Hi,

I get negative beq values when I run refinement of for a sample using LaB6 standard.
Even without the LaB6 are negative values for beq allowed? Should I stop the refinement and fix them to 1?

I am enclosing the cif and data file as well

lle27-lab6-12186-exported.txt

53kB

nb2snc.txt

5kB

lab6-nist.txt

3kB

Here is the code I used -

`'continue_after_convergence 'To continue refinement

'---------------------------- Weighted profile factors, expected R factors, and Goodness of fit values-------------------------------------------------------------------------------
r_p 16.9016764 r_p_dash 29.647421
r_wp 24.798923 r_wp_dash 36.0398251
r_exp 2.59190554 r_exp_dash 3.76676933
gof 9.5678344
weighted_Durbin_Watson 0.987039393 'autocorrelation in the residuals from the statistical regression analysis

'do_errors 'calculates the corelation matrix - last step

Backup_INP

'------------------------[File name & Location]---------------------------------------------------------------------------------------------------------------------------------------

xdd "C:\Users\sunee\OneDrive\Graduate_Studies\Birkel_Group\Processed_DATA\XRD_Analysis\D2_Phaser\LaB6_Refinement\Lin-LIn_D2\LLE27\Added\LLE27_LaB6_12186_exported.raw"

r_exp	2.59190554	r_exp_dash	3.76676933
r_wp	24.798923	r_wp_dash	36.0398251
r_p		16.9016764	r_p_dash	29.647421
weighted_Durbin_Watson	0.987039393	gof	9.5678344
'weighting = 1/Sqrt(Yobs);

start_X  10    'starting 2Th value for data
finish_X  90	'end 2Th value for data
x_calculation_step 0.001 'calculation step size for 2Th
bkg @  614.319855` -315.081606` -130.261592`  80.0577518` -5.41802902` '5 order polynamial background refinement

range 1
LP_Factor ( 0)
Specimen_Displacement ( ,-0.08930)

Rp	141
Rs	141
lam
	ymin_on_ymax	0.0001
	la  0.653817 lo  1.540596 lh  0.501844
	la  0.346183 lo  1.544493 lh  0.626579

'------------------------- [Strcutre_data_from_CIF_LaB6]-----------------------------------------------------------------------------------------------------------------------------------

str
local !CIF_PHASE_ID 1

'spherical_harmonics_hkl sh
'sh_order 4

TCHZ_Peak_Type(, 0.07128,,-0.00396,,-0.00689,, 0,, 0.08839,, 0)
'TCHZ_Peak_Type(@, 0.01,@, 0.01,@, 0.01,, 0,@, 0.01,, 0)


r_bragg	11.4594
phase_MAC	237.338517
phase_name	"LaB6"

MVW( 203.772, 71.827, 32.625`)
space_group 221
scale @  0.00896710325`

'scale_pks = Max (sh, 0); 

Phase_LAC_1_on_cm( 1118.08681)
Phase_Density_g_on_cm3( 4.71094)

Cubic( 4.1568260)
site La1	num_posns  1 x  0.0000 	y  0.000	z  0.000	occ La	1 beq  1
site B1		num_posns  6 x  0.1975	y  =1/2;	z  =1/2;	occ B	1 beq  1

'Out_CIF_STR ("LaB6.cif")

'------------------------------------------[Main_MAX_Phase - Nb2Sn0.6Zn0.4C]--------------------------------------------------------------------------------------------------------------------
str
local !CIF_PHASE_ID 2

'spherical_harmonics_hkl sh
'sh_order 4

'TCHZ_Peak_Type(, 0.01,, 0.01,, 0.01,, 0,, 0.01,, 0)
TCHZ_Peak_Type(@,-0.35594`,@, 0.33300`,@,-0.06891`,, 0,@, 0.36992`,, 0)

r_bragg	5.48051861
phase_MAC	155.845396
phase_name	"Nb2Sn0.6Zn0.4C"

MVW( 590.426, 121.612`, 67.375`)
space_group 194
scale @  0.00377479994`

'scale_pks = Max (sh, 0);

Hexagonal( @  3.167963`, @  13.992207`)


site	Nb	num_posns	4	x	!xNb	=1/3;	y	!yNb	=2/3;	z	zNb	0.58749`	occ	Nb	1	beq	@  1.96027`
site	Sn	num_posns	2	x	!xSN	=1/3;	y	!ySn	=2/3;	z	!zSn	=1/4;	occ Sn !a  0.600 beq b  3.17805` occ Zn =1-a; :  0.40000 beq =b; :  3.17805`
site	C	num_posns	2	x	!xC		0.00	y	!yC		0.00	z	!zC		0.00	occ	C	1	beq	@ -5.37254`

'Out_CIF_STR ("Nb2Sn0.6Zn0.4C.cif") 'creates CIF with all strcutre paramters

'------------------------------------------[Custom_Macros]----------------------------------------------------------------------------------------------------------------------------

'Graphical_Data (40Zn_Graphical_Data.txt)
'Two_Th_Data (2Th_data.txt)
'Editor (40Zn_Editor_Data.txt)

'---------------------------------[END]-----------------------------------------------------------------------------------------------------------------------------------------------`