EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src1290

Report generated Oct 08, 2007; 15:40:50

Unit cell

11055 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)6.6318 +/- 0.0003
b (Angstrom)9.4254 +/- 0.0004
c (Angstrom)12.0872 +/- 0.0004
alpha (°)112.574 +/- 0.002
beta (°)90.805 +/- 0.002
gamma (°)96.144 +/- 0.002
Volume (A**3)692.39 +/- 0.05
Mosaicity (°)0.635 +/- 0.002

Data collection

Summary

Total number of images collected377
Total exposure time126.3 minutes
Data collection exposure time125.0 minutes
Data collection wall-clock time146.9 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°20 secondsYes
data collections02f13 26.0° omega2.000°20 secondsYes
data collections03f13 26.0° omega2.000°20 secondsYes
data collections04f55110.0° omega2.000°20 secondsYes
data collections05f55110.0° omega2.000°20 secondsYes
data collections06f52104.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Overload or incomplete profile 500
Sigma cutoff 145
High resolution limit  53

Final Data Set

Scale factor10.00
Number of 'full' reflections  7836
Number of 'partial' reflections  6079
Total number of integrated reflections 13089
Total number of unique reflections  3166
Data completeness  99.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   81.7
Average Sigma(I)    2.3
Overall R-merge (linear)  0.113

Sadabs Results

Parameter refinement on 10418 reflections reduced R(int) from 0.0988 to 0.0487

Before rejection, 13113 reflections total and 3206 unique

After rejection, 11780 reflections total and 3196 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0488   0.734 - 1.081   0.965 - 1.166   2.138    5835    4687
    2   14.6  0.0458   0.711 - 0.841   0.972 - 1.099   2.026     360     306
    3   14.6  0.0468   0.669 - 0.789   0.965 - 1.108   2.143     351     278
    4   14.6  0.0491   0.560 - 0.739   0.977 - 1.124   2.133    1781    1393
    5   14.6  0.0542   1.541 - 2.306   0.997 - 1.108   2.178    1779    1364
    6   14.6  0.0494   0.699 - 1.004   0.972 - 1.167   2.191    1674    1302
Ratio of minimum to maximum apparent transmission: 0.827304

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. I. Collins  
  Local Code   LAS-1163-152B  
  Formula   C14 H14 N4 O3 S1  
  Crystal Colour    Light Brown  
  Crystal Habit    Block  
  Crystal Size   0.09 x 0.08 x 0.04 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   75 (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 2007/2 (Sheldrick, G.M., 2007)'

_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    '10cm confocal mirrors'
_diffrn_measurement_device_type   'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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. (2007). SADABS. Version 2007/2. 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/