Institute of Chemical Sciences

CHEM-451-I

Advance Inorganic Chemistry Lab-I

Semester Lab Report

Submitted To:

[Link] Tariq

Associate Professor

Submitted By:

Iqra Haq

BS-CH-22-33

Semester 7 (Inorganic Major)

Date of Submission:

15 December 2025

Table of contents
1 Synthesis and characterization of tris(acetylacetonato) chromium (III) complex

2 Synthesis and characterization of bis(acetylacetonate) Cu(III) complex

3 Synthesis and characterization of tris (acetylacetonato) Iron (III) complex

4 Synthesis and characterization of tris (acetylacetonato) Mn (III) complex

5 Synthesis and characterization of tris acetylacetonato Al(III) complex

6 Synthesis of Zn(II) oxalate

7 Synthesis of Cu(II) oxalate

8 Synthesis of Magnese( II) complex

9 Synthesis of Nickel (II) oxalate

10 Synthesis of potassium Tris(oxalato) chromate (III) complex

11 Synthesis of potassium Tris (oxalato)aluminate (III)

12 Synthesis of Nickel (II) Anthranilate

Synthesis and characterization of tris (acetylacetonato)

chromium (III) Complex
Abstract
Tris (acetylacetonato) chromium(III) complex was prepared using a laboratory-scale
synthesis method and its properties were investigated. Chromium(III) salt was allowed
to react with acetylacetone under basic conditions to obtain the desired coordination
compound. The synthesized complex was subjected to spectroscopic analysis to verify
its formation. Infrared spectroscopy was used to identify the bonding mode of the
acetylacetonate ligands, while UV–Visible spectroscopy was employed to study the
electronic transitions of the chromium(III) center. The experimental observations
confirmed the formation of a stable octahedral chromium(III) complex. Such metal–
acetylacetonate complexes are widely studied due to their significance in inorganic
chemistry and their applications in various industrial and research fields.

1 Introduction
Coordination compounds play an important role in inorganic chemistry due to their
diverse structures and applications. Tris(acetylacetonato) chromium(III) is a well-known
coordination complex containing chromium in the +3 oxidation state acts as a bidentate
ligand and forms stable chelate rings with the metal [Link] synthesis of this complex
helps in understanding metal–ligand bonding and chelation effects. Characterization
techniques are essential to confirm the formation and structure of the complex. Infrared
spectroscopy is used to identify ligand coordination through metal–oxygen [Link]–
Visible spectroscopy provides information about the electronic structure of the
chromium(III) complex.

2 Experimental

2.1 Chemicals
Chromium chloride hexahydrate (CrCl2.6H2O), Urea, Acetylaceton and distilled water
were purchased from Sigma Aldrich and used as such without any purification.

2.2 Synthesis of tris (acetylacetonato )chromium ( III) Complex

100ml of distilled water will be taken in be 250ml Beaker 2.69g(10mmol) of chromium
chloride hexahydrate will be added to beaker 10g (165 mmol) of Urea and 6.18mL of
acetylacetone will be added to beaker The mixture will be covered by watch glass and
heated by placing the large beaker of boiling water for 90 min. The mixture will be
allowed to cool and product will be collected by Filtration. The crystals will be washed
distilled and air dried. The % yield water and air will be collected

3 Result and discussion

The tris (acetylacetonato) chromium( III )Complex was prepared by reaction of
chromium chloride hexahydrate and acetylacetone. The physical data is given in table
1

Properties Ligand Complex

Colour Colourless Violet or purple
Melting point (C) ____ 180-190
Molar mass (g/mol) 100.13 349.32
Magnetic moment (B.M) ___ 3.87
Magnetic Behavior ___ Paramagnetic
Hybridization and energy ___ d2sp3
CFSE(Dq) ___ -12

4.1 Spectroscopic Characterization

4.1.1 UV Visible spectral Analysis F

Acetylacetone exhibits weak absorption below 300 nm in the UV region due to π→π*
transitions of its conjugated enone system . In its predominant enol form, this
intramolecularly hydrogen-bonded chelate ring shows a slightly red-shifted absorption
Fig:1 UV visible spectrum of acetylacetone
Fig:1 UV Visible spectrum of acetylacetone
Cr(III) complexes typically exhibit absorption bands in the visible region due to d-d
transitions. These often appear as two main bands, one around 400-500 nm (violet-blue
absorption) and another near 550-600 nm (yellow-orange absorption). The transmitted
or reflected light is therefore green or violet, depending on the exact ligand field.

Fig: 2 UV visible spectrum of Cr(acac)3

Characteristic strong broad band around 1600-1700 cm⁻¹ for C=O stretching. Sharp
band near 1520 cm⁻¹ for C=C stretching in the enol form. Broad band around 3000 cm⁻¹
for intramolecular hydrogen-bonded O-H stretch
The dominant enol form shows a very broad O-H stretch at 2500-3000 cm⁻¹ from
intramolecular hydrogen bonding. Strong coupled C=O/C=C stretches appear near 1620
& 1580 cm⁻¹. Sharp methyl C-H stretches (~2950 cm⁻¹) sit atop the broad O-H band.

