RE: Preferred orientation and lattice parameters [SEC=UNCLASSIFIED]

[CHEVREAU, Hubert]

Dear  Breogan,

It could also come from the flexibility of the MOF which is really common in 
this class of materials (it can reach 230% in some case). Was the single 
crystal and PXRD measurement performed in the same condition (temperature, 
pressure and same solvent within the pores)? To get a better understanding, you 
can perform PXRD on the solid but in different conditions (ex: as-synthesized, 
dried, and different solvent) or even better a thermo X-ray diffraction.

Regards
Hub

From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On Behalf Of 
Andreas Leineweber
Sent: Thursday, 6 February 2014 5:25 PM
To: Breogan Pato Doldan; rietveld_l@ill.fr
Subject: Re: Preferred orientation and lattice parameters

Dear Breogan,

just three small additions:
(i) .25 Å is a lot, if the lattice parameter in that direction is 4 Å, but much 
less if it is 40 Å
(ii) Definitely, as Peter indicated, partial exchange of guest molecules could 
be responsible for the differences. This could then be indicated by a 
broadening of the peaks .
(iii) If there is a texture as you have described, one could also consider the 
possibility that differently oriented crystals in your specimen have different 
lattice parameters. That is (effectively) the case in the case of residual 
macrostress, but may be also conceivable (as a slightly exotic case) in the 
case composition variations This could be checked by measuring the lattice 
parameters in transmission and reflection geometry.

Best regards
Andreas

On 05.02.2014 20:11, Breogan Pato Doldan wrote:
I would like to thank you both.
It is a small mismatch (about 0.25 A).
Due to the structure of the compound and its porosity it really makes sense 
that the exchange of the guest inside the cavity can affect the lattice.
Regards


De: "Peter Stephens" 

Para: "Breogan Pato Doldan" , 
"rietveld_l@ill.fr" 

Enviados: Miércoles, 5 de Febrero 2014 11:55:59
Asunto: Re: Preferred orientation and lattice parameters

How much mismatch?  If you're getting a good profile fit, I'd be inclined to 
doubt that it is a consequence of preferred orientation.  You could mix your 
sample with another material (corundum powder, cork) to try to reduce the 
degree of preferred orientation, and see if that makes a difference.

Instead of a Le Bail fit, you could try a full Rietveld to see if the powder 
really is the same phase as the single crystal.  One could also imagine that a 
powder would be more facile in exchanging solvent with the environment, which 
could affect lattice parameters.


On Wed, Feb 5, 2014 at 1:37 PM, Breogan Pato Doldan 
mailto:breogan.p...@udc.es>> wrote:

Dear rietvelders,

I have carried out the single crystal resolution and the PXRD Le Bail 
refinement of a Metal Organic Framework.
The compound crystalizes as needles and there is a clear in-plane preferred 
orientation along the c-axis.
There is a mismatch between the single crystal and the Le Bail refinement data 
in the lattice parameter c.
Could this mismatch be due to the preferred orientations?

Regards,
Breogán Pato Doldán,
Fundamental Chemistry Department.
Faculty of Sciences. University of A Coruña
Rúa da Fraga 10, 15008, A Coruña. Spain.
Tel: +34 981167000 ext. 2061




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--

**
Peter W. Stephens
Professor, Department of Physics and Astronomy
Associate Dean for Curriculum, College of Arts and Sciences
Stony Brook University
(631) 632-8156
http://mini.physics.sunysb.edu/~pstephens
Please update your records to my new email: 
peter.steph...@stonybrook.edu





--

Dr. Andreas Leineweber

Max-Planck-Institut fuer Intelligente Systeme

(ehemals Max-Planck-Institut fuer Metallforschung)

Heisenbergstrasse 3

70569 Stuttgart

Germany

Tel. +49 711 689 3365

Fax. +49 711 689 3312

e-mail: a.leinewe...@mf.mpg.de

home page of department: http://www.is.mpg.de/de/mittemeijer


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Re: Preferred orientation and lattice parameters

[Andreas Leineweber]

Dear Breogan,

just three small additions:
(i) .25 Å is a lot, if the lattice parameter in that direction is 4 Å, 
but much less if it is 40 Å
(ii) Definitely, as Peter indicated, partial exchange of guest molecules 
could be responsible for the differences. This could then be indicated 
by a broadening of the peaks .
(iii) If there is a texture as you have described, one could also 
consider the possibility that differently oriented crystals in your 
specimen have different lattice parameters. That is (effectively) the 
case in the case of residual macrostress, but may be also conceivable 
(as a slightly exotic case) in the case composition variations This 
could be checked by measuring the lattice parameters in transmission and 
reflection geometry.


