EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2007src0078y

Report generated Feb 08, 2007; 10:50:37

Unit cell

4938 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p2
a (Angstrom)8.5794 +/- 0.0003
b (Angstrom)8.5966 +/- 0.0002
c (Angstrom)11.4708 +/- 0.0003
alpha (°) 90.000
beta (°)98.9569 +/- 0.0017
gamma (°) 90.000
Volume (A**3)835.70 +/- 0.04
Mosaicity (°)0.347 +/- 0.002

Data collection

Summary

Total number of images collected191
Total exposure time63.0 minutes
Data collection exposure time61.7 minutes
Data collection wall-clock time76.8 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 collections01f98196.0° phi2.000°20 secondsYes
data collections02f51102.0° omega2.000°20 secondsYes
data collections03f34 68.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected  56
Zero sigma or profile test   1
Overload or incomplete profile 258
Sigma cutoff  26

Final Data Set

Scale factor range9.83-10.25
Number of 'full' reflections  8444
Number of 'partial' reflections  2887
Total number of integrated reflections 10942
Total number of unique reflections  2039
Data completeness  98.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  128.8
Average Sigma(I)    3.2
Overall R-merge (linear)  0.037

Sadabs Results

Parameter refinement on 8140 reflections reduced R(int) from 0.0566 to 0.0347

Before rejection, 10885 reflections total and 2041 unique

After rejection, 10755 reflections total and 2040 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0363   1.015 - 1.135   0.954 - 1.174   1.275    5753    4519
    2    6.8  0.0373   0.793 - 0.858   0.962 - 1.072   1.242    3020    2350
    3    6.8  0.0365   0.767 - 0.840   0.984 - 1.156   1.263    1982    1550
Ratio of minimum to maximum apparent transmission: 0.812636

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. E. McDonald  
  Local Code   LAS-1037-241  
  Formula   C7 H8 N4 O2  
  Crystal Colour    Light Yellow  
  Crystal Habit    Block  
  Crystal Size   0.36 x 0.22 x 0.15 (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/