The FTIR spectrum of Cr(acac)⁻ shows strong bands around 1500-1600 cm⁻¹ due to
ν(C=O) and ν(C=C) stretches of the chelated acac ligand. Key features include a sharp
peak near 1520 cm⁻¹ for ν(C=O) and around 1570 cm⁻¹ for ν(C=C), indicating enolate
formation. Additional peaks appear for δ(C-H) near 1350 cm⁻¹ and ring vibrations below
1000 cm⁻¹.

Fig:4 FTIR spectrum of acetylacetonato chromium III Complex

Conclusion
In this report we have been provided import characterization and synthesis of Tris
acetylactonato chromium III complex.
2 Synthesis and characterization of bis(acetylacetonato) copper (II) complex

Abstract
Bis(acetylacetonato)copper(II) Cu(acac)2 was synthesized through a ligand exchange
reaction between copper(II) salts and acetylacetone. The complex was purified and its
formation was confirmed using various techniques, including UV-Vis, FTIR spectroscopy
, and magnetic susceptibility measurements.

1 Introduction
Bis(acetylacetonato)copper(II), or Cu(acac)2, is a foundational coordination complex
recognized for its vibrant blue color and remarkable stability. Its structure involves
aCu^2+ ion held in a square planar geometry by two bidentate ligands acac-, forming
two robust six-membered chelate rings. This combination of stability and organic
solubility makes it an invaluable, versatile reagent.

2 Experimental

2.1 chemicals:

Copper (II) chloride dihydrate, sodium acetate - acetone, methanol & distilled water

2.2 Synthesis of bis(acetylacetonato)copper(II)complex

In a beaker 1.36g of copper (II) chloride dissolved in 12.5mL distilled waters over a
period of 10 min with stirring.2.5mL acetylacetone solution solution in 5min methanol
was added in it over 5min continuous stirring of sodium acetate in 12.5mL distilled. 3.49
water was added in above solution. The reaction was heated to 80°C, followed by
cooling in an ice bath. The precipitates were Filtered, washed with cold water and dried
in oven at 100°C- The percentage yield was calculated.

3 Results and discussion

The Cu(acac)2 was prepared by reaction of copper II chloride with acetylacetone in
presence of sodium acetate. The physical data is given in table 2

Properties Acetylacetone Cu(acac)2

Colour Colourless Blue to gray
Melting point (C) _____ 240-250
Magnetic moment (B.M) _____ 1.8 B.M
Magnetic Behavior _____ Paramagnetic
CFSE(Dq) _____ -12
4.1Spectroscopic Characterization
4.1.1 UV visible spectral Analysis Acetylacetone primarily absorbs in the UV
region (below 350 nm) due to π→π* and weak n→π* transitions of its conjugated enone
system. It is colorless in solution as it possesses no significant absorption in the visible
spectrum. The exact peak position is influenced by its tautomeric equilibrium between
ketone and enol.

Fig:1 UV Visible spectrum of acetylacetone The UV-Visible spectrum of

Cu(acac)⁻ features intense ligand-based UV bands (<300 nm), a ligand-to-metal
charge transfer band (~300-350 6), and a broad, weak d-d band in the visible region
(~600-700 nm), which gives the complex its characteristic bluish-green color.

Fig:2 UV visible spectrum of bis(acetylacetonato) copper II complex

The FTIR spectrum of acetylacetone (1,3-diketo form) shows a strong, broad O–H
stretch around 3000–2700 cm⁻¹ from intramolecular hydrogen bonding, a sharp C=O
stretch around 1705 cm⁻¹ (ketonic) and 1630 cm⁻¹ (enolic, H-bonded), and C–H
stretches near 2900 cm⁻¹.
 Fig:3 FTIR spectrum of acetylacetone
The FTIR spectrum shows a characteristic broad enol C=O stretch around 1600 cm⁻¹,
indicating Chelation. The O–H stretch (~3000 cm⁻¹) is absent, confirming
deprotonation. Peaks for C–H and C–C stretches from the acetylacetonate rings appear
in the 1500-1300 cm⁻¹ region.
The FTIR spectrum of Cu(acac)₂ is defined by chelation shifts. The key spectrum

disappearance of the sharp ~1710 cm⁻¹ C=O peak of free acetylacetone. Instead, two
strong bands near 1575 cm⁻¹ and 1520 cm⁻¹ appear due to coupled C=O/C=C
stretches in the resonant chelate ring. A broad, weak band around 700 cm⁻¹
corresponds to the Cu–O bond. These two strong peaks in the 1520-1600 cm⁻¹ range
are the definitive fingerprint of the complex.

