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Precipitation Gravimetry01:03

Precipitation Gravimetry

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Precipitation gravimetry is based on converting an analyte into a sparingly soluble precipitate, which is separated by filtration and weighed. An ideal precipitate should be pure, insoluble, of known composition, and easily filtered from the reaction mixture.
In determining nickel by gravimetric analysis, a precipitant of ethanolic dimethylglyoxime is added to a hot nickel salt solution. This is quickly followed by the dropwise addition of dilute ammonia solution until precipitation occurs. A...
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Formation of Complex Ions03:45

Formation of Complex Ions

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A type of Lewis acid-base chemistry involves the formation of a complex ion (or a coordination complex) comprising a central atom, typically a transition metal cation, surrounded by ions or molecules called ligands. These ligands can be neutral molecules like H2O or NH3, or ions such as CN− or OH−. Often, the ligands act as Lewis bases, donating a pair of electrons to the central atom. These types of Lewis acid-base reactions are examples of a broad subdiscipline called coordination...
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Valence Bond Theory02:42

Valence Bond Theory

8.6K
Coordination compounds and complexes exhibit different colors, geometries, and magnetic behavior, depending on the metal atom/ion and ligands from which they are composed. In an attempt to explain the bonding and structure of coordination complexes, Linus Pauling proposed the valence bond theory, or VBT, using the concepts of hybridization and the overlapping of the atomic orbitals. According to VBT, the central metal atom or ion (Lewis acid) hybridizes to provide empty orbitals of suitable...
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Electrodeposition01:08

Electrodeposition

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Electrodeposition is a technique used to separate an analyte from interferents by electrochemical processes. Here, the analyte is a metal ion that can be deposited on an electrode immersed in the sample solution. The electrochemical setup consists of an anode and a cathode. When an electric current is applied to the setup, oxidation occurs at the anode. At the cathode, which consists of a large metal surface, metal ions undergo reduction and deposit onto the surface.
Electrodeposition can...
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Coordination Number and Geometry02:57

Coordination Number and Geometry

15.9K
For transition metal complexes, the coordination number determines the geometry around the central metal ion. Table 1 compares coordination numbers to molecular geometry. The most common structures of the complexes in coordination compounds are octahedral, tetrahedral, and square planar.
15.9K
Nitriles to Amines: LiAlH4 Reduction00:55

Nitriles to Amines: LiAlH4 Reduction

3.5K
Nitriles are reduced to amines in the presence of strong reducing agents like lithium aluminum hydride through a typical nucleophilic acyl substitution. The reaction requires two equivalents of the reducing agent. The reducing agent acts as a source of hydride ions.
As shown below, the mechanism involves three steps. Firstly, the hydride ion acting as a nucleophile attacks the nitrile carbon to form an anion. In the second step, a second equivalent of the hydride ion attacks the anion to...
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Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction
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Electroreductive Synthesis of Nickel(0) Complexes.

Camille Z Rubel1,2, Yilin Cao1, Tamara El-Hayek Ewing1

  • 1Department of Chemistry, The Scripps Research Institute, 10550 N. Torrey Pines Road, La Jolla, CA 92037, USA.

Angewandte Chemie (International Ed. in English)
|November 20, 2023
PubMed
Summary
This summary is machine-generated.

Electrolysis offers a reproducible and scalable method to synthesize nickel(0) precatalysts from nickel(II) salts, replacing hazardous reagents and enabling broader use in organic synthesis.

Keywords:
ElectrochemistryFlow ChemistryGreen ChemistryNickel CatalysisPrecatalyst

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Author Spotlight: A Rapid, Microwave-Assisted Hydrothermal Synthesis Of Nickel Hydroxide Nanosheets
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Area of Science:

  • Organometallic Chemistry
  • Catalysis
  • Electrochemistry

Background:

  • Nickel catalysts are crucial for organic transformations, with Ni(0) sources being effective precatalysts.
  • Traditional synthesis of Ni(0) precatalysts relies on pyrophoric aluminum-hydride reductants, posing safety and atom-economy challenges.
  • Existing methods often lack reproducibility and require cryogenic temperatures.

Purpose of the Study:

  • To develop a scalable, reproducible, and safer method for synthesizing low-valent nickel precatalysts.
  • To establish an electrochemical route for generating Ni(0) complexes from readily available Ni(II) salts.
  • To facilitate the broader application of nickel catalysis in organic synthesis.

Main Methods:

  • Preparative scale reduction of Ni(II) salts using electrolysis.
  • Standardization of the electrochemical procedure for robustness and reproducibility.
  • Development of an electrochemical recirculating flow process for large-scale synthesis.
  • Implementation of an in situ reduction protocol for generating catalytic Ni(0).

Main Results:

  • Successful synthesis of various Ni(0) and Ni(II) complexes, including bis(1,5-cyclooctadiene)nickel(0) [Ni(COD)2].
  • Demonstration of a robust and reproducible electrochemical method for Ni(0) precatalyst preparation.
  • Scalability of the method via an electrochemical recirculating flow process.
  • Viability of in situ generation of Ni(0) for catalytic applications.

Conclusions:

  • Electrochemical reduction provides a superior alternative to traditional methods for synthesizing Ni(0) precatalysts.
  • This approach enhances safety, reproducibility, and scalability in organometallic complex preparation.
  • The developed method is expected to accelerate the adoption of electrochemistry for synthesizing low-valent nickel complexes in research and industry.