Small Molecules X-Ray

Diffraction
By Rajan Hardaha Vinod Saini

X- Ray Diffraction
An X Ray Diffraction refers to technique in which a beam of X-Rays strike a single crystal producing scattered beams. The atoms in a crystal are arranged in a periodic array and since the wavelength of X rays are similar to the distance between atoms, they can diffract light. The scattering of X-rays from atoms produces a diffraction pattern, which contains information about the atomic arrangement within the crystal
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The wave-length of x-rays is of the same order as inter-atomic or inter-molecular distances. (10-8 cm or 0.00000001 cm)

Unit Cell
The unit cell is the basic repeating unit that defines the crystal structure The unit cell contains the maximum symmetry that uniquely defines the crystal structure. The unit cell might contain more than one molecule: for example, the quartz unit cell contains 3 complete molecules of SiO2.

The shape of unit cell depends on crystal system and is described by lattice parameters.

Crystals use (7) different shapes of regular box to build up into a crystal. Actually there are only (5) unique shapes, the other two are special cases of one of the five. Hexagonal
Tetragonal
A stretched cube
c g

Cubic

In hexagonal a=b c a = b = 90o g =120o In cubic a=b =c a = b = g = 90o Rhombohedral a=b =c a = b = g 90o

In tetragonal a=b c a = b = g = 90o (a column or pillar)

Space Group- a space group is the symmetry group of a configuration in space, usually in three dimensions . There are 219 space groups in 3 D.

Point groups-a point group is a group of geometric symmetries (isometries) that keep at least one point fixed. There are 32 point groups in 3D.

Single Crystal XRD and Powder XRD

Single Crystal XRD is done for long range ordering crystals, where we can get about individual planes and diffraction pattern is in the form of spots The material size should be more than 30*10*10 cm.

Powder XRD is done for polycrystalline materials,where short range ordering is there. We can't get information about individual planes and the diffraction pattern is in the Form of ring types. Powder XRD is useful for phase identification.

X Ray Diffraction of MgB2

We did X Ray Diffraction of MgB2 and got the following graph of 2 Theta Versus Intensity. After Matching Peaks with ICDD, we confirmed that the compound was MgB2

Compounds molecular weight- 836.56 Schematic Diagram CCDC Number- 643169

Mercury Hydrogen Bonding Diagram

Packing Diagram

Observation
Intermolecular Interaction- Two Hydrogen Bonding were observed between Hydrogen and Oxygen as evident from Mercury Diagram. 1.949 Angstrom and 2.156 Angstrom. Properties- These compounds can improve efficacy of medicinal chelators .

N-isonicotinoyl benzaldehydehydrazone
Compounds molecular weight- 225.25 Compounds schematic Diagram-

Mercury Hydrogen Bonding Diagram

Packing Diagram

Here also two types of Hydrogen Bonding were observed between Nitrogen and Hydrogen as seen from Mercury Diagram, 2.224 Angstorm and 2.218 Angstorm

Compounds molecular weight- 3100.27 Schematic Diagram-

CCDC Number-912202

Mercury Hydrogen Bonding Diagram

Packing Diagram

Observations
Many Hydrogen Bonding were observed , some weak, some strong. Bonds between Nitrogen and Hydrogen were shown to be of moderate interaction as bond length between them was 2.28 and
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Properties
It displays field induced magnetization relaxation, typical of single molecule magnet behavior.

Compound Name : 2-(2-Hydroxybenzylidene)-1-(2-picoloyl)hydrazine Hemihydrate

Compounds molecular weight- 250.26 Compounds schematic Diagram-

Mercury Hydrogen Bonding Diagram

Packing Diagram

Observations

Strong Hydrogen bonding interaction is observed as bonding between hydrogen and Oxygen was measured to be about 1.844 Angstrom.
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