Conclusion
This report provides a comprehensive analysis of bis(acetylacetonato) cupper II
complex

3 Synthesis and characterization of tris acetylacetonato Iron (III) complex

Abstract
The complex tris(acetylacetonato) iron(III),Fe(acac)3 , was successfully synthesized
through the direct reaction of Fe^+3ions and acetylacetone under controlled PH
conditions. The resulting product was isolated as a stable, crystalline dark-red solid with
high purity. IR spectroscopy confirmed the characteristic vibrational shifts indicative of
the acac ligand's bidentate chelation to the central iron atom. UV-Vis analysis supported
the high-spin, Fe(III) coordination environment. This preparation provides a highly
effective and foundational laboratory method. The resulting complex is a key reference
material in coordination and catalytic

1 Introduction
The Fe(acac)3 complex features an Fe^+3center coordinated to three bidentate
acetylacetonate acac^- ligands. Each ligand uses its two oxygen atoms to form stable,
six-membered chelate rings. This results in a stable, neutral molecule with an
octahedral geometry. The complex is a dark red, crystalline solid and exhibits solubility
in nonpolar organic solvents. It is structurally defined by its d5 high-spin configuration.
Fe(acac)3 is widely used as a precursor in materials science and as a catalyst.

2 Experimental

2.1 Chemicals
Ferric chloride hexahydrate ( FeCl3) , acetylacetone (acacH), sodium acetate, distilled
water and methanol were purchased from Sigma Aldrich and used as such without any
further purification.

2.2 Synthesis of tris (acetylacetonato) Iron(III) complex

In a beaker 1.36g(of copper (II) chloride was dissolved in 12.5ml distilled water over
period of 10 min with stirring, 3.4 g(2.4 mmol) of sodium acetate in 12.5ml distilled water
was added in above solution . The reaction mixture was heated. By cooling in a ice
bath. The precipitates was Filtered, washed with cold water and dry in oven at 100C.
The % yield was calculated.

3 Results and discussion

The Fe (acac)3 was prepared by reaction of Iron III chloride with acetylacetone. The
physical data is given in table 3

Properties Ligand Complex

 Colour Colourless Orange to red-orange
Melting point(C) ____ 180-185C
Magnetic moment (B.M) ____ 5.92
CFSE(Dq) ____ 0
4.1 Spectroscopic characterization
4.1.1 UV Visible Spectral Analysis Acetylacetone primarily absorbs in the UV region
(below 350 nm) due to π→π* and weak n→π* transitions of its conjugated enone
system. It is colorless in solution as it possesses no significant absorption in the visible
spectrum. The exact peak position is influenced by its tautomeric equilibrium between
ketone and enol.

The UV-Vis spectrum of Fe(acac)⁻ features intense ligand-centered π→π transitions*

in the UV region (~280-350 nm). In the visible region, it typically shows a broad,
moderately intense ligand-to-metal charge transfer (LMCT) band around 400-500 nm,
often appearing yellowish-orange. This LMCT band and the pale yellow to orange color
result from the transfer of electron density from the oxygen p-orbitals of the acac ligand
to the Fe³⁺ center.

The FTIR spectrum of acetylacetone (Hacac) shows a strong, sharp carbonyl (C=O)
stretch at ~1710 cm⁻¹ due to its keto form. A medium-intensity C=C stretch appears at

~1625-1640 cm⁻¹, indicating significant enol tautomer presence. A broad O–H stretch is
visible at ~2800-3000 cm⁻¹ for the enol's intramolecular hydrogen bond. In-plane and
out-of-plane O–H bending modes are seen around ~1410 cm⁻¹ and ~950 cm⁻¹,
respectively. Methyl group (C–H) stretches are present near ~2950-3000 cm⁻¹. . The
spectrum confirms the enol-keto tautomer equilibrium in the liquid or solid state.
Fig 3 FTIR spectrum of acetylacetone

The FTIR spectrum of Fe(acac)⁻ is nearly identical to Cu(acac)⁻, showing the same
key fingerprint: the disappearance of the free C=O stretch (~1710 cm⁻¹) and its
replacement by two strong, coupled ν(C=O+C=C) bands in the 1520-1600 cm⁻¹ region
due to chelate ring resonance. Fig 4 FTIR spectrum of tris (acetylacetonato )Iron III
complex
Conclusion This report has been successfully summarized synthesis of
Tris(acetylacetonato) cupper(II) .
Synthesis and characterization of tris acetylacetonato Mn(III) Complex
Abstract. The
tris(acetylacetonato)manganese(III) complex was synthesized and characterized by
elemental analysis, FTIR, and UV-Vis spectroscopy, confirming its octahedral geometry.
Magnetic susceptibility measurements indicated the high-spin d⁴ configuration with four
unpaired electrons.
[Link] Manganese(III) acetylacetonate,
[Mn(acac)⁻], is a classic coordination compound exemplifying octahedral geometry with
O⁻ donor set. Its synthesis via simple metathesis reaction provides a fundamental
study in transition metal chemistry. This complex is pivotal for exploring Jahn-Teller
distortion, redox behavior, and serves as a precursor in materials science.
[Link] 2.1 Chemicals
Manganese chloride tetrahydrate, sodium acetate, Acetylacetone, potassium
permanganate and distilled water

2.2 Synthesis of tris( acetylacetonato) Mn( III) complex

2.5 g (15.4 mmol) of powdered KMnO⁻ was dissolved in a minimum volume of water
by slight warming over a steam bath. The solution was filtered . 11g(approx. 73.5%
excess) of acetylacetone was added with vigorous stirring. The mixture was stirred for 5
minutes and then was allowed to cool for 40 minutes. Stirring was continued, and the
beaker was heated on a hot plate to 60–70 °C for 15 minutes. The mixture was cooled
to room temperature and then was placed in an ice bath. The dark precipitate was
formed, filtered, and washed using a small amount of cold distilled water. Finally, the
product was dried and was saved in a glass vial.

