SIC3021 Inorganic Chemistry III Laboratory Manual

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Questions and Answers

What does a positive magnetic susceptibility indicate about a material?

  • It is always diamagnetic.
  • It can be paramagnetic or ferromagnetic. (correct)
  • It is not affected by magnetic fields.
  • It has all paired electrons.

Which method is used for measuring magnetic susceptibility in solids?

  • Evans’ method
  • SQUID technique
  • Gouy method (correct)
  • NMR spectroscopy

What is true about transition metals regarding their magnetic properties?

  • They have completely filled d subshells.
  • They have at least one incomplete d subshell. (correct)
  • They are always diamagnetic.
  • They cannot exhibit paramagnetism.

How are magnetic properties used in the study of compounds?

<p>To characterize systems like alloys and coordination complexes. (B)</p> Signup and view all the answers

What does the number of unpaired electrons in a transition metal indicate?

<p>The oxidation state and electron configuration. (B)</p> Signup and view all the answers

What role do superconducting loops play in SQUID magnetometers?

<p>They are used to measure extremely subtle magnetic fields. (D)</p> Signup and view all the answers

What is the purpose of adding acetylacetone during the preparation procedure?

<p>To provide a stabilizing ligand. (C)</p> Signup and view all the answers

At what temperature is the mixture heated during the preparation of the manganese complex?

<p>60°C (C)</p> Signup and view all the answers

What is one of the main pharmacological utilities of phosphine-based compounds?

<p>Antiviral agents (A)</p> Signup and view all the answers

What role do tertiary phosphine complexes play in catalysis?

<p>They serve as homogeneous catalysts. (C)</p> Signup and view all the answers

Why is nickel catalysis considered appealing?

<p>It is cost-effective. (A)</p> Signup and view all the answers

During the synthesis of dichlorobis(triphenylphosphino)nickel(II), what is the first step involving triphenylphosphine?

<p>Melting it in a water bath (C)</p> Signup and view all the answers

In the preparation process of the Schiff base, what is the role of salicyldehyde?

<p>It serves as a ligand. (C)</p> Signup and view all the answers

What is a significant safety precaution mentioned in the synthesis of nickel(II) complex?

<p>Handle glacial acetic acid with care. (D)</p> Signup and view all the answers

What analytical techniques are suggested for characterizing the prepared Schiff base?

<p>IR and 1H NMR (D)</p> Signup and view all the answers

What byproduct must be removed after synthesizing dichlorobis(triphenylphosphino)nickel(II)?

<p>Triphenylphosphine (D)</p> Signup and view all the answers

What should be done before re-precipitating the complex after dissolving the chelate?

<p>Filter the solution (A)</p> Signup and view all the answers

Which solvent should be subtracted from the frequency shift to correct for diamagnetism?

<p>Warm toluene (B)</p> Signup and view all the answers

What is the diamagnetic correction value for Carbon (aromatic)?

<p>6.24 (C)</p> Signup and view all the answers

At equilibrium, what relationship holds between the effective magnetic moment (µeff) and molar magnetic susceptibility (χM)?

<p>µeff = constant x χM (D)</p> Signup and view all the answers

Which of the following complexes can be determined using tert-butanol methyl resonance as a reference?

<p>Fe(CN)6^3- in aqueous solution (C)</p> Signup and view all the answers

What is the first step to calculate magnetic susceptibility in solution?

<p>Prepare a pure solvent capillary reference (B)</p> Signup and view all the answers

Which element has the highest diamagnetic correction value according to the provided data?

<p>Ni2+ (B)</p> Signup and view all the answers

In the Tanabe-Sugano diagrams, what are these diagrams used to depict?

<p>Energies of electronic states as a function of ligand field strength (A)</p> Signup and view all the answers

What is essential to understand before applying the spin-only formula to calculate the effective magnetic moment?

<p>The complex must contain unpaired electrons (C)</p> Signup and view all the answers

Which option represents a common mistake when referencing magnetic susceptibility in organic solvents?

<p>Using a solvent with unpaired electrons as reference (D)</p> Signup and view all the answers

What is the effective magnetic moment (µeff) for a tetrahedral [Ni(salen)2] complex in solution as mentioned?

<p>3.3 (B)</p> Signup and view all the answers

What is necessary for calculating ê­•M and ê­•Mcorr in relation to the complex magnetic properties?

<p>The diamagnetic correction for ligands must be included (B)</p> Signup and view all the answers

What is the diamagnetic correction value for Oxygen in the context of alcohol?

