QUESTIONNAIRE FOR the
STRUCTURE DETERMINATION BY POWDER DIFFRACTOMETRY ROUND ROBIN - 2



Please answer all questions as completely as possible. Provide
one filled questionnaire for each data (samples 1, 2 and 3).

Forward the results no later than Sunday 24th November 2002 to :
     Lachlan M.D. cranswick
     Collaborative Computational Project No 14 (CCP14) for Single
     Crystal and Powder Diffraction.
by email : L.M.D.cranswick@dl.ac.uk (dl for Daresbury Laboratory).
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.


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 Is the third 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 from the
      chemical formula ? If yes, how and what information ?
      (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):  


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
            anneling, scratch, other) ?

      2.3.2 Which program(s) did you use ?

      2.3.3 If you used molecule location 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...).

   Lachlan has large disk space.