EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/06jec001

Report generated Jan 12, 2006; 20:18:45

Unit cell

4657 reflections with 1.00°<theta<27.48° (resolution between 20.40A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)6.2024 +/- 0.0004
b (Angstrom)11.1908 +/- 0.0007
c (Angstrom)17.9677 +/- 0.0011
alpha (°)78.609 +/- 0.003
beta (°)80.053 +/- 0.004
gamma (°)73.892 +/- 0.004
Volume (A**3)1165.32 +/- 0.13
Mosaicity (°)0.962 +/- 0.004

Data collection

Summary

Total number of images collected352
Total exposure time230.9 minutes
Data collection exposure time229.2 minutes
Data collection wall-clock time5.0 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°10 seconds45.00 mmNo
data collections01f164328.0° phi2.000°40 seconds31.00 mmYes
data collections02f17 34.0° omega2.000°40 seconds31.00 mmYes
data collections03f56112.0° omega2.000°40 seconds31.00 mmYes
data collections04f55110.0° omega2.000°40 seconds31.00 mmYes
data collections05f50100.0° omega2.000°40 seconds31.00 mmYes

Scalepack Scaling

Deleted observations

Rejected 177
Zero sigma or profile test   4
Overload or incomplete profile 554
Sigma cutoff  19
High resolution limit 295

Final Data Set

Scale factor range8.33-21.28
Number of 'full' reflections 10323
Number of 'partial' reflections 17019
Total number of integrated reflections 19063
Total number of unique reflections  5189
Data completeness  97.9%
Resolution range20.40-0.77 A
Theta range1.00°-27.48°
Average Intensity   17.9
Average Sