EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src1152

Report generated Nov 02, 2009; 13:49:59

Unit cell

21669 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)8.3907 +/- 0.0005
b (Angstrom)8.7207 +/- 0.0004
c (Angstrom)15.3024 +/- 0.0009
alpha (°)87.410 +/- 0.004
beta (°)75.837 +/- 0.003
gamma (°)62.831 +/- 0.003
Volume (A**3)963.02 +/- 0.10
Mosaicity (°)0.892 +/- 0.003

Data collection

Summary

Total number of images collected355
Total exposure time178.1 minutes
Data collection exposure time175.4 minutes
Data collection wall-clock time190.5 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 collections01f50100.0° omega2.000°30 secondsYes
data collections02f44 88.0° omega2.000°30 secondsYes
data collections03f50100.0° omega2.000°30 secondsYes
data collections04f48 96.0° omega2.000°30 secondsYes
data collections05f50100.0° omega2.000°30 secondsYes
data collections06f23 46.0° omega2.000°30 secondsYes
data collections07f34 68.0° omega2.000°30 secondsYes
data collections08f48 96.0° omega2.000°30 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Zero sigma or profile test   9
Overload or incomplete profile 710
Sigma cutoff 572
Low resolution limit   9
High resolution limit   1

Final Data Set

Scale factor10.00
Number of 'full' reflections  8946
Number of 'partial' reflections 13805
Total number of integrated reflections 20558
Total number of unique reflections  4434
Data completeness  96.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   14.5
Average Sigma(I)    1.1
Overall R-merge (linear)  0.228

Sadabs Results

Parameter refinement on 11698 reflections reduced R(int) from 0.1665 to 0.0825

Before rejection, 20841 reflections total and 4464 unique

After rejection, 17745 reflections total and 4434 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    5.3  0.1042   0.973 - 1.136   0.892 - 1.089   1.992    2651    1536
    2    5.5  0.1154   0.639 - 0.946   0.856 - 1.076   1.973    2288    1225
    3   10.1  0.1374   1.120 - 2.190   0.769 - 1.090   2.146    2590    1194
    4   10.2  0.1084   0.650 - 0.838   0.970 - 1.075   1.984    2446    1329
    5   10.2  0.1322   0.655 - 1.197   0.971 - 1.157   2.058    2565    1295
    6   10.2  0.1388   0.584 - 0.770   0.971 - 1.111   2.044    1095     557
    7   10.2  0.1112   0.419 - 0.484   0.970 - 1.137   1.950    1672     958
    8   10.2  0.1135   0.712 - 0.822   0.907 - 1.071   1.976    2438    1355
Ratio of minimum to maximum apparent transmission: 0.664294

Metadata

  Group    Service  
  Operator   Graham Tizzard  
  Sample Owner   Dr J Spencer  
  Local Code   IRINA  
  Formula   C22H18N4O4  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.14 x 0.1 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/