EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/06skc0058

Report generated Oct 04, 2006; 11:28:25

Unit cell

1767 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)7.5551 +/- 0.0003
b (Angstrom)8.1170 +/- 0.0002
c (Angstrom)10.9179 +/- 0.0004
alpha (°)90.014 +/- 0.002
beta (°)90.0000 +/- 0.0016
gamma (°)68.4345 +/- 0.0018
Volume (A**3)622.67 +/- 0.04
Mosaicity (°)0.365 +/- 0.002

Data collection

Summary

Total number of images collected315
Total exposure time136.7 minutes
Data collection exposure time133.3 minutes
Data collection wall-clock time164.7 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°20 seconds45.00 mmNo
data collections01f-a164328.0° phi2.000°26 seconds31.00 mmNo
data collections01f-b11 22.0° phi2.000°26 seconds31.00 mmNo
data collections02f-a22 44.0° omega2.000°26 seconds31.00 mmNo
data collections02f-b4  8.0° omega2.000°26 seconds31.00 mmNo
data collections03f24 48.0° omega2.000°26 seconds31.00 mmYes
data collections04f56112.0° omega2.000°26 seconds31.00 mmYes
data collections05f24 48.0° omega2.000°26 seconds31.00 mmYes

Scalepack Scaling

Deleted observations

Rejected  57
Overload or incomplete profile 228
Sigma cutoff  12
High resolution limit   9

Final Data Set

Scale factor range9.58-10.24
Number of 'full' reflections  7573
Number of 'partial' reflections  2921
Total number of integrated reflections 10052
Total number of unique reflections  1781
Data completeness  99.9%
Resolution range20.40-0.90 A
Theta range1.00°-23.26°
Average Intensity  127.7
Average Sigma(I)    2.7
Overall R-merge (linear)  0.028

Sadabs Results

Parameter refinement on 7560 reflections reduced R(int) from 0.4602 to 0.0389

Before rejection, 9506 reflections total and 1184 unique

After rejection, 6196 reflections total and 990 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0365   0.952 - 1.050   0.975 - 1.061   1.409    3564    2841
    2   -7.8  0.0343   0.860 - 0.920   0.975 - 1.031   1.266     457     374
    3   -7.8  0.0413   0.860 - 0.962   0.958 - 1.032   1.209     538     442
    4   -7.8  0.0350   0.895 - 0.985   0.954 - 1.030   1.311    1139     902
    5   -7.8  0.0378   0.895 - 0.951   0.969 - 1.043   1.319     498     389
Ratio of minimum to maximum apparent transmission: 0.898625

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp11 g1  
  Formula   C8H18O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.3 x 0.2 x 0.18 (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/