QUESTIONNAIRE FOR the
STRUCTURE DETERMINATION BY POWDER DIFFRACTOMETRY ROUND ROBIN - 3
Please answer all questions as completely as possible. Provide
one filled questionnaire for each data (samples 1 and 2).
Preferably, attach the results as one PDF file or as a MS Word
document compressed by Winzip.
It is advised to complete the form as the structure determination
progress.
O.0 Precise date of
- data download : ex : Fri, 1 Feb 2008 10:33:52 -0500
- results submission :
0.1 Is the first sample structure solvable with this quality
of data ? Yes [ ] No [ ]
0.2 Is the second sample structure solvable with this quality
of data ? Yes [ ] No [ ]
0.3 If not, what data would be required ?
Then, for each sample :
1. Preliminary work
1.1 Did you obtained additional informations ?
(for instance from CSD or ICSD or ICDD databases)
1.2 Did you obtained additional informations from the
powder pattern ? If yes, how and what information ?
(for instance using the JCPDS-ICDD database)
1.3 Did you extract the structure factors ? Yes [ ] No [ ]
1.3.1 If yes, which program(s) did you use ?
1.3.2 Give the angular range:
1.3.3 Give the number of extracted structure factors:
1.3.4 Give the Rp and Rwp (conventional Rietveld, background subtracted):
1.3.5 Give the Rp and Rwp (background not subtracted):
1.3.6 If not, did you use the whole pattern ?
1.3.7 Or a partial pattern (if yes, give the angular range):
1.3.8 If you use the whole or a partial pattern, did you keep fixed the
profile parameters, and if yes, how did you obtained them ?
2- Structure solution
2.1 Did you use direct methods ? Yes [ ] No [ ]
2.1.1 If yes, was it on the whole dataset ?
2.1.2 Or on a partial dataset ?
2.1.3 Give the number of reflections:
2.1.4 Which program(s) did you use ?
2.1.5 Did you modified intensities of closely neighbouring
reflections ? If yes, explain how.
2.2 Did you use Patterson methods ? Yes [ ] No [ ]
2.2.1 If yes, was it on the whole dataset ?
2.2.2 Or on a partial dataset ?
2.2.3 Give the number of reflections:
2.2.4 Which program(s) did you use ?
2.2.5 Did you modified intensities of closely neighbouring
reflections ? If yes, explain how.
2.3 Did you use another method ? Yes [ ] No [ ]
2.3.1 If yes, which method(s) (give details : molecule location
by direct space - genetic algorithm, Monte Carlo, Simulated
annealing, scratch, charge flipping, other) ?
2.3.2 Which program(s) did you use (name and reference) ?
2.3.3 If you used direct space methods, how many independent
molecules did you use (give details on these molecules)? How
many degrees of freedom (total) ? How many torsion angles ?
2.4 Did you first locate the whole structure ? Yes [ ] No [ ]
2.4.1 If not, how many atoms did you locate ?
2.4.2 Give their name and initial atomic coordinates
Atom x y z
................................
................................
................................
2.4.3 Were the initial atomic coordinates taken from a known
structure ? Yes [ ] No [ ]
If yes, which one (give reference) ?
3- Structure completion
3.1 Did you performed Fourier difference syntheses before
refining the structure by the Rietveld method ? Yes [ ] No [ ]
3.2 If yes, with what program ?
3.3 If yes, how many additional atoms did you obtained from Fourier
difference syntheses ?
3.4 Give their name and atomic coordinates as they were obtained
Atom x y z
.................................
.................................
.................................
3.5 Did you made first Rietveld refinements without preliminary
Fourier difference syntheses ? Yes [ ] No [ ]
3.5.1 If yes, with what program ?
3.5.2 What were the Rp and Rwp (background subtracted AND not
subtracted) and RB and RF that you obtained at the first
Rietveld application ?
3.5.3 Did you get the structure factors from this result and
performed a Fourier difference synthesis ?
3.5.4 Did you locate additional atoms at this stage ?
3.5.5 And which one ?
Atom x y z
.................................
.................................
.................................
3.5.6 If you repeated Rietveld refinements and Fourier synthese
several times before to complete the model, give the number
of times and which atoms you locate and the Rp, Rwp
RB, RF at each times.
Atom x y z
.................................
.................................
.................................
4- Final refinement
- Give the final atomic coordinates, thermal parameters,
standard deviations, Reliability factors...........
Atom x y z B
...........................................
...........................................
...........................................
- Give details about constraints, restraints
5- Feel free to add any intermediate results (list of extracted structure
factors, software decisive input and output data...) or comments you
might consider as essential (details on hardware, time for solving the
structure, number of moves by Monte Carlo or molecule position trial,
any picture...).