3 Result and discussion

Tris acetylacetonato Mn III complex was successfully prepared by reaction of MnCl2
and Acetylacetone.

The physical data is given in table

Properties Ligand Complex

Color Colour less Dark brown
Melting point (C) _____ 180-185C
Magnetic moment (B.M) _____ 4.89
CFSE(Dq) _____ -6 Dq

4 Spectroscopic characterization

4.1 UV visible spectral Analysis

Acetylacetone exhibits weak absorption below 300 nm in the UV region due to π→π*
transitions of its conjugated enone system . In its predominant enol form, this
intramolecularly hydrogen-bonded chelate ring shows a slightly red-shifted absorption

Fig 1 UV visible spectrum of acetylacetone

The spectrum shows strong UV ligand-based π→π* transitions near 260 nm and 350
nm. A broad, weak band in the visible region (~450-550 nm) corresponds to spin-
forbidden d-d transitions of the high-spin d⁴ Mn(III) ion. This absorption pattern results in
the characteristic green color of the complex.

Fig 2 UV visible spectrum of tris acetylacetonato Mn III complex

The FTIR spectrum of acetylacetone (1,3-diketo form) shows a strong,

broad O–H stretch around 3000–2700 cm⁻¹ from intramolecular hydrogen bonding, a
sharp C=O stretch around 1705 cm⁻¹ (ketonic) and 1630 cm⁻¹ (enolic, H-bonded), and
C–H stretches near 2900 cm⁻¹.
FTIR spectrum of tris acetylacetone

The FTIR spectrum of Mn(acac)⁻ shows the hallmark of chelation: two strong bands at
~1570 cm⁻¹ (asymmetric C-O/C-C stretch) and ~1510 cm⁻¹ (symmetric stretch) from the
delocalized enolate ring. The free C=O stretch (~1710 cm⁻¹) disappears, replaced by
these lower-energy peaks. Additional features include C-H stretches (~2900 cm⁻¹),
methyl bends (~1380 cm⁻¹), and C-H out-of-plane bends (~790 cm⁻¹).

Fig 4 FTIR spectrum of tris acetylacetonato Mn III complex

Conclusion This report has been successfully synthesized Tris(acetylacetonato) Mn
complex.
5 Synthesis and characterization of tris( acetylacetonato )Aluminum( III) complex
Abstract This work details the
synthesis of the volatile tris(acetylacetonato)aluminum(III) complex, Al(acac)⁻, via a
metathesis reaction between an aluminum salt and acetylacetone. Comprehensive
characterization using FT-IR and ¹H NMR spectroscopy confirmed ligand coordination
and the complex's high symmetry. Elemental analysis verified its stoichiometry, while
thermogravimetric analysis demonstrated its thermal stability and sublimation behavior.
The collective data confirm the formation of a pure, homoleptic complex with an
octahedral geometry. These properties establish Al(acac)⁻ as a suitable precursor for
materials deposition applications like chemical vapor deposition.
1 Introduction

The tris(acetylacetonato)aluminum(III) complex, Al(acac)⁻, is a highly stable and

volatile metal-organic compound belonging to the class of β-diketonates. It is
characterized by an octahedral geometry where the central aluminum(III) ion is chelated
by three bidentate acetylacetonate ligands. Due to its excellent thermal properties and
well-defined structure, it serves as a fundamental model complex in coordination
chemistry and a crucial precursor for depositing aluminum oxide films in materials
science.

2 Experiment

2.1 Chemicals
Acetylacetone, ammonia solution, Aluminum sulphate and distilled water. All the
chemicals used were purchased from Sigma-Aldrich and were used without any further
purification.

2.2 Synthesis of tris acetylacetonato Aluminum III complex

3 mL acetylactone was added in a conical flask along with 40 mL distilled water which
was followed by 8 mL Dil. Ammonia solution. Aluminum sulphate was dissolved in 30 mL
distilled water. To this solution, the ammonical solution was added gradually with
stirring. After complete addition of acetylactone the solution was checked for neutrality.
The flask was placed in an ice bath until cream colored ppts were formed. The product
was filtered and washed with small amount of distilled water and we’re dried .
Percentage yield was calculated.

