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TITLE
DEDICATION
CERTIFICATE
DECLARATION
ACKNOWLEDGEMENT
CONTENTS
Preface
LIST OF TABLES
LIST OF FIGURES
List of Notations and Abbreviations
1 Introduction
1.1 Iron-General Chemistry
1.1.1 Iron (III) -Coordination Chemistry
1.1 Various coordination geometries displayed by iron (III) complexes
1.1.2 Iron (III) -Electronic Spectra and Magnetism
1.2 Cobalt-General Chemistry
1.2.1 Cobalt (II) -Coordination Chemistry
1.2 Various coordination geometries displayed by cobalt (II) complexes
1.2.2 Cobalt (II) -Electronic Spectra and Magnetism.
1.1 Orgel diagram for tetrahedral and octahedral cobalt (II)
1.3 Nickel-General Chemistry
1.3.1 Nickel (II) -Coordination Chemistry
1.3 Various coordination geometries displayed by nickel (II) complexes
1.2 d-orbital splitting pattern for tetrahedral, octahedral, tetragonally distorted and square planar Ni2+
1.3.2 Nickel (II) -Electronic Spectra and Magnetism.
1.4 Copper-General Chemistry
1.4.1 Copper (II) -Coordination Chemistry
1.4 Various coordination geometries displayed by copper (II) complexes
1.4.2 Copper (II) -Electronic Spectra and Magnetism.
1.3 Splitting of 2E, and 2T2, states in copper (II)
1.5 Application of Transition Metal Complexes
1.6 First Row Transition Metal Complexes of Antipyrine and its Derivatives: A Review
2 Reagents and Physicochemical Methods
2.1 Reagents
2.1.1 Metal Salts
2.1.2 Schiff Bases
2.1.3 Solvents Used
2.1.4 Other Reagents
2.2 Analyses of Complexes
2.2.1 Estimation of Metal Content
Estimation of Iron
Estimation of Cobalt
Estimation of Nickel
Estimation of Copper
2.2.2 Estimation of Perchlorate Content
2.2.3 Estimation of Halide Content
2.3 Physicochemical Methods Used in the Present Study
2.3.1 Electrical Conductance
2.3.2 Magnetic Susceptibility
2.1 Molar conductance of the complexes dissolved in some selected solvents
2.3.3 Infrared Spectra
Ligand Vibrations Characteristic of the Ligand
Skeletal Vibrations Characteristic of the Whole Complex Molecule
Coupled Vibrations
i) The Coordination Site of the Ligand
ii) The Relative Strength of Metal-ligand Bond
iii) The Coordination Nature of Anion
Perchlorate Ion
2.2 Vibrations of the perchlorate ion as a function of symmetry
Nitrate Ion
Thiocyanate Ion
Halide Ions
Metal-oxygen and Metal-nitrogen Vibrations
2.3.4 Electronic Spectra
2.3.5 EPR Spectra
2.3.6 Thermal Studies
Thermogravimetry (TG)
Advantages of Non-isothermal Method
Derivative Thermogravimetry (DTG)
Differential Thermal Analysis (DTA)
Applications of Thermogravimetry in Solids
i) Phenomenological Aspects
ii) Kinetic Aspects
2.3 Commonly used g (α) forms for solid state reactions
2.3.7 Analysis of Carbon, Hydrogen and Nitrogen
3 Studies on lron (III), Cobalt (ll), Nickel (II) and Copper (ll) Complexes of N, N-Bis (4-antipyrylmethylidene) ethylenediamine
3.1 N, N-Bis (4-antipyrylmethylidebe) ethylenediamine
3.1 Preparation of the Complexes
Iron (III) Complexes
Cobalt (II) Complexes
Nickel (II) Complexes
Copper (II) Complexes
3.2 Results and Discussion
3.2.1 Appearance and Solubility of the Complexes
3.2.2 Elemental Analyses
3.2.3 Electrical Conductance
3.2.4 Infrared Spectra
Iron (III) Complexes
Cobalt (II) Complexes
Nickel (II) Complexes
Copper (II) Complexes
3.2.5 Electronic Spectral Studies
3.2.6 Magnetic Behaviour
3.2.7 EPR Spectra
3.2 EPR spectra of the copper (II) complexes of BAME
3.3 Summary and Conclusion
3.3 Tentative structures of iron (III) complexes of BAME
