'-chelating function, define the basal plane. To characterise additionally the structural state of the cadmium atom in this fivefold coordination, Cd-113 chemical shift anisotropy (CSA) parameters, delta(aniso) and eta, were calculated from experimental MAS NMR spectra that revealed an almost axially symmetric Cd-113 chemical shift tensor. From a combination of TG and DSC measurements taken under an argon atmosphere, we found that the mass of adduct 1 is lost in two steps involving initial desorption of coordinated py molecules with subsequent thermal destruction of liberated cadmium(II) di-iso-butyldithiocarbamate, with yellow-orange, fine-powdered solid CdS as the final product.

• 出版日期2011-3-15