[Link] and Discussion:

The complex was prepared by the reaction of aluminum sulphate with the ammonical
solution of acetylactone. The physical data table is given as follows:

Table 1 Physical data of ligand and complex

 Properties Ligand Complex

Color Colour less Pale yellow

Melting point (C) _____ 190-195
Magnetic moment _____ 0
Magnetic Behavior _____ Diamagnetic
CFSE( Dq) _____ 0
4. Spectroscopic characterization

4.1 UV spectral Analysis

Fig 1 UV Visible spectrum of acetylacetone

Acetylacetone primarily absorbs in the UV region (below 350 nm) due to π→π* and
weak n→π* transitions of its conjugated enone system. It is colorless in solution as it
possesses no significant absorption in the visible spectrum. The exact peak position is
influenced by its tautomeric equilibrium between ketone and enol Fig2 Tris

(acetylacetonato) Aluminum (III)complex

Fig 3 FTIR spectrum of tris (acetylacetonato) Aluminum( III )complex

The tris(acetylacetonato)aluminium(III) complex typically shows weak d-d transitions in

the UV region due to its d⁰ electronic configuration. Its spectrum is dominated by intense
ligand-centered π→π* transitions in the ultraviolet range, often below 300 nm. The
complex is usually colorless in solution as it does not absorb significantly in the visible
region (400–700 nm).

Conclusion
This report has been provided important characterization and synthesis of Tris
(acetylacetonato) Aluminum(II) complex.

6 Synthesis of Metal Transition Complexes with oxalic acid

Abstract

Transition metal complexes with oxalic acid (oxalate ligand) are synthesized for Zn, Cu,
Mn, and Ni. These typically form coordination compounds where oxalate acts as a
bidentate chelating agent. The synthesis often involves reacting metal salts (e.g.,
sulfates or chlorides) with oxalic acid or its salt in aqueous solution. The resulting
complexes, such as K2[Zn(ox)2] or [Cu(ox)(H2O)2], vary in geometry and color based
on the metal. They are studied for their magnetic, catalytic, and structural properties.

1Introduction
Oxalic acid, a versatile bidentate ligand, forms stable coordination compounds with
transition metals like Zn, Cu, Mn, and Ni. The synthesis of these complexes involves
simple metathesis reactions between metal salts and oxalate ions in solution, yielding
compounds with distinct geometries and properties. These complexes are fundamental
in coordination chemistry for exploring metal-ligand interactions, magnetism, and their
potential applications in catalysis and materials science.

2 Experimental Synthesis

1Synthesis of Zinc (II) oxalate

Take 0.8g of NaOH in 10 mL of distilled water in a beaker and stirr it to prepare

2M solution of NaOH. Take 1.26g of oxalic acid powder in 10 mL of distilled water in
separate beaker to prepare 1M solution of oxalic acid. Mix both the solution in one
beaker and stirr to make clear solution of sodium salt of oxalic acid. Then take Zinc
acetate and dissolve it in 5 mL of distilled water. Mix the metal salt solution to above
sodium oxalate solution and stirring vigorously. As a result white ppts of zinc oxalate
complex were formed. Filter them and dry at room temperature.

2 Synthesis of Copper (II) oxalate

Take 0.8g of NaOH in 10 mL of distilled water in a beaker and stirr it to prepare
2M solution of NaOH. Take 1.26g of oxalic acid powder in 10 mL of distilled water in
separate beaker to prepare 1M solution of oxalic acid. Mix both the solution in one
beaker and stirr to make clear solution of sodium salt of oxalic acid. Then take Copper
nitrate and dissolve it in 5 mL of distilled water. Mix the metal salt solution to above
sodium oxalate solution and stirring vigorously. As a result dark cyan color ppts of
copper oxalate complex will be formed. Filter them and dry at room temperature.

3 Synthesis of Manganese (II) oxalate

Take 0.8g of NaOH in 10 mL of distilled water in a beaker and stirr it to prepare 2M
solution of NaOH. Take 1.26g of oxalic acid powder in 10 mL of distilled water in
separate beaker to prepare 1M solution of oxalic acid. Mix both the solution in one
beaker and stirr to make clear solution of sodium salt of oxalic acid. Then take
manganese chloride and dissolve it in 5 mL of distilled water. Mix the metal salt solution
to above sodium oxalate solution and stirring vigorously. As a result light brown colored
ppts of manganese oxalate complex will be formed. Filter them and dry at room
temperature.

4 Synthesis of Nickel (II) oxalate

Take 0.8g of NaOH in 10 mL of distilled water in a beaker and stirr it to prepare 2M
solution of NaOH. Take 1.26g of oxalic acid powder in 10 mL of distilled water in
separate beaker to prepare 1M solution of oxalic acid. Mix both the solution in one
beaker and stirr to make clear solution of sodium salt of oxalic acid. Then take Nickel
chloride and dissolve it in 5 mL of distilled water. Mix the metal salt solution to above
sodium oxalate solution and stirring vigorously. As a result light green colored ppts of
Nickel oxalate complex will be formed. Filter them and dry at room temperature.