3.4 Tentative structure of cobalt (II) complexes of BAME
3.5 Tentative structure of nickel (II) complexes of BAME
3.6 Tentative structure of copper (II) complexes of BAME
4 Studies on lron (IIl), Cobalt (Il), Nickel (lI) and Copper (ll) Complexes of N-Benzoyl-N- (4-antipyrylmethylidene) hydrazine
4.1 N-Benzoyl-N- (4-antipyrylmethyl idene) hydrazine (BAMH)
4.1 Preparation of the Complexes
4.2 Results and Discussion
4.2.1 Appearance and Solubility of the Complexes
4.2.2 Elemental Analyses
4.2.3 Electrical Conductance
4.2.4 Infrared Spectra
4.2.5 Electronic Spectral Studies
4.2.6 Magnetic Behaviour
4.2.7 EPR Spectra
4.2 EPR spectra of copper (II) complexes of BAMH
4.3 Summary and Conclusion
4.3 Tentative structures of iron (III) complexes of BAMH
4.4 Tentative structure of cobalt (II) complexes of BAMH
4.5 Tentative structures of nickel (II) complexes of BAMH
4.6 Tentative structures of copper (II) complexes of BAMH
5 Thermal Studies on Complexes of Iron (Ill), Cobalt (ll), Nickel (II) and Copper (ll) with Some Antipyrine Derivatives
5.1 Experimental
5.1.1 Preparation of the Ligands and the Complexes
5.2 Results and Discussion
5.3 Phenomenological Aspects
5.3.1 Complexes of BAME
5.3.1.1 Structure-Thermal Stability Relation
5.3.2 Complexes of BAMH
5.3.2.1 Structure-Thermal Stability Relation
5.4 Kinetic Aspects
5.4.1 Complexes of BAME
5.4.2 Complexes of BAMH
5.5. Mechanistic Aspects
5.6. Summary and Conclusion
6 Summary and Conclusion
6.1 Complexes of BAME
6.2 Complexes of BAMH
6.3 Thermal Studies on Complexes of BAME and BAMH
6.4 Future Scope of the Work
3.1 Analytical data of the iron (III) complexes of BAME
3.2 Analytical data of the cobalt (II) complexes of BAME
3.3 Analytical data of the nickel (II) complexes of BAME
3.4 Analytical data of the copper (II) complexes of BAME
3.5 Molar conductance data of the iron (III) complexes of BAME
3.6 Molar conductance data of the cobalt (II) complexes of BAME
3.7 Molar conductance data of the nickel (II) complexes of BAME
3.8 Molar conductance data of the copper (II) complexes of BAME
3.9 Important infrared spectral bands (cm-1) of BAME and its iron (III) complexes
3.10 Important infrared spectral bands (cm-1) of BAME and its cobalt (II) complexes
3.11 Important infrared spectral bands (cm-1f) of BAME and its nickel (II) complexes
3.12 Important infrared spectral bands (cm-1) of BAME and its copper (II) complexes
3.13 Electronic spectral data and magnetic moments of iron (III) complexes of BAME
3.14 Electronic spectral data and magnetic moments of cobalt (II) complexes of BAME
3.15 Electronic spectral data and magnetic moments of nickel (II) complexes of BAME
3.16 Electronic spectral data and magnetic moments of copper (II) complexes of BAME
3.17 EPR bonding parameters of the copper (II) complexes of BAME in 1: 1 methanol-toluene at liquid nitrogen temperature
4.1 Analytical data of the iron (III) complexes of BAMH
4.2 Analytical data of the cobalt (II) complexes of BAMH
4.3 Analytical data of the nickel (II) complexes of BAMH
4.4 Analytical data of the copper (II) complexes of BAMH
4.5 Molar conductance data of the iron (Ill) complexes of RAMH
4.6 Molar conductance data of the cobalt (II) complexes of BAMH
4.7 Molar conductance data of the nickel (II) complexes of KAMH
4.8 Molar conductance data of the copper (II) complexes of BAMH
4.9 Important infrared spectral bands (cm-1) of BAMH and its iron (III) complexes
4.10 Important infrared spectral bands (cm-1) of BAMH and its cobalt (II) complexes
