An excellent paper by R.L. Harlow, detailing many of the issues involved, can be found in J. of Research of the National Institute of Standards and Technology, (1996), 101, 327-339. Troublesome Crystal Structures: Prevention, Detection, and Resolution.
Structural data provided in CIF-format may be validated in terms of consistency, missing relevant data, proper procedure and overlooked problems.
PLATON implements a large variety of such tests specified in check.def
The PLATON validation test set includes many of the official IUCR Validation Procedures in use for the validation of Acta Cryst. papers reporting single crystal structures.
This set is complemented with a more involved analysis of the data themselves with techniques available in PLATON (ADDSYM/VOIDS/Thermal Motion Analysis etc.)
It should be realized that validation has at least three faces:
Refined structures should be routinely checked for these problems prior to submission to a journal.
Common problems include misplaced hydrogen atoms.
This includes a discussion on issues related to pseudo-symmetry, disorder etc.
This includes interesting short intermolecular contacts.
Note: A subset of the the validation checks is applied for CCDC-FDAT structured files.
In all cases, a copy of the file 'check.def' should be present in the current directory.
Alternatively, the path to check.def may be given via the environment variable 'CHECKDEF'.
Example: setenv CHECKDEF /mnt/user/check.def
The results of the validation can be found on the file '<dataname>.chk'
The preparation of a small shell script may be helpful. Below is an example of such a script that can be made available systemwide by placing it in /usr/local/bin
#!/bin/csh
ln -sf /mnt/spea/acc/check.def
platon -u $1.cif
/usr/sbin/unlink check.def
less $1.chk
The validation than runs for CIF sk1000.cif by:
chk sk1000
#=============================================================================== # PLATON/CHECK run versus check.def version of 08/02/00 for entry: I # Data From: e60.cif - Data Type: CIF # CELL 1.54178 16.645 25.768 7.066 90.00 90.00 90.00 3030.70 # SpaceGroup P212121 Rep: P 21 21 21 # MoietyFormula C34 H52 O4 # Reported C34 H52 O4 # SumFormula C34 H52 O4 Rep: C34 H52 O4 # Mr = 524.76[Calc], 524.76[Rep] # Dx,gcm-3 = 1.150[Calc], 1.150[Rep] # Z = 4[Calc], 4[Rep] # Mu (mm-1) = 0.568[Calc], 0.568[Rep] # Reported T limits: Tmin=0.940 Tmax=0.970 '\Y SCAN' # Calculated T limits: Tmin=0.815 Tmin'=0.797 Tmax=0.945 # Reported Hmax= 20, Kmax= 31, Lmax= 8, Nref= 3292 , Th(max)= 70.01 # Calculated Hmax= 20, Kmax= 31, Lmax= 8, Nref= 3291( 5758), Ratio= 1.00( 0.57) # R= 0.0463( 2929), wR2= 0.1367( 3292), S = 1.162, Npar= 347, Flack=-0.40( 4) #=============================================================================== >>> The Following ALERTS were generated <<< 052_ALERT A (proper) absorption correction method missing 702_ALERT A Rep. Angle 174 Dev. from Calcd 110.00 5.00 Sigma 702_ALERT A Rep. Angle 176 Dev. from Calcd 110.00 5.00 Sigma 702_ALERT A Rep. Angle 177 Dev. from Calcd 109.00 5.00 Sigma 702_ALERT A Rep. Angle 183 Dev. from Calcd 109.00 5.00 Sigma #=============================================================================== 222_ALERT B Large Non-Solvent H Ueq(max)/Ueq(min) . 4.02 range #=============================================================================== 032_ALERT C Std Uncertainty in Flack parameter too high .. 0.40 033_ALERT C Flack Parameter value deviates from zero ..... -0.40 057_ALERT C Correction for absorption required RT(exp) = 1.16 089_ALERT C Poor Data / Parameter ratio .................. 9.49 220_ALERT C Large Non-Solvent C Ueq(max)/Ueq(min) . 3.23 range 412_ALERT C Short intra XH3 .. XHn : H(242) .. H(253) = 1.81 Ang. 412_ALERT C Short intra XH3 .. XHn : H(251) .. H(262) = 1.83 Ang. 701_ALERT C Rep. Bond 61 Dev. from Calcd 0.9614 1.43 Sigma 701_ALERT C Rep. Bond 81 Dev. from Calcd 0.9588 1.23 Sigma 702_ALERT C Rep. Angle 167 Dev. from Calcd 109.40 1.03 Sigma ALERT Level Summary 5 ALERT Level A = In General: Serious Problem 1 ALERT Level B = Potentially Serious Problem 10 ALERT Level C = Check & Explain #===============================================================================