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Chemical Ionization (CI) Mass Spectrometry

Chemical Ionization (CI) Mass Spectrometry

The molecular ion peak of a molecule in the mass spectrum provides vital information for molecular identification. However, conventional electron impact ionization can lead to the rapid dissociation of some molecular ions before they reach the detector. A milder ionization method is required to increase the lifetime of such ionized analyte molecules. Chemical ionization (CI) is a gas-phase protonation reaction useful for mass-analyzing analyte molecules that are easily protonated to yield the...

Diazonium Group Substitution: –OH and –H

Diazonium Group Substitution: –OH and –H

Nitrous acid, a weak acid, is prepared in situ via the reaction of sodium nitrite with a strong acid under cold conditions. This nitrous acid prepared in situ reacts with primary arylamines to form arenediazonium salts. Such reactions are known as diazotization reactions. As shown in Figure 1, the formation of arenediazonium salts begins with the decomposition of nitrous acid in an acidic solution to give nitrosonium ions.

1° Amines to Diazonium or Aryldiazonium Salts: Diazotization with NaNO2 Mechanism

1° Amines to Diazonium or Aryldiazonium Salts: Diazotization with NaNO₂ Mechanism

Nitrous acid is a relatively weak and unstable acid prepared in situ by the reaction of sodium nitrite and cold, dilute hydrochloric acid. In an acidic solution, the nitrous acid undergoes protonation when it loses water to form a nitrosonium ion—an electrophile. Nitrous acid reacts with primary amines to give diazonium salts. The reaction is called diazotization of primary amines.

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1,1-Dimethyl-hydrazin-1-ium picrate.

Xiao-Gang Mu¹, Xuan-Jun Wang, Xiang-Xuan Liu

¹No. 503 Faculty, Xi'an Research Institute of High Technology, Hongqing Town, Xi'an 710025, People's Republic of China.

Acta Crystallographica. Section E, Structure Reports Online

|November 8, 2011

Summary

This study details the crystal structure of a compound, revealing specific molecular arrangements and hydrogen bonding. The findings illustrate how molecules connect in a two-dimensional network within the crystal lattice.

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Area of Science:

Crystallography
Chemical Physics
Materials Science

Background:

Understanding molecular interactions and crystal packing is crucial for predicting material properties.
The specific compound investigated, [Chemical Name/Formula], presents an interesting case for structural analysis.

Purpose of the Study:

To elucidate the crystal structure of the title compound.
To analyze the dihedral angles between nitro groups and the benzene ring.
To investigate the intermolecular interactions, specifically hydrogen bonding, within the crystal.

Main Methods:

Single-crystal X-ray diffraction was employed to determine the molecular and crystal structure.
Analysis of bond lengths, bond angles, and dihedral angles provided insights into molecular geometry.
Hydrogen bonding networks were identified and characterized using crystallographic data.

Main Results:

The crystal structure of C(2)H(9)N(2) (+)·C(6)H(2)N(3)O(7) (-) was determined.
Significant dihedral angles (63.5°, 10.5°, 10.4°) were observed between the nitro groups and the benzene ring.
A two-dimensional hydrogen-bonded network parallel to the (001) plane was identified, involving N-H⋯O interactions.

Conclusions:

The study provides a detailed structural description of the title compound.
The observed dihedral angles suggest specific electronic and steric influences within the molecule.
The formation of a 2D hydrogen-bonded network highlights the importance of intermolecular forces in directing crystal assembly.