4.11 Important infrared spectral bands (cm-1) of BAMH and its nickel (ll) complexes
4.12 Important infrared spectral bands (cm-1) of BAMH and its copper (II) complexes
4.13 Electronic spectral data and magnetic moments of the iron (III) complexes of BAMH
4.14 Electronic spectral data and magnetic moments of the cobalt (II) complexes of BAMH
4.15 Electronic spectral data and magnetic moments of the nickel (II) complexes of BAMH
4.16 Electronic spectral data and magnetic moments of the copper (II) complexes of BAMH
4.17 EPR bonding parameters of the copper (II) complexes of BAMH at liquid nitrogen temperature
5. 1 Phenomenological data for the thermal decomposition of the nitrate complexes of iron (III), cobalt (II), nickel (II), and copper (II) with BAME
5.2 Phenomenological data for the thermal decomposition of the nickel (II) complexes of BAME
5.3 Phenomenological data for the thermal decomposition of the nitrate complexes of iron (III), cobalt (II), nickel (II), and copper (II) with BAMH
5.4 Phenomenological data for the thermal decomposition of the nickel (II) complexes of BAMH
5.5 Kinetic parameters for the thermal decomposition of the nitrate complexes of iron (III), cobalt (II), nickel (II), and copper (II) with BAME
5.6 Kinetic parameters for the thermal decomposition of the nickel (II) complexes of BAME
5.7 Kinetic parameters for the thermal decomposition of the nitrate complexes of iron (III), cobalt (II), nickel (II), and copper (II) with BAMH
5.8 Kinetic parameters for the thermal decomposition of the nickel (II) complexes of BAMH
5.9 Correlation coefficients calculated using the nine forms of g (α) for the nitrate complexes of iron (III), cobalt (II), nickel (II) and copper (II) with BAME
5.10 Correlation coefficients calculated using the nine forms of g (α) for the nickel (II) complexes of BAME
5.11 Correlation coefficients calculated using the nine forms of g (α) for the nitrate complexes of iron (III), cobalt (II), nickel (II) and copper (II) with BAMH
5.12 Correlation coefficients calculated using the nine forms of g (α) for the nickel (II) complexes of BAMH
5.1 TG and DTG curves of [Fe (BAME) 2 (NO3] (N03) 2
5.2 TG and DTG curves of [Co (BAME) 2] (N03) 2
5.3 TG and DTG curves of [Ni (BAME) 2] (N03) 2
5.4 TG and DTG curves of [Cu (BAME) 2] (N03) 2
5.5 TG and DTG curves of [Ni (BAME) 2] (CI04) 2
5.6 TG and DTG curves of [Ni (BAME) 2]C12
5.7 TG and DTG curves of [Ni (BAME) 2]Br2
5.8 TG and DTG curves of [Ni (BAME) 2]I2
5.9 TG and DTG curves of [Fe (BAMH) 2 (N03) ] (NO3) 2
5.10 TG and DTG curves of [Co (BAMH) 2] (NO3) 2
5.11 TG and DTG curves of [Ni (BAMH) 2 (NO3) ] (NO3)
5.12 TG and DTG curves of [Cu (BAMH) 2] (NO3) 2
5.13.TG and DTG curves of [Ni (BAMH) 2 (CI04) ] (CI04)
5.14 TG and DTG curves of [Ni (BAMH) 2C12]
5.15 TG and DTG curves of [Ni (BAMH) 2Br2]
5.16 TG and DTG curves of [Ni (BAMH) 2I2]
5.17 Log [g (α) /T2] vs 1000/T plots for the thermal decomposition of the nitrate complexes of iron (III), cobalt (II), nickel (II), and copper (II) with BAME
5.18 Log[g (α) /T2j vs I000/T plots for the thermal decomposition of the nickel (II) complexes of BAME
5.19 Log [g (α) /T2]vs 1000/T plots for the thermal decomposition of the nitrate complexes of iron (III), cobalt (Il), nickel (II), and copper (II) with BAMH
5.20 Log[g (α) /T2] vs 1000/T plots for the thermal decomposition of the nickel (II) complexes of BAMH
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