EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2005src0377

Report generated Apr 01, 2005; 15:23:56

Unit cell

2813 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
c2
a (Angstrom)14.0447 +/- 0.0002
b (Angstrom)7.5861 +/- 0.0002
c (Angstrom)22.3083 +/- 0.0005
alpha (°) 90.000
beta (°)104.4176 +/- 0.0013
gamma (°) 90.000
Volume (A**3)2301.97 +/- 0.09
Mosaicity (°)0.5680 +/- 0.0010

Data collection

Summary

Total number of images collected423
Total exposure time71.3 minutes
Data collection exposure time70.6 minutes
Data collection wall-clock time168.2 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f214214.0° phi1.000°10 secondsYes
data collections02f107107.0° omega1.000°10 secondsYes
data collections03f94 94.0° omega1.000°10 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected 118
Zero sigma or profile test   4
Overload or incomplete profile 536
Sigma cutoff   6
High resolution limit   5

Final Data Set

Scale factor range9.71-10.21
Number of 'full' reflections  4777
Number of 'partial' reflections 12734
Total number of integrated reflections 16665
Total number of unique reflections  2839
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   94.1
Average Sigma(I)    2.2
Overall R-merge (linear)  0.032

Sadabs Results

Parameter refinement on 12788 reflections reduced R(int) from 0.0826 to 0.0319

Before rejection, 17032 reflections total and 2842 unique

After rejection, 16820 reflections total and 2840 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0320   1.047 - 1.243   0.948 - 1.143   1.266    8735    6814
    2   -6.8  0.0329   1.081 - 1.180   0.944 - 1.142   1.243    4324    3339
    3   -6.8  0.0316   0.615 - 0.729   0.949 - 1.100   1.254    3761    2938
Ratio of minimum to maximum apparent transmission: 0.825711

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Lancaster  
  Local Code   DP3-143  
  Formula   C22H8Cl2F10N4Ti  
  Crystal Colour    Black  
  Crystal Habit    Block  
  Crystal Size   0.3 x 0.2 x 0.1 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

SampleCode.zip
      SampleCode.hkl - data corrected using  SADABS
      SampleCode_merge_none.hkl - equivalents and friedels kept separate  (See "Final Data Set" table in this report)
      SampleCode.p4p - skeleton p4p file for use with XPREP
      SampleCode.htm - this summary file


Southampton CIF entry fields

_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    'graphite'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   9.091

_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 

Software References

Unit Cell Determination using DirAx:
Duisenberg AJM. Indexing in Single-Crystal Diffractometry with an Obstinate List of Reflections. Journal of Applied Crystallography 1992; 25: 92-96.
Duisenberg AJM, Hooft RWW, Schreurs AMM, Kroon J. Accurate cells from area-detector images. Journal of Applied Crystallography 2000; 33: 893-898.

Diffractometer control and strategy calculation using COLLECT:
Hooft RWW. COLLECT data collection software, Nonius B.V., 1998.

Standard Data Reduction using HKL(Denzo & Scalepack):
Otwinowski Z, Minor W. Processing of X-ray diffraction data collected in oscillation mode. Macromolecular Crystallography, Pt A. 1997; 276: 307-326.

Absorption Correction
Sheldrick, G. M. (2003). SADABS. Version 2.10. Bruker AXS Inc., Madison, Wisconsin, USA.

Non-Standard Data Reduction using EvalCCD:
Duisenberg AJM, Kroon-Batenburg LMJ, Schreurs AMM. An intensity evaluation method: EVAL-14. Journal of Applied Crystallography 2003; 36: 220-229.

For more information visit the service web site at: http://www.soton.ac.uk/~xservice/