Best regards
Andreas

On 05.02.2014 20:11, Breogan Pato Doldan wrote:

I would like to thank you both.
It is a small mismatch (about 0.25 A).
Due to the structure of the compound and its porosity it really makes 
sense that the exchange of the guest inside the cavity can affect the 
lattice.

Regards


*De: *"Peter Stephens" 
*Para: *"Breogan Pato Doldan" , 
"rietveld_l@ill.fr" 

*Enviados: *Miércoles, 5 de Febrero 2014 11:55:59
*Asunto: *Re: Preferred orientation and lattice parameters

How much mismatch?  If you're getting a good profile fit, I'd be 
inclined to doubt that it is a consequence of preferred orientation. 
 You could mix your sample with another material (corundum powder, 
cork) to try to reduce the degree of preferred orientation, and see if 
that makes a difference.


Instead of a Le Bail fit, you could try a full Rietveld to see if the 
powder really is the same phase as the single crystal.  One could also 
imagine that a powder would be more facile in exchanging solvent with 
the environment, which could affect lattice parameters.



On Wed, Feb 5, 2014 at 1:37 PM, Breogan Pato Doldan 
mailto:breogan.p...@udc.es>> wrote:


Dear rietvelders,

I have carried out the single crystal resolution and the PXRD Le
Bail refinement of a Metal Organic Framework.
The compound crystalizes as needles and there is a clear in-plane
preferred orientation along the c-axis.
There is a mismatch between the single crystal and the Le Bail
refinement data in the lattice parameter c.
Could this mismatch be due to the preferred orientations?

Regards,
Breogán Pato Doldán,
Fundamental Chemistry Department.
Faculty of Sciences. University of A Coruña
Rúa da Fraga 10, 15008, A Coruña. Spain.
Tel: +34 981167000 ext. 2061 




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--

**
Peter W. Stephens
Professor, Department of Physics and Astronomy
Associate Dean for Curriculum, College of Arts and Sciences
Stony Brook University
(631) 632-8156
http://mini.physics.sunysb.edu/~pstephens 

Please update your records to my new email: 
peter.steph...@stonybrook.edu 





--
Dr. Andreas Leineweber
Max-Planck-Institut fuer Intelligente Systeme
(ehemals Max-Planck-Institut fuer Metallforschung)
Heisenbergstrasse 3
70569 Stuttgart
Germany
Tel. +49 711 689 3365
Fax. +49 711 689 3312
e-mail: a.leinewe...@mf.mpg.de
home page of department: http://www.is.mpg.de/de/mittemeijer

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Re: Preferred orientation and lattice parameters

[Łukasz Kruszewski]

Hi! Be careful with LeBail. There is a paper (I can send it to you)
showing, that this method may give some errors (so is probably also for
Pawley method).

Best regards!

Btw: preferred orientation should not influence the c parameter, but the
intensity of an reflection. It can be influenced by sample displacement or
(detector or XRD plane) zero shift, and of course due to impurities.

Try Rietveld.

Good luck!

L. Kruszewski

-- 
Łukasz Kruszewski, Ph.D., adjunct
Polish Academy of Sciences
Institute of Geological Sciences
X-Ray Diffraction Laboratory (coordinator)
Twarda 51/55 str.
00-818 Warsaw
Poland



> Dear rietvelders,
>
> I have carried out the single crystal resolution and the PXRD Le Bail
> refinement of a Metal Organic Framework.
> The compound crystalizes as needles and there is a clear in-plane
> preferred orientation along the c-axis.
> There is a mismatch between the single crystal and the Le Bail refinement
> data in the lattice parameter c.
> Could this mismatch be due to the preferred orientations?
>
> Regards,
> Breogán Pato Doldán,
> Fundamental Chemistry Department.
> Faculty of Sciences. University of A Coruña
> Rúa da Fraga 10, 15008, A Coruña. Spain.
> Tel: +34 981167000 ext. 2061
>
>
>
>





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Re: Preferred orientation and lattice parameters

[Breogan Pato Doldan]

I would like to thank you both. 
It is a small mismatch (about 0.25 A). 
Due to the structure of the compound and its porosity it really makes sense 
that the exchange of the guest inside the cavity can affect the lattice. 
Regards 

- Mensaje original -

De: "Peter Stephens"  
Para: "Breogan Pato Doldan" , "rietveld_l@ill.fr" 
 
Enviados: Miércoles, 5 de Febrero 2014 11:55:59 
Asunto: Re: Preferred orientation and lattice parameters 

How much mismatch? If you're getting a good profile fit, I'd be inclined to 
doubt that it is a consequence of preferred orientation. You could mix your 
sample with another material (corundum powder, cork) to try to reduce the 
degree of preferred orientation, and see if that makes a difference. 

