I would like to know the complete structure of ZSM-5 exchanged with transition metal ions (3%). Powder X-ray diffraction or single crystal X-ray diffraction?
first of all which transition metal ion (TMI) have you used? Powder X-ray diffraction is usually used, and I refer you to the article "Zeolite structure determination from X-ray diffraction" by Bennett et al., just as a stating point. There is also a data book of all zeolites structures by X-ray and other techniques, and you can just Google it.
In fact, you can use many other spectroscopic techniques such as EPR, NMR, IR, EXAFS etc. I suggest you to have a look at research papers by Prof. Michael Hunger in University of Stuttgart, who is really an expert in zeolite studies.
if you are really interested in crystal structure of transition metal exchanged zsm-5 zeolite, I may suggest you to have laboratory xrd and then after having the preliminary examination you need to have information about its chemical composition by xrf or icp or aas, . Then for this small concentration of 3% you really need to synchrotron powder xrd data. Then you can use Rietveld refinement to perform structure completion,.use of fourier transform will help you to locate extraframework moieties,
if it is post_synthesis exchange.. How one can grow single crystal.. Use of synchrotron radiation to probe this zeolite is well known in the literature instead of growing single crystal,..