Result and Discussion

The complexes were successfully synthesized . The physical data table for these
complexes is as follows:

Properties Zinc oxalate Copper oxalate Magnese Nickel oxalate

oxalate
Melting point 100 100-180 Approx. 200-250
100
Magnetic 0 1.73-1.90 5.9-6.1 2.83-3.2
moment ( B.M)
CFSE( Dq) 0 0.6 0 1.2
Spectral Analysis

UV visible spectrum of Zn(oxalate) II complex

Fig 1 UV visible spectrum of Zn(II) oxalate

Zn(II) oxalate typically does not absorb significantly in the visible region (400-700 nm).
Its UV-Vis spectrum usually shows strong charge-transfer or ligand-centered absorption
bands in the ultraviolet range (<400 nm). In aqueous solution, it appears colorless,
indicating no d-d transitions as Zn²⁺ has a d¹⁰ configuration.

FTIR spectrum Analysis

Fig2 FTIR spectrum of Zn(oxalate)II complex

Key FTIR bands: C=O stretching near 1630 cm⁻¹, C-O stretching around 1310 cm⁻¹,
and O-C=O bending near 780 cm⁻¹. Broad band ~3200 cm⁻¹ indicates hydrated water.
Metal-oxygen (Zn-O) vibration appears as a strong band below 500 cm⁻¹.

UV visible spectrum of Magnese(II) oxalate complex

The UV-visible spectrum of the manganese(II) oxalate complex typically shows weak,
broad absorption bands in the visible region due to spin-forbidden d-d transitions. These
bands often appear around 450-550 nm, corresponding to the pale pink color of the
complex. The exact positions can vary slightly based on the specific coordination
environment and concentration.
FTIR spectrum of Magnese (II) oxalate complex

The FTIR spectrum shows strong C=O stretches around 1640-1680 cm⁻¹ and 1360-
1320 cm⁻¹ from the oxalate ligand. A broad feature near 3400 cm⁻¹ indicates lattice or
coordinated water. The spectrum lacks high-energy carbonyl peaks, confirming the
oxalate is coordinated as a bidentate ligand.

Conclusion

The report has been provided important characterization and synthesis of transition
metal complexes with oxalic acid.

9 Synthesis of potassium trisoxalato III complex

Abstract
The potassium tris(oxalato)magnate(III) complex is synthesized and characterized to
study the coordination chemistry of magnesium in the +3 oxidation state. Spectroscopic
techniques confirm the octahedral geometry with oxalate ligands chelating the central
metal ion. Magnetic and thermal analysis reveals its stability and paramagnetic
properties. The complex serves as a model for understanding high-valent magnesium
coordination compounds.
1 Introduction High-valent magnesium complexes are rare and intriguing targets in
coordination chemistry. The potassium tris(oxalato)magnate(III) complex is a classical
example, synthesized to explore the stability and properties of Mg(III). Its study provides
fundamental insights into ligand-field effects and the behavior of magnesium beyond its
common +2 oxidation state.
Experiment Synthesis

Chemicals
Potassium permanganate, potassium oxalate K2C2O4.H2O, oxalic acid, Ethanol and
distilled water
Synthesis of potassium trisoxalato magnate III complex

1g of KMnO4 was added in 20 ml distilled water and added into k2C2O4.H2O solution
(3.5g K2C2O4.H2O) dissolved in 20ml distilled water. The mixture was cooled in an ice
bath for 15 min and then oxalic acid in 20ml distilled water was added. The solution was
stirred for 1 hour in ice bath. The black color solution was filtered and ethanol was
added to get black complex K3[Mn(C2O4)3].

Result and Discussion

Potassium trisoxalato magnate III complex was successfully prepared by reaction of

potassium permanganate and potassium oxalate and oxalic acid

Properties Ligand Complex

Colour Colour less Green colour
Melting point ____ 230C
Magnetic Behavior ____ Paramagnetic
CFSE(Dq) ___ 10

Spectral characterization

UV Visible Spectrum of potassium trisoxalato III complex

The UV-visible spectrum of potassium tris(oxalato)ferrate(III) (K⁻[Fe(C⁻O⁻)⁻])

typically shows an intense charge transfer band in the UV region and a weaker, broad
d-d transition band in the visible region (~600-700 nm), giving the complex its
characteristic greenish-yellow color. The high-energy ligand-to-metal charge transfer
(LMCT) from oxalate to Fe(III) is responsible for the strong UV absorption. The weak
visible band corresponds to the spin-forbidden d-d transition of the high-spin d⁵ Fe(III)
ion.

Conclusion

This report has been successfully synthesized potassium trisoxalato ferrate (III)
complex. Synthesis of potassium trisoxalato chromate ( III )complex

Abstract
The potassium tris(oxalato)chromate(III) complex features chromium(III) coordinated to
three bidentate oxalate ligands. This octahedral complex is characterized by its vivid
color, photochemical activity, and optical isomerism. It serves as a classic example for
studying coordination chemistry and ligand field theory.

