Dear Lu Yu,
SHELXL is usually very stable so there must be an error in your .ins
file, but it is difficult fo us to guess what it is without seeing
the full file. A common error that can cause such instability is
caused by a long-standing bug in Coot, which sets some occupancies
in the .ins file to 1.0 (meaning that they can be refined freely
starting at 1.0) rather than the usual 11.0 (which means that they
should be fixed at 1.0; you can add 10 to a parameter to fix it).
Another possibility is that Coot has not understood a 'free
variable' that has been used for e.g. occupancy refinement. The
small molecule people use other graphical GUIs for SHELXL (shelXle,
WinGX, Olex2, System-S, XSEED, Oscail, XSHELL etc.) that make far
fewer mistakes. The .ins files written by Coot should always be
checked carefully and if necessary edited before running SHELXL.
Best wishes, George
On 03/19/2012 05:00 PM, Lu Yu wrote:
[log in to unmask]"
type="cite">Hi all,
I was using SHELXL for the refinement of a small peptide molecule
(6-7 residues), and it was working for the first round. But then
it gave me an error message. I don't know what's going on and have
you had the same problems? Can you give me some suggestions?
For more information:
I was using coot to read in .fcf and .res file, and after model
building, coot can generate an .ins file. I was using this .ins
file and the original .hkl for the next round of SHELXL, except I
added one line "ANIS" in the .ins file:
"DEFS 0.02 0.1 0.01 0.04
CGLS 10 -1
SHEL 10 0.1
FMAP 2
PLAN 200 2.3
LIST 6
WPDB 2
ANIS"
I checked the working .ins and not-working (generated from coot)
.ins files,
1) the working .ins (generated from .res file at the very
beginning) has:
"WGHT 0.100000
SWAT 1.352762 2.1931
FVAR 2.6206 0.5 0.5 0.5 0.5"
2) the not-workind(generated from coot) .ins has:
"WGHT 0.1
FVAR 1.00000"
The refinement is shown as follows:
"Read instructions and data
** Warning: unusual EXTI or SWAT parameter **
** Warning: 8 bad CHIV instructions ignored **
Data: 6342 unique, 0 suppressed R(int) = 0.0000
R(sigma) = 0.0615
Systematic absence violations: 0 Bad equivalents: 0
wR2 = 0.4370 before cycle 1 for 6058 data and 1690 / 1690
parameters
GooF = S = 4.279; Restrained GooF = 5.862 for
2243 restraints
Max. shift = 0.259 A for O_1131b Max. dU =-0.409 for O_1131b
at 06:08:24
wR2 = 0.7365 before cycle 2 for 6058 data and 1690 / 1690
parameters
GooF = S = 12.229; Restrained GooF = 12.221 for
2243 restraints
Max. shift = 0.175 A for O_2131a Max. dU =-0.157 for O_5017
at 06:08:25
** REFINEMENT UNSTABLE **"
The other peptide dataset also has similar problem:
I was using coot-SHELXL, model building - refinement cycle successfully
for the first 3 rounds, but then, it gave me an error
message:
"Read instructions and data
** Warning: unusual EXTI or SWAT parameter **
** Warning: no match for 1 atoms in CONN **
** CANNOT RESOLVE ISOR .. O > LAST **"
I checked the working .ins and not-working .ins files (both
generated from coot this case),
1) the working .ins:
"WGHT 0.100000
SWAT 1.288932 3.0398
FVAR 2.6472 0.5 0.5"
2) the not-working .ins:
"WGHT 0.100000
SWAT 1.344708 3.0452
FVAR 2.731 0.54231 0.5409"
I was really confused, since I was using coot for model building
for other datasets, and the .ins file generated from coot is good
for SHELXL, but it didn't work all the time, eg. it work for the
first few rounds, then there is a problem.
Can you give me some suggestions about what I should do to get
the SHELXL running again?
Thanks,
Lu
--
Prof. George M. Sheldrick FRS
Dept. Structural Chemistry,
University of Goettingen,
Tammannstr. 4,
D37077 Goettingen, Germany
Tel. +49-551-39-3021 or -3068
Fax. +49-551-39-22582