Instead of a Le Bail fit, you could try a full Rietveld to see if the powder 
really is the same phase as the single crystal. One could also imagine that a 
powder would be more facile in exchanging solvent with the environment, which 
could affect lattice parameters. 


On Wed, Feb 5, 2014 at 1:37 PM, Breogan Pato Doldan < breogan.p...@udc.es > 
wrote: 


Dear rietvelders, 

I have carried out the single crystal resolution and the PXRD Le Bail 
refinement of a Metal Organic Framework. 
The compound crystalizes as needles and there is a clear in-plane preferred 
orientation along the c-axis. 
There is a mismatch between the single crystal and the Le Bail refinement data 
in the lattice parameter c. 
Could this mismatch be due to the preferred orientations? 

Regards, 
Breogán Pato Doldán, 
Fundamental Chemistry Department. 
Faculty of Sciences. University of A Coruña 
Rúa da Fraga 10, 15008, A Coruña. Spain. 
Tel: +34 981167000 ext. 2061 




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++ 








-- 

** 
Peter W. Stephens 
Professor, Department of Physics and Astronomy 
Associate Dean for Curriculum, College of Arts and Sciences 
Stony Brook University 
(631) 632-8156 
http://mini.physics.sunysb.edu/~pstephens 
Please update your records to my new email: peter.steph...@stonybrook.edu 

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Re: Preferred orientation and lattice parameters

[Peter Stephens]

How much mismatch?  If you're getting a good profile fit, I'd be inclined
to doubt that it is a consequence of preferred orientation.  You could mix
your sample with another material (corundum powder, cork) to try to reduce
the degree of preferred orientation, and see if that makes a difference.

Instead of a Le Bail fit, you could try a full Rietveld to see if the
powder really is the same phase as the single crystal.  One could also
imagine that a powder would be more facile in exchanging solvent with the
environment, which could affect lattice parameters.


On Wed, Feb 5, 2014 at 1:37 PM, Breogan Pato Doldan wrote:

> Dear rietvelders,
>
> I have carried out the single crystal resolution and the PXRD Le Bail
> refinement of a Metal Organic Framework.
> The compound crystalizes as needles and there is a clear in-plane
> preferred orientation along the c-axis.
> There is a mismatch between the single crystal and the Le Bail refinement
> data in the lattice parameter c.
> Could this mismatch be due to the preferred orientations?
>
> Regards,
> Breogán Pato Doldán,
> Fundamental Chemistry Department.
> Faculty of Sciences. University of A Coruña
> Rúa da Fraga 10, 15008, A Coruña. Spain.
> Tel: +34 981167000 ext. 2061
>
>
>
>
> ++
> Please do NOT attach files to the whole list  >
> Send commands to  eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>
>


-- 

**
Peter W. Stephens
Professor, Department of Physics and Astronomy
Associate Dean for Curriculum, College of Arts and Sciences
Stony Brook University
(631) 632-8156
http://mini.physics.sunysb.edu/~pstephens
Please update your records to my new email: peter.steph...@stonybrook.edu
++
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Preferred orientation and lattice parameters

[Breogan Pato Doldan]

Dear rietvelders,

I have carried out the single crystal resolution and the PXRD Le Bail 
refinement of a Metal Organic Framework.
The compound crystalizes as needles and there is a clear in-plane preferred 
orientation along the c-axis.
There is a mismatch between the single crystal and the Le Bail refinement data 
in the lattice parameter c.
Could this mismatch be due to the preferred orientations?

Regards,
Breogán Pato Doldán, 
Fundamental Chemistry Department. 
Faculty of Sciences. University of A Coruña 
Rúa da Fraga 10, 15008, A Coruña. Spain. 
Tel: +34 981167000 ext. 2061



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