Introduction
The synthesis and study of potassium tris(oxalato)chromate(III) is a foundational
experiment in inorganic chemistry. It demonstrates key concepts including coordination
geometry, ligand field theory, and the stability of chelate complexes. This complex is
particularly noted for its photochemical properties and role in understanding optical
isomerism in octahedral metal complexes.
Experiment Synthesis

Chemicals

Potassium oxalate monohydrate, potassium dichromate, oxalic acid, distilled water were
used. All the chemicals used were purchased from Sigma-Aldrich and were used
without any further purification.

Synthesis of Potassium Tris oxalato chromate III trihydrate

A solution of potassium oxalate monohydrate (2.3g, 12.5mmol) and oxalic acid (5.5g,
43.6mmol) was prepared in 110-120 mL of distilled water. To this solution solid
potassium dichromate (1.9g, 6.45mmol) was added in small portions, with continuous
stirring. The solution was concentrated to near dryness. On cooling deep green shiny
crystals of potassium tris-oxalate chromate III trihydrate were formed. The solid was
filtered and dried by pressing between the filter paper.

Result and Discussion

The complex was successfully synthesized by the reaction of potassium oxalate and
oxalic acid. The physical data of complex and ligand is given as follows

Table 1 Physical data of ligand and complex

 Properties Ligand Complex
Melting point (C) 189-191 Varies
Molar mass 126 498
Color White Dark Green
Spectrum Characterization

UV Visible Spectrum analysis

Oxalic acid
Oxalic acid is essentially transparent in the standard UV-Vis range (200-800 nm)
because its main electronic transition is a strong π→π* absorption below 190 nm. Any
significant absorption above 200 nm indicates impurities, complex formation (e.g., with
metals), or sample degradation. In its pure, aqueous form, it is a colorless compound
with no characteristic peaks in the typical analytical UV spectrum.
UV Visible spectrum of tris oxalate chromate III complex
The tris(oxalato)chromate(III) complex exhibits a UV-visible spectrum with a major,

broad absorption band in the visible region (around 500-700 nm). This band
corresponds to a spin-allowed d - d transition) within the chromium(III) ion's d^3
configuration. The resulting green or violet color (depending on exact energy) is due to
the complement of the absorbed yellow/red light.

FTIR Spectral Analysis ( FTIR spectrum of oxalic acid)

The FTIR spectrum of oxalic acid dihydrate is dominated by a very broad O-H stretch
(3300-2500 cm⁻¹) from its strong hydrogen-bonded network. The carbonyl C=O stretch
is lowered (~1680-1660 cm⁻¹) due to conjugation and hydrogen bonding. Key lower-
frequency bands include C-O-H bending (~1250 cm⁻¹) and C-C/C-O stretches and O-H
bending (below 800 cm⁻¹).
FTIR spectrum of Tris acetylacetonato chromate III complex

The FTIR spectrum of K⁻[Cr(C⁻O⁻)⁻]·3H⁻O is dominated by strong, split bands at

~1700-1600 cm⁻¹ for asymmetric (νₐₛ(COO)) and ~1300-1200 cm⁻¹ for symmetric
(νₛ(COO)) carbonyl stretches. The large separation (~300 cm⁻¹) between these bands
confirms the bidentate coordination of the oxalate ligand to Cr(III). Additional peaks for
coordinated water (OH stretches/bends) and C-C/C-O stretches appear between 800-
500 cm⁻¹.

Conclusion
This report has successfully summarized the synthesis of Potassium Tris oxalato
chromate III trihydrate complex
11. Synthesis of potassium trisoxalato aluminate III hydrate

Abstract

The colorless, crystalline potassium tris(oxalato)aluminate(III) trihydrate was

synthesized by reacting aluminum metal with oxalic acid and potassium oxalate in
aqueous solution. Following dissolution via heating, the complex was crystallized by
cooling and isolated by filtration. The synthesis was assessed through yield calculation
and confirmed by characterization via FT-IR spectroscopy and melting point analysis.

Introduction
The potassium tris(oxalato)aluminate(III) complex, K⁻[Al(C⁻O⁻)⁻]·3H⁻O, is a classic
octahedral coordination compound where Al³⁻ is chelated by three bidentate oxalate
ligands. Its synthesis and characterization demonstrate fundamental principles of
coordination chemistry, such as the chelate effect and ligand-field stabilization. This
complex also serves as a model for studying metal-oxalate bonding and has relevance
in materials chemistry.
Experiment Synthesis

Chemical
Aluminum sulphate, sodium hydroxide, oxalic acid dihydrate, potassium oxalate. All the
chemicals used were purchased from Sigma-Aldrich and were used without any further
purification.

