EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src0683

Report generated Jul 08, 2009; 13:19:34

Unit cell

28436 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)12.4624 +/- 0.0003
b (Angstrom)4.75500 +/- 0.00010
c (Angstrom)24.7840 +/- 0.0007
alpha (°) 90.000
beta (°) 90.029
gamma (°) 90.000
Volume (A**3)1468.67 +/- 0.06
Mosaicity (°)0.715 +/- 0.002

Data collection

Summary

Total number of images collected468
Total exposure time103.5 minutes
Data collection exposure time102.1 minutes
Data collection wall-clock time120.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance37.40 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f88114.4° omega1.300°13 secondsYes
data collections02f82106.6° omega1.300°13 secondsYes
data collections03f88114.4° omega1.300°13 secondsYes
data collections04f75 97.5° omega1.300°13 secondsYes
data collections05f47 61.1° omega1.300°13 secondsYes
data collections06f80104.0° omega1.300°13 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   4
Zero sigma or profile test  25
Overload or incomplete profile 664
Sigma cutoff 228
High resolution limit  46

Final Data Set

Scale factor10.00
Number of 'full' reflections  6408
Number of 'partial' reflections 15113
Total number of integrated reflections 18821
Total number of unique reflections  3751
Data completeness  99.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   44.6
Average Sigma(I)    1.5
Overall R-merge (linear)  0.237

Sadabs Results

Parameter refinement on 16927 reflections reduced R(int) from 0.1898 to 0.0567

Before rejection, 20445 reflections total and 3782 unique

After rejection, 17754 reflections total and 3771 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    3.3  0.0514   0.771 - 0.946   0.980 - 1.133   2.088    3391    3020
    2   16.4  0.0522   0.605 - 1.262   0.976 - 1.173   1.967    3284    2804
    3   16.4  0.0544   0.786 - 1.441   0.980 - 1.112   2.091    3373    2718
    4   16.4  0.0681   0.544 - 1.030   0.995 - 1.188   2.139    2869    2138
    5   16.4  0.0478   0.822 - 1.056   0.976 - 1.078   2.001    1755    1486
    6   16.4  0.0629   0.738 - 1.330   0.986 - 1.249   2.170    3082    2316
Ratio of minimum to maximum apparent transmission: 0.781152

Metadata

  Group    Service  
  Operator   Graham Tizzard  
  Sample Owner   Dr AK Croft  
  Local Code   GNPO  
  Formula   C14H15N1O7  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.2 x 0.07 x 0.01 (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 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/