<p>-4.61 (A)</p> Signup and view all the answers

What role does the capillary tube with pure CHCl3 serve in NMR analysis?

<p>It provides a reference for chemical shifts (D)</p> Signup and view all the answers

Calculate the effective magnetic moment (µeff) from the given observations if the molar susceptibility (χM) is assumed to have a certain constant. Which formula is correct?

<p>µeff = K x χM (D)</p> Signup and view all the answers

What is the diamagnetic correction value for Carbon in general, not specifically for the aromatic form?

<p>-6.00 (A)</p> Signup and view all the answers

What is the relationship between mass susceptibility and density?

<p>Mass susceptibility introduces a density factor inversely. (A)</p> Signup and view all the answers

What is typically the best measurement to compare different materials' magnetism?

<p>Molar susceptibility (B)</p> Signup and view all the answers

What is magnetic susceptibility defined as?

<p>The ratio of the intensity of magnetism induced in a substance to the magnetizing force. (A)</p> Signup and view all the answers

Which formula correctly represents the calculation for corrected molar susceptibility?

<p>χ Μcorr = χ exp - χdia (C)</p> Signup and view all the answers

Which methods are traditionally used to measure magnetic susceptibility?

<p>Gouy and Faraday methods. (A)</p> Signup and view all the answers

How is effective magnetic moment, µeff, calculated?

<p>µeff = √n(n + 2) B.M. (D)</p> Signup and view all the answers

What happens to the effective magnetic moment in a system adhering to Curie law?

<p>There is no or negligible orbital contribution. (D)</p> Signup and view all the answers

What advantage did Professor Evans's innovative method provide?

<p>The shift from measuring weight changes to detecting force on a magnet. (C)</p> Signup and view all the answers

Which model of magnetic susceptibility balance is mentioned as being used in the laboratory?

<p>MSB-AUTO (D)</p> Signup and view all the answers

What is the main purpose of knowing the molecular weight, MW, in the context of susceptibility?

<p>To convert χg to χM. (C)</p> Signup and view all the answers

Which method is primarily used to obtain a χg value from χν?

<p>Inputting sample length and weight into the Auto. (A)</p> Signup and view all the answers

How is volume susceptibility typically expressed?

<p>As the ratio of the intensity of magnetism to the volume of the sample. (C)</p> Signup and view all the answers

What is suggested for cleaning difficult residue in sample tubes?

<p>Conventional detergents and strong acids. (D)</p> Signup and view all the answers

Which of the following statements about the measurement of magnetic susceptibility is incorrect?

<p>The variety of methods evolved include only digital systems. (B)</p> Signup and view all the answers

What are the three common ways magnetic susceptibility values are expressed?

<p>Volume, mass, and molar. (B)</p> Signup and view all the answers

What can lead to variability in volume susceptibility measurements?

<p>Changes in the density of the substance. (A)</p> Signup and view all the answers

Flashcards

Nickel(II) complex stabilization

Using bulky ligands like triphenylphosphine to prevent the formation of reactive nickel(II) species, enabling interaction with biological targets.

Triphenylphosphine

A bulky ligand used in stabilizing metal complexes and catalysis.

Dichlorobis(triphenylphosphine)nickel(II) synthesis

A chemical reaction to produce NiCl2(PPh3)2.

Schiff base synthesis

Preparation of benzoic acid-(2-hydroxy-benzylidene)-hydrazide ligand.

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Mixed ligand metal complexes

Metal complexes containing different ligands attached to the central metal.

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Glacial acetic acid

Highly pure form of acetic acid used in the synthesis reactions.

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Homogeneous catalysis

Catalysis that involves the catalyst in the same phase as the reactants

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Nickel catalysis

Catalytic processes using nickel as a catalyst.

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Magnetic Susceptibility

A measure of how much a material gets magnetized when exposed to a magnetic field.

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Paramagnetism

A type of magnetism where materials are weakly attracted to a magnetic field due to unpaired electrons.

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Diamagnetism

A type of magnetism where materials are weakly repelled by a magnetic field because all electrons are paired.

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Gouy Method

A technique to measure the magnetic susceptibility of solid samples.

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Evans' Method

A technique for determining the magnetic susceptibility of solutions.

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SQUID

A highly sensitive magnetometer used for measuring magnetic fields.

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Ligand Strength

The ability of a ligand to attract electrons from the central metal atom.

