EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/06skc0059

Report generated Oct 06, 2006; 07:59:06

Unit cell

1618 reflections with 1.00°<theta<23.26° (resolution between 20.40A and 0.90A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)7.0536 +/- 0.0005
b (Angstrom)8.2164 +/- 0.0004
c (Angstrom)10.0678 +/- 0.0007
alpha (°)75.736 +/- 0.004
beta (°)89.991 +/- 0.003
gamma (°)89.965 +/- 0.003
Volume (A**3)565.49 +/- 0.06
Mosaicity (°)0.680 +/- 0.003

Data collection

Summary

Total number of images collected358
Total exposure time10.8 hours
Data collection exposure time10.7 hours
Data collection wall-clock time11.1 hours

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°40 seconds45.00 mmNo
data collections01f181362.0° phi2.000°110 seconds31.00 mmYes
data collections02f16 32.0° omega2.000°110 seconds31.00 mmYes
data collections03f17 34.0° omega2.000°110 seconds31.00 mmYes
data collections04f24 48.0° omega2.000°110 seconds31.00 mmYes
data collections05f56112.0° omega2.000°110 seconds31.00 mmYes
data collections06f54108.0° omega2.000°110 seconds31.00 mmYes

Scalepack Scaling

Deleted observations

Rejected  51
Overload or incomplete profile 186
Sigma cutoff   8
High resolution limit   3

Final Data Set

Scale factor range9.64-10.48
Number of 'full' reflections  5667
Number of 'partial' reflections  5252
Total number of integrated reflections 10341
Total number of unique reflections  1626
Data completeness  99.2%
Resolution range20.40-0.90 A
Theta range1.00°-23.26°
Average Intensity   31.4
Average Sigma(I)    1.1
Overall R-merge (linear)  0.054

Sadabs Results

Parameter refinement on 7642 reflections reduced R(int) from 0.3814 to 0.0634

Before rejection, 10315 reflections total and 1014 unique

After rejection, 7124 reflections total and 943 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0806   0.840 - 1.008   0.957 - 1.123   1.460    3797    2790
    2   -7.8  0.0891   0.771 - 0.828   0.977 - 1.101   1.482     304     231
    3   -7.8  0.0878   0.849 - 0.895   0.968 - 1.051   1.490     296     214
    4   -7.8  0.0723   0.931 - 0.985   0.977 - 1.116   1.271     471     364
    5   -7.8  0.0743   0.886 - 0.990   0.949 - 1.071   1.460    1100     818
    6   -7.8  0.0789   0.919 - 1.024   0.968 - 1.101   1.427    1156     897
Ratio of minimum to maximum apparent transmission: 0.845532

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp11 f1  
  Formula   C8H10O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.2 x 0.11 x 0.03 (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/