X-ray diffraction workshop 2023-2024

Q 1 Which ONE of the following statements is TRUE?

a) X-rays are scattered mainly from atomic nuclei, allowing us to see atom positions as a result
b) The intensity of a scattered X-ray beam is related to the types of atoms present in the unit cell
c) X-rays are reflected from real physical planes that lie within the unit cell
d) There are only three imaginary planes in a unit cell
e) X-rays have a typical wavelength of around 1 nm

Q 2 A unit cell has dimensions a=3.4 Å, b=7.2 Å, c=9.1 Å, =90, =90, =90 degrees. Which term BEST
describes it?

a) Monoclinic
b) Amorphous
c) Orthorhombic
d) Brick
e) None of the above

Q 3 A patent states that a particular crystal structure of ranitidine is characterised a diffraction peak at
14.2 2 when using =0.707Å. You collect PXRD data from a powder sample of this crystal using
=1.5406Å. Where would you expect to see that diffraction peak in your PXRD data?

a) still at 14.2 2
b) at some value significantly larger than 14.2 2
c) at some value significantly less than 14.2 2
d) at some value very close to 14.2 2
e) the peak will not be visible in the pattern

Q 4 A unit cell contains eight molecules of which only one is unique. Which of the following statements is
TRUE?

a) Z'=1 and Z=1

b) Z'=1 and Z=8
c) Z'=8 and Z=1
d) Z'=8 and Z=8
e) You cannot tell without knowing the symmetry inside the cell

Q 5 Which one of the following statements is FALSE?

a) X-ray crystallography can return information about atomic positions

b) X-ray crystallography can return information about atomic vibrations
c) X-ray crystallography can allow us to work out atom connectivity
d) X-ray crystallography can reveal molecular conformation in solution
e) X-ray crystallography can tell us about hydrogen bonding patterns between molecules
Q 6 An amorphous material gives no clear Bragg diffraction peaks because:

a) It is highly crystalline with long-range order

b) Molecules in the material have no long-range order
c) It contains no molecules
d) The molecules have all been destroyed by milling
e) It is almost a single crystal and so diffracts strongly

Q 7 The X-ray powder diffraction patterns of TWO distinct crystalline polymorphs of pure famotidine,
collected on the same diffractometer under identical conditions, differ because:

a) The polymorphs are different chemical entities

b) The polymorphs are both crystalline
c) The polymorphs have different unit cells and atomic positions
d) Powder diffraction is not a sensitive enough technique
e) Impurities in the sample contribute to the observed diffraction patterns

Q 8 When a crystal scatters X-rays, the patterns we see are actually the result of:

a) Reflection from real planes in the crystal

b) Reflection from imaginary planes in the crystal
c) Diffraction from real planes in the crystal
d) Diffraction from imaginary planes in the crystal
e) Diffraction from atoms in the crystal

Q 9 A particular X-ray reflection is found to be very strong. What does this observation suggest to you?

a) The crystal is strongly scattering

b) There are a significant number of atoms lying in the plane associated with the crystal reflection in
question
c) There are lots of strong reflections
d) The crystal structure is amorphous
e) The incident X-ray beam is very strong

Q 10 Single crystal diffraction is preferred to powder diffraction when a crystal can be grown because

a) Crystals can be used for NMR as well

b) Single crystals are always easy to grow
c) Powder diffraction is too expensive to carry out
d) It is the definitive method for crystal structure determination
e) Powder diffraction instruments are too complicated
Q 11 A chemist synthesises a molecule that has a chiral centre and claims that he has made the pure R
enantiomer. You grow a single crystal and work out that the space group for the crystal possesses a centre
of symmetry. What do you tell the chemist?

a) Speak to an NMR specialist

b) Congratulations, you do indeed have a pure enantiometer
c) Nothing, because the crystallography has no bearing on the chemistry of the molecule
d) Sorry, I think it might be the S enantiomer
e) Sorry, this cannot possibly be pure R ; it must be a mixture of R and S i.e. a racemate

Q 12 A crystalline-to-crystalline phase transformation is most likely to be detected by which ONE of the

following changes in the PXRD pattern?

a) Change in reflection positions and intensities

b) Change in reflection positions only
c) A large change in pattern background
d) Change in reflection intensities only
e) Disappearance of all reflections

Q 13 Which ONE of the following features of a crystal structure affects at what value of 2 in a PXRD
pattern a reflection appears?

a) Atomic positions
b) Crystallite size
c) Amorphous content
d) Unit cell size and shape
e) Atomic vibrations

Q 14 You are approached by a chemist who asks you if it is possible to determine the 3-dimensional
structure of a molecule that he has synthesised. Which of the following is the BEST description of the
advice you should give them?

a) No, you can only get 2-dimensional structural information about molecules
b) Yes – please give me a polycrystalline (i.e. powder) sample for me to analyse using PXRD
c) Yes – go and speak with an expert in solution NMR, who will be able to help you
d) Yes – please attempt to grow a small single crystal and I will be able to give you the 3D structure
you desire
e) Yes – please mill your powder sample to make it amorphous, then I will analyse it using PXRD

Q 15 Which ONE of the following is the correct equation for Bragg’s law?

a)  = d sin
b)  = 2d sin
c)  = d sin2
d)  = 2d sin2
e)  = 2d cos
Q 16 Which ONE of the following fractional atomic coordinates lies exactly in the centre of a unit cell?

a) 0.33, 0.5, 0.5

b) 0.1, 0.2, 0.3
c) 0.5, 0.5 0.5
d) 0.1, 0.1, 0.1
e) 0.5, 0.5, 0.33

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