EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/06skc0060

Report generated Oct 06, 2006; 13:02:08

Unit cell

2724 reflections with 1.00°<theta<27.48° (resolution between 20.40A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)6.5398 +/- 0.0002
b (Angstrom)9.4990 +/- 0.0004
c (Angstrom)10.2235 +/- 0.0003
alpha (°)91.506 +/- 0.002
beta (°)91.387 +/- 0.003
gamma (°)107.3456 +/- 0.0018
Volume (A**3)605.67 +/- 0.04
Mosaicity (°)0.500 +/- 0.002

Data collection

Summary

Total number of images collected337
Total exposure time111.9 minutes
Data collection exposure time110.2 minutes
Data collection wall-clock time139.3 minutes

Experimental Conditions

Wavelength0.71073 A

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Detector
distance		Used in
scaling
cell determinationi01f10 10.0° phi1.000°10 seconds45.00 mmNo
data collections01f179358.0° phi2.000°20 seconds31.00 mmYes
data collections02f16 32.0° omega2.000°20 seconds31.00 mmYes
data collections03f56112.0° omega2.000°20 seconds31.00 mmYes
data collections04f24 48.0° omega2.000°20 seconds31.00 mmYes
data collections05f52104.0° omega2.000°20 seconds31.00 mmYes

Scalepack Scaling

Deleted observations

Rejected  60
Zero sigma or profile test   2
Overload or incomplete profile 404
Sigma cutoff  23
High resolution limit   1

Final Data Set

Scale factor range9.73-10.36
Number of 'full' reflections  9019
Number of 'partial' reflections  5082
Total number of integrated reflections 13602
Total number of unique reflections  2791
Data completeness  99.9%
Resolution range20.40-0.77 A
Theta range1.00°-27.48°
Average Intensity   67.0
Average Sigma(I)    2.2
Overall R-merge (linear)  0.037

Sadabs Results

Parameter refinement on 9036 reflections reduced R(int) from 0.0868 to 0.0317

Before rejection, 13403 reflections total and 2789 unique

After rejection, 13267 reflections total and 2786 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0373   0.758 - 0.878   0.951 - 1.118   1.148    7383    5403
    2   -7.8  0.0393   1.486 - 1.563   0.974 - 1.031   1.169     590     447
    3   -7.8  0.0386   1.515 - 1.613   0.967 - 1.071   1.081    2269    1680
    4   -7.8  0.0388   1.483 - 1.559   0.973 - 1.043   1.190     925     676
    5   -7.8  0.0362   0.786 - 0.841   0.954 - 1.079   1.096    2100    1563
Ratio of minimum to maximum apparent transmission: 0.850327

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp11 f8  
  Formula   C9H12O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.39 x 0.28 x 0.21 (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/