A series of new complex salts of the type [A]2[MCl2I2] where A=1,3,5-trimethylpyridinium cation, M= Mn+2,Co+2, Ni+2,Cu+2 and Zn+2 were prepared by the reaction of the metal chloride and 1,3,5-trimethylpyridinium iodide in (1:2) molar ratio and characterized by elemental analysis, molar conductance, IR, Uv/Vis., spectral studies and magnetic measurements. The crystal structure of 1,3,5-trimethylpyridinuim iodide was determined by single crystal x-ray crystallography.
The structure of the anion part and a 1,3,5- trimethylpyridinium cation which crystallizes in the orthorhombic space group (Cmcm) with a=8.9850(9), b=15.767(2), c=6.9940(6)A°, V=990.82 (16)A°, Z=4. Which is on a crystallographic mirror plane perpendicular to C-axis except for methyl hydrogen atoms. The anion and cation are connected through hydrogen bonds between I and the cation by hydrogen bonding, electrostatic interaction and weak π-π interaction are also expected.
Table of Contents
1. Abstract
2. Introduction
3. Experimental
4. Synthesis
4.1 1,3,5-trimethylpyridinium iodide
4.2 Preparation of [C8H12N]2[MnCl2I2]
4.3 [C8H12N]2[CoCl2I2]
4.4 [C8H12N]2[NiCl2I2]
4.5 [C8H12N]2[CuCl2I2]
4.6 [C8H12N]2[ZnCl2I2]
4.7 Crystallography
5. Results and Discussion
Research Objectives and Key Topics
The primary objective of this study is the synthesis and comprehensive characterization of new transition metal complex salts based on the 1,3,5-trimethylpyridinium cation, specifically examining their structural, magnetic, and spectroscopic properties to understand the interactions between the anion and cation components.
- Synthesis of [A]2[MCl2I2] complex salts (M = Mn, Co, Ni, Cu, Zn).
- Determination of the crystal structure of 1,3,5-trimethylpyridinium iodide.
- Physicochemical characterization using IR, Uv/Vis, and magnetic measurements.
- Analysis of packing interactions and electrostatic bonding in the crystalline state.
Excerpt from the Book
Crystallography
A yellow block specimen crystal (0.24x0.2x0.17 mm3) was mounted on the RIGAKU R-AxIs PAPIDIP camera. The diffraction data was measured at 169(2)K using Mok X-ray (=0.71073A). The crystal structure was solved by direct methods (SHELEX-97 (Sheldrick, 2008) and refried by full-matrix least-squares (SHELEX-97 (Sheldrick, 2008) with anisotropic temperature factors. Hydrogen atoms were located by geometrical calculations and included in the calculation using riding atom model. Crystallographic data and geometrical parameter are listed on Table 1 and 2, respectively.
Summary of Chapters
1. Abstract: Provides a concise overview of the synthesis of the new complex salts and the determination of the crystal structure of the pyridinium salt.
2. Introduction: Reviews existing literature on transition metal halide complexes and their structural/magnetic studies, establishing the rationale for the current investigation.
3. Experimental: Details the chemical materials used, the preparation conditions under nitrogen atmosphere, and the analytical instruments employed for characterization.
4. Synthesis: Documents the step-by-step preparation procedures for the 1,3,5-trimethylpyridinium iodide and the specific transition metal complexes (Mn, Co, Ni, Cu, Zn), including crystallography methods.
5. Results and Discussion: Analyzes the collected experimental data, including IR spectra, magnetic measurements, Uv/Vis electronic spectra, and the crystal structure interpretation.
Keywords
Pyridinium Salt, Crystal Structure, 1,3,5-Trimethylpyridinium Iodide, Transition Metal Complexes, Mn(II), Co(II), Ni(II), Cu(II), Zn(II), X-ray Crystallography, Infrared Spectroscopy, Magnetic Moment, Electronic Spectra, Coordination Chemistry, Electrostatic Interaction.
Frequently Asked Questions
What is the core focus of this research?
The research focuses on the synthesis and characterization of a series of novel complex salts involving the 1,3,5-trimethylpyridinium cation and various transition metal chlorides.
Which metal ions were investigated?
The study examines Manganese (Mn+2), Cobalt (Co+2), Nickel (Ni+2), Copper (Cu+2), and Zinc (Zn+2) complex salts.
What is the main research objective?
The primary goal is to synthesize these compounds and determine their physicochemical properties, particularly the crystal structure of the organic salt component and the bonding nature within the complexes.
What scientific methods were applied?
The authors utilized elemental analysis, molar conductance, infrared (IR) and ultraviolet-visible (Uv/Vis) spectroscopy, magnetic measurements, and single-crystal X-ray crystallography.
What topics are covered in the main section?
The main sections cover the experimental synthesis, the determination of crystal parameters, and the analysis of bonding, geometry, and electronic transitions.
How would you characterize this work with keywords?
The work is defined by terms such as Pyridinium Salt, Crystal Structure, 1,3,5-Trimethylpyridinium Iodide, and transition metal coordination chemistry.
What does the crystal structure analysis reveal about the pyridinium cation?
The analysis shows that the 1,3,5-trimethylpyridinium cation crystallizes in the orthorhombic space group (Cmcm) and features mirror plane symmetry.
How do the cation and anion interact in the crystal structure?
The structure reveals that the components are connected through hydrogen bonding between iodine and the cation, alongside electrostatic interactions and weak pi-pi stacking.
- Citation du texte
- Amer Taqa (Auteur), Nebeel H. Buttrus (Auteur), Eman M. Rumadthan (Auteur), H. Uekusa (Auteur), 2012, Synthesis and Characterization of Mn+2, Co+2, Ni+2, Cu+2 and Zn+2, Munich, GRIN Verlag, https://www.grin.com/document/209002
