EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2009src1319

Report generated Feb 02, 2010; 08:07:17

Unit cell

71743 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)10.1895 +/- 0.0010
b (Angstrom)11.4764 +/- 0.0016
c (Angstrom)17.763 +/- 0.003
alpha (°)102.487 +/- 0.005
beta (°)96.931 +/- 0.008
gamma (°)101.360 +/- 0.008
Volume (A**3)1959.1 +/- 0.5
Mosaicity (°)2.285 +/- 0.005

Data collection

Summary

Total number of images collected314
Total exposure time13.0 hours
Data collection exposure time12.8 hours
Data collection wall-clock time13.2 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°150 secondsYes
data collections02f16 32.0° omega2.000°150 secondsYes
data collections03f24 48.0° omega2.000°150 secondsYes
data collections04f24 48.0° omega2.000°150 secondsYes
data collections05f37 74.0° omega2.000°150 secondsYes
data collections06f24 48.0° omega2.000°150 secondsYes
Phi/Chii01f - i08f8100 seconds

Scalepack Scaling

Deleted observations

Rejected  77
Zero sigma or profile test  27
Overload or incomplete profile1964
Sigma cutoff 134
High resolution limit 228

Final Data Set

Scale factor10.00
Number of 'full' reflections     0
Number of 'partial' reflections 35883
Total number of integrated reflections 28116
Total number of unique reflections  8020
Data completeness  89.3%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   18.2
Average Sigma(I)    2.7
Overall R-merge (linear)  0.179

Sadabs Results

Estimated minimum and maximum transmission: 0.4507 0.7455

Metadata

  Group    Service  
  Operator   Graham Tizzard  
  Sample Owner   Dr PJ Holliman  
  Local Code   MI TA-St-CHO  
  Formula   C27H21N1O1  
  Crystal Colour    Yellow  
  Crystal Habit    Block  
  Crystal Size   0.41 x 0.07 x 0.05 (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    'graphite'
_diffrn_measurement_device_type   'Bruker-Nonius Roper 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. (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/