Synthesis of potassium trisoxalato aluminate (III) complex

3.5g of aluminum sulphate was weighed and dissolved in 25 mL of water and to this
solution , solution of sodium hydroxide (1.5g in 10mL of water) was added the ppts of
Al(OH)3 were filtered off. And washed with 20 mL of distilled water thrice. The ppts were
boiled with aqueous oxalic acid (2.5g) and potassium oxalate (3.87g) in 50 mL of water.
The solution was evaporated to saturation to effect crystalization. The product was
filtered off and washed with small quantity of distilled water. Percentage yield was
calculated.
Result and discussion

The complex was synthesized by the reaction of aluminum sulphate with oxalic acid

The physical data table is as follows

Table 1 Physical data of ligand and complex

Properties Ligand Complex

Melting point 189-191 Varies
Molar mass 126g/mol 462g/mol
Colour White White

Spectrum Characterization
UV Visible spectrum of oxalic acid

UV Visible spectral Analysis

Oxalic acid

Oxalic acid is essentially transparent in the standard UV-Vis range (200-800 nm)
because its main electronic transition is a strong π→π* absorption below 190 nm. Any
significant absorption above 200 nm indicates impurities, complex formation (e.g., with
metals), or sample degradation. In its pure, aqueous form, it is a colorless compound
with no characteristic peaks in the typical analytical UV spectrum.

UV Visible spectrum of potassium trisoxalato aluminate III complex

The UV-visible spectrum typically shows a strong charge transfer band in the ultraviolet
region. It may also display weaker d-d transition bands in the visible region, often
appearing pale in color. The exact peak positions depend on the ligand field strength
and molecular geometry
FTIR spectrum of oxalic acid

The FTIR spectrum of oxalic acid dihydrate is dominated by a very broad O-H stretch
(3300-2500 cm⁻¹) from its strong hydrogen-bonded network. The carbonyl C=O stretch
is lowered (~1680-1660 cm⁻¹) due to conjugation and hydrogen bonding. Key lower-
frequency bands include C-O-H bending (~1250 cm⁻¹) and C-C/C-O stretches and O-H
bending (below 800 cm⁻¹).

FTIR spectrum of potassium trisoxalato aluminate III complex

The FTIR spectrum shows strong bands around 1700-1600 cm⁻¹ for asymmetric C=O
stretches, and near 1300-1200 cm⁻¹ for symmetric C=O stretches of the oxalate ligands.
Bands around 800-500 cm⁻¹ are typically assigned to Al–O stretching vibrations,
confirming coordination. The absence of a free oxalate signature confirms the oxalate
acts as a chelating ligand.

Conclusion

This report has successfully summarized the synthesis and characterization of

potassium Tris oxalato aluminate III complex

13 Synthesis and characterization of Nickel II Anthranilate Complex

Abstract

This study synthesized and characterized a novel nickel(II) anthranilate complex.

Characterization via spectroscopy (FT-IR, UV-Vis) and elemental analysis confirmed its
composition and coordination geometry. Magnetic moment and thermal analysis
provided insights into its electronic structure and stability. The complex exhibited notable
antibacterial activity against tested strains. Results suggest potential for applications in
coordination chemistry and bioinorganic materials.

Introduction
Nickel(II) complexes with anthranilate ligands are studied for their versatile coordination
modes and functional properties. This work details the synthesis and characterization of
a novel nickel(II) anthranilate complex. Its structural features, thermal stability, and
potential antibacterial activity are investigated.

Experimental Synthesis

Chemical
2-amino benzoic acid, ethanol, sodium hydroxide, Nickel acetate and distilled water. All
the chemicals used were purchased from Sigma-Aldrich and were used without any
further purification.

Synthesis of Nickel II anthranilate complex

1g of 2-aminobenzoic acid was dissolved in 6.67 mL of ethanol. 0.1g of sodium
hydroxide was dissolved in 10 mL of ethanol. Both solutions were mixed and stirred for
half an hour. Then, 0.9g of Nickel acetate was dissolved in 10 mL of water and added
into the above solution. The whole mixture was stirred for an hour . After that, the
solution mixture was cooled and ppts were filtered out.

Result and Discussion

The complex was prepared by the reaction of 2-aminobenzoic acid and nickel acetate
and the physical data table is as follows:

Table 1 physical data of ligand and complex

 Properties Ligand Complex
Colour Light brown Light green
Melting point 144 - 148 280
Molar mass (g/mol) 137.14 367
Spectral Analysis

UV visible spectrum of 2 aminobenzoic acid

The UV-visible spectrum of 2-aminobenzoic acid (anthranilic acid) typically shows two
main absorption bands. A primary band appears around 230-280 nm due to the π→π*
transitions of the aromatic ring. A secondary, broader band in the 300-350 nm region
arises from n→π* transitions involving the amino and carboxyl substituents.

UV Visible spectrum of Nickel (II) Anthranilate

The UV-visible spectrum of a nickel(II) anthranilate complex typically shows d-d
transition bands in the 350–600 nm region (visible range) due to octahedral or pseudo-
octahedral geometry. A strong, higher-energy charge transfer band from the anthranilate
ligand to the nickel center often appears in the UV region (<350 nm). The exact peak
positions depend on the specific coordination environment and ligand field strength.
Conclusion
This report has successfully summarized the synthesis and characterization of Nickel II
Anthranilate Complex .