[Ifeffit] Regarding a fit for Fe(OTf)2

pushkar shejwalkar pshejwalkar2004 at gmail.com
Tue Dec 2 19:22:37 CST 2014


Dear All,
            I am experiencing problem during my fit for Fe(OTf)2 anhydrous.
The problem is as follows.
I collected the data and used a model to fit. The fitting values and other
technical information is as below. The basic problem is Fe(OTf)2 in
anhydrous condition is probably not cyrstalline because of which there are
no crystal data available. Although .cif file is available for hexahydrate
and tetra acetonitrile. But obviously it is not directly useful as I am
looking for Fe(OTf)2 only. I used hexahydrate for fitting, and the fit
information is given. Is this fit acceptable?

*Now two questions*
1) Why do I not see any scattering or peak for Fe-S. I expected S to be a
strong scatterer and would  show a peak. Under given circumstances it looks
like Fe is all surrounded by water and no triflate is present near Fe at
all. Is this assumption even make sense (when the bottle said anhydrous)
The bottle was not kept under inert condition (and its my fault), but does
it mean Fe(OTf)2 is so hygroscopic and that it can actually form such
hexahydrate to the full extent?
OR there is some inherent problem with my fitting and collection itself. I
used RBKG=1.0

2) Is anybody working on Fe(OTf)2 and had such or any other problem
indicating that Fe(OTf)2 by itself is a bad choice of precursor because of
its reactivity. Also any comments on purification method etc. does anybody
know if crystal structure is available for Fe(OTf)2 anhydrous? I could not
find it on the quick search or on CCDC. Any other site where I can get
crystal data and .cif information?

Thank you very much for all the help, I hope the question is asked
appropriately and all the other information is provided, however, if
anybody needs any other information please let me know.
Thank you in an anticipation
Best
Pushkar


Independent points          : 16.1250000
Number of variables         : 4
Chi-square                  : 7324.9401796
Reduced chi-square          : 604.1187777

R-factor                    : 0.0195782

Measurement uncertainty (k) : 0.0001264
Measurement uncertainty (R) : 0.0004142
Number of data sets         : 1

guess parameters:

  SO                 =   1.06525455    # +/-   0.05504541     [1.00000]
  delE               =  -2.32587026    # +/-   0.59606221     [-2.77870]
  delR               =   0.00911122    # +/-   0.00503027     [-0.02322]
  ss                 =   0.00706809    # +/-   0.00071967     [0.00300]

Correlations between variables:

                delr & dele               -->  0.9154
                  ss & so                 -->  0.9023
All other correlations below 0.4

 name        N       S02     sigma^2   e0     delr     Reff     R
=========================================================================
 O1.1      6.000   1.065   0.00707  -2.326  0.00911  2.09150  2.10061


-- 
Best Regards,
Pushkar Shejwalkar.
Post-doctoral -Researcher,JSPS Fellow
Hokkaido University,
Sapporo,
Japan
[image: Inline image 3]
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