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Coordination Complex

A central metal atom surrounded by ligands that are bonded to it.

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Paramagnetic Susceptibility

A measure of how much a substance is attracted to a magnetic field. Paramagnetic substances are weakly attracted because they contain unpaired electrons.

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NMR Spectroscopy

A technique that uses radio waves and magnetic fields to determine the structure and properties of molecules. It is particularly useful for studying hydrogen atoms (protons) in molecules.

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Diamagnetic Correction

Subtracting the magnetic susceptibility contribution of the solvent from the overall magnetic susceptibility measurement to isolate the contribution specifically from the complex.

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Magnetic Susceptibility in Solution

The susceptibility of a metal complex dissolved in a specific solvent, measured using NMR.

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Spin-Only Formula

A simple equation used to predict the magnetic moment of a complex based on the number of unpaired electrons. It provides a good approximation but doesn't take into account orbital contributions.

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Conditions for Spin-Only Formula Applicability

The spin-only formula is most accurate for complexes where the metal ion has a single oxidation state and the ligands are weak field.

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Requirements for Solution Susceptibility Measurement

The complex should be stable in solution, and the solvent and reference should satisfy specific criteria. For example, the reference should not interact significantly with the complex.

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Feasibility of Measurement

Assess whether a complex can be successfully analyzed based on the specific solvent and reference used in the NMR experiment

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Mass Susceptibility (χg)

A measure of how much a material gets magnetized per unit mass when exposed to a magnetic field. It incorporates the density of the substance.

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Molar Susceptibility (χM)

A measure of how much a material gets magnetized per mole when exposed to a magnetic field. It accounts for the molecular weight and is independent of sample density.

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How is χM related to χg?

Molar susceptibility (χM) is calculated by multiplying the mass susceptibility (χg) by the molecular weight (MW) of the substance: χM = χg x MW.

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Diamagnetic Contribution (χdia)

A correction applied to the measured molar susceptibility (χexp) to account for the inherent diamagnetic properties of the ligands and metal ions in a complex, resulting in a corrected molar susceptibility (χMcorr).

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Effective Magnetic Moment (µeff)

A measure of the overall magnetic moment of a substance, reflecting the contribution from both spin and orbital angular momentum of the electrons.

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How is µeff related to χM?

The effective magnetic moment (µeff) is calculated using the corrected molar susceptibility (χMcorr) and a formula involving the number of unpaired electrons (n).

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Curie Law

A law stating that the magnetic susceptibility of a paramagnetic substance is inversely proportional to the absolute temperature. A system obeying Curie law has negligible orbital contribution to the magnetic moment.

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Cleaning Sample Tubes

The sample tubes used in magnetobalances are delicate and require careful cleaning. Conventional detergents, organic solvents, or strong acids (like HCl or HNO3) may be needed, depending on the sample.

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Volume Susceptibility

The magnetic susceptibility of a material expressed per unit volume.

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What are the three types of magnetic susceptibility?

The three common ways to express magnetic susceptibility are volume susceptibility (χv), mass susceptibility (χm), and molar susceptibility (χM).

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Faraday Method

A technique for measuring the magnetic susceptibility of solid samples, involving measuring the force acting on a sample suspended in a magnetic field gradient.

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What is the significance of magnetic susceptibility?

Magnetic susceptibility provides information about the electronic structure of compounds, particularly transition metal and rare earth metal complexes.

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MSB-AUTO

A modern magnetic susceptibility balance that utilizes Evans' method and offers improved features for precise and efficient measurements.

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What are the main types of magnetic behaviour?

There are two main types of magnetic behavior in materials: Paramagnetism and Diamagnetism.

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Tanabe-Sugano (TS) Diagrams

Correlation diagrams that visualize the relationship between electronic state energies in a complex and the strength of the ligand field.

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Study Notes

Laboratory Manual

  • SIC3021 Practical of Inorganic Chemistry III
  • This is a laboratory manual for a course at Universiti Malaya
  • The manual covers different experiments
  • Includes synthesis of Nickel complexes with mixed ligand systems

Contents

  • Experiment 1: Synthesis of Nickel complex with mixed ligand system
  • Experiment 2: Preparation and characterization of mesitylenetricarbonylmolybdenum(0)
  • Experiment 3: Magnetic susceptibility
  • Experiment 4: Electronic spectra of Nickel(II) complexes
  • Each experiment has a specific page number

Emergency Telephone Numbers

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  • These numbers are current as of October 5th, 2022

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