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Structures of Solids02:22

Structures of Solids

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Solids in which the atoms, ions, or molecules are arranged in a definite repeating pattern are known as crystalline solids. Metals and ionic compounds typically form ordered, crystalline solids. A crystalline solid has a precise melting temperature because each atom or molecule of the same type is held in place with the same forces or energy. Amorphous solids or non-crystalline solids (or, sometimes, glasses) which lack an ordered internal structure and are randomly arranged. Substances that...
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Molecular and Ionic Solids02:54

Molecular and Ionic Solids

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Crystalline solids are divided into four types: molecular, ionic, metallic, and covalent network based on the type of constituent units and their interparticle interactions.
Molecular Solids
Molecular crystalline solids, such as ice, sucrose (table sugar), and iodine, are solids that are composed of neutral molecules as their constituent units. These molecules are held together by weak intermolecular forces such as London dispersion forces, dipole-dipole interactions, or hydrogen bonds, which...
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Molecular Comparison of Gases, Liquids, and Solids02:26

Molecular Comparison of Gases, Liquids, and Solids

55.1K
Particles in a solid are tightly packed together (fixed shape) and often arranged in a regular pattern; in a liquid, they are close together with no regular arrangement (no fixed shape); in a gas, they are far apart with no regular arrangement (no fixed shape). Particles in a solid vibrate about fixed positions (cannot flow) and do not generally move in relation to one another; in a liquid, they move past each other (can flow) but remain in essentially constant contact; in a gas, they move...
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Metallic Solids02:37

Metallic Solids

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Metallic solids such as crystals of copper, aluminum, and iron are formed by metal atoms. The structure of metallic crystals is often described as a uniform distribution of atomic nuclei within a “sea” of delocalized electrons. The atoms within such a metallic solid are held together by a unique force known as metallic bonding that gives rise to many useful and varied bulk properties.
All metallic solids exhibit high thermal and electrical conductivity, metallic luster, and malleability....
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Molecular Structure and Acidity02:34

Molecular Structure and Acidity

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An acid can be deprotonated to form a conjugate base or an anion. If the produced anion is more stable, then the acid is stronger. On the contrary, if the anion is unstable, then the acid is weaker. Hence, to determine the acidity of the compound, the stability of its conjugate base is studied using various factors.
The size effect explains the change in atomic size on acidity. When comparing the acids formed from elements that belong to the same column in the periodic table, their atomic sizes...
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Acid Strength and Molecular Structure03:05

Acid Strength and Molecular Structure

33.1K
Binary Acids and Bases
In the absence of any leveling effect, the acid strength of binary compounds of hydrogen with nonmetals (A) increases as the H-A bond strength decreases down a group in the periodic table. For group 17, the order of increasing acidity is HF < HCl < HBr < HI. Likewise, for group 16, the order of increasing acid strength is H2O < H2S < H2Se < H2Te. Across a row in the periodic table, the acid strength of binary hydrogen compounds increases with increasing...
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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy

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Structure determination of supra-molecular assemblies by solid-state NMR: Practical considerations.

Jean-Philippe Demers1, Pascal Fricke2, Chaowei Shi2

  • 1Department of Molecular Biophysics, Leibniz-Forschungsinstitut für Molekulare Pharmakologie (FMP), 13125 Berlin, Germany; Laboratory of Cell Biology, Center for Cancer Research (CCR), National Cancer Institute (NCI), National Institutes of Health (NIH), Bethesda, MD 20892, USA.

Progress in Nuclear Magnetic Resonance Spectroscopy
|December 12, 2018
PubMed
Summary

Solid-state NMR (ssNMR) spectroscopy enables atomic structure determination of large biomolecular assemblies. This guide details initial steps for studying these molecular machines using ssNMR, from sample preparation to spectral analysis.

Keywords:
Isotope labelingProtein expressionProtein structureSolid-state Nuclear Magnetic ResonanceSupra-molecular assembly

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Area of Science:

  • Biophysics
  • Structural Biology
  • Biochemistry

Background:

  • Biomolecules form large complexes acting as molecular machines within cells.
  • Determining the structure of intact assemblies reveals context-specific conformations and interactions.
  • Solid-state NMR (ssNMR) spectroscopy is ideal for high-molecular-weight samples, enabling atomic structure determination under near-physiological conditions.

Purpose of the Study:

  • To provide a practical guide for initiating the study of biological supramolecular assemblies using ssNMR.
  • To outline methods for sample preparation, including isotope labeling and in situ studies.
  • To detail experimental setup and spectral analysis for ssNMR of large assemblies.

Main Methods:

  • Utilizing various methods for isotope-labeled sample production: recombinant expression, cell-free synthesis, direct cellular extraction, or in situ whole-cell studies.
  • Implementing specialized isotope labeling schemes (mixed, diluted, segmental) to aid chemical shift assignment and study inter-molecular interfaces.
  • Setting up magic-angle spinning (MAS) ssNMR experiments, including rotor selection, sample preparation, instrument calibration, and diagnostic spectral evaluation.

Main Results:

  • Demonstration of practical approaches for sample preparation and labeling tailored for ssNMR studies of large assemblies.
  • Presentation of detailed procedures for magic-angle spinning (MAS) ssNMR experimental setup and calibration.
  • Review of diagnostic spectra for assessing sample quality and methods to improve spectral resolution and sensitivity.

Conclusions:

  • ssNMR is a powerful technique for elucidating the structure and interactions of large biomolecular assemblies.
  • Careful sample preparation, specialized labeling, and optimized experimental setup are crucial for successful ssNMR studies.
  • This review offers a foundational guide for researchers beginning ssNMR investigations of supramolecular structures.