Dear Subin,

many thanks for sharing this interesting technical problem with the RG community. In fact, we never used this software since we are synthetic inorganic chemists. However, over the years I made the experience that it often pays off to check the "Questions" and "Publications" sections of RG to find closely related questions and relevant references about a certain topic. In your case, it will certainly be helpful reading the 10 answers given to the previously asked RG question "What factor decide intensity profile in crystallographic analysis using fullprof software?" Here an RG member asked "I am using fullprof software to analyse peaks profile of sio2. but I am getting intensity profile error check your instr parameter." Just search RG for the original phrase and then click on "Questions".

Good luck with solving your problem!

Hello. First, before that you can do a Rietveld refinement, it is necessary to carry out a search-march analysis with some software with a powder diffraction pattern database, like PDF-4 (https://www.icdd.com/pdf-4/) or Qualx2 (http://www.ba.ic.cnr.it/softwareic/qualx/). Or you could calculate the powder pattern of the phases and superpose with the experimental pattern.

If you do any of these procedures, you will notice that the pattern has several phases. I suspect at least three phases, if not more. I examined the pattern with Qualx2 and found the phases of NiTe2 and Te, plus other peaks of impurities (check the synthesis or other possible products that may have been formed). The rietveld analysis can be complicated for you, also being a newbie running Fullprof.

I recommend doing some examples from the manual or reviewing some videos from the internet. Pay attention to how the files are built for a refinement Le Bail or Rietveld, they have very specific commands that if one is missing it does not work. In the case of several phases, sometimes the program does not minimize well, especially if there is no dominant phase. It seems that you have 2 phases with similar proportions, at first glance. You must proceed with caution, using both phases at the same time.

Subin Kim check the input *.pcr or *.new file. For XY data the flag Ins should be 10. This flag can be found in this line:

!Ipr Ppl Ioc Mat Pcr Ls1 Ls2 Ls3 NLI Prf Ins Rpa Sym Hkl Fou Sho Ana

BTW remove empty lines from the beginning of datafile.

In the first line of your data.dat file you should right "XYDATA".

Then you have to check that in your *.pcr or *.new file there is "10" under the label "Ins" (as also indicated above by L. Gondek)

Dear Subin Kim, first of all, your sample is not a single phase as Analio Dugarte mentioned. So there's no point to do Rietveld refinement without identifying all peaks.

Dear Subin,

many thanks for sharing this interesting technical problem with the RG community. I have also had the same problem and thanks to this community I have managed to solve this problem. In my case, it was about ensuring that it was the X, Y, SIGMA (XYDATA) format. Usually I work in free format (2ThetaI, step, 2ThetaF) for that reason it presented this error. I hope it helps you all.

Dear Renzo Rueda Vellasmín how did you prepare the pcr file for X,Y, Sigma (XYDATA)?!

I got the same problem using Free Format. I'm grateful if you can help!

Dear Ricardo Francisco Alves , you must format the *.dat file. This depends on the state of your data file. If you have the data file in two columns, you can format this in XY format. But, if you have the data file in free format, then you can use the PowDLL Converter software. I hope I've helped you, otherwise you can consult again.

Dear Renzo Rueda Vellasmín , My XRD data file is also a two column file. Could you explain how *.dat file should be prepared from it?

Dear @Swathi Sakthivel you can easily use PowDLL converter software to get your .dat file.