Synthesis, Characterization, and X-Ray Structure of Bis(O-butyldithiocarbonato)bis(3-ethyl pyridine)nickel(II)

Inderjeet Kaur,Rajni Kant,Gurvinder Kaur,Renu Sachar,Vivek K Gupta,Kuldeep Singh

doi:10.1155/2014/642839

Abstract

A new series of additional complexes of bis(O-butyldithiocarbonato)nickel(II) with ethylpyridines have been prepared and characterized by physicochemical techniques like elemental analysis, molar conductance measurements, TGA-DTA and UV-visible electronic spectroscopy, and IR-spectral data. The structure of [Ni(S2COC4H9)2(C7H9N)2] has been established by X-ray crystallography. The complex crystallizes in the monoclinic space group P1/n with unit cell parameters a=14.0721(6), b=7.0078(2), and c=15.3604(7) Å and α=90.00, β=108.065(5), and γ=90.00°. The Ni atom in the title complex is octahedrally coordinated within a trans-N2S4 donor set, with the Ni atom located on a centre of inversion. Crystal structure was solved by direct methods and refined by full matrix least squares procedures to a final R-value of 0.0545 for 1984 observed reflections. The butyl chain is disordered over two sets of sites, with occupancy ratio of 0.572 : 0.427.

Highlights

O-alkyldithiocarbonate (ROCS2−), named xanthate, represents an important class of 1, 1 dithiolato ligands which have been studied extensively [1, 2]
As a part of our ongoing research on nickel(II) xanthate complexes with substituted pyridines, we report here the synthesis and characterization of 1 : 2 adducts of bis(O-butyldithiocarbonato)nickel(II) with ethyl pyridines and the crystal structure of the adduct bis(Obutyldithiocarbonato)bis(3-ethylpyridine)nickel(II)
The plane formed by the atoms Ni1, S1, C1, and S2 makes a dihedral angle of 88.20(9)∘ with the plane of ethyl-pyridine ring, meaning thereby that both planes are held almost perpendicular to each other

Summary

Introduction

O-alkyldithiocarbonate (ROCS2−), named xanthate, represents an important class of 1, 1 dithiolato ligands which have been studied extensively [1, 2]. These compounds form water insoluble complexes with most of the transition metals and are extensively employed for the separation and quantitative determination of cations of transition metals [3]. Xanthates as ligand are extensively studied for a wide variety of structural features. They are known to coordinate as a monodentate, bidentate, or as a bridging ligand. As a part of our ongoing research on nickel(II) xanthate complexes with substituted pyridines, we report here the synthesis and characterization of 1 : 2 adducts of bis(O-butyldithiocarbonato)nickel(II) with ethyl pyridines and the crystal structure of the adduct bis(Obutyldithiocarbonato)bis(3-ethylpyridine)nickel(II)

Experimental

Synthesis of the Title Complex

Results and Discussion

C O CH2 CH2 CH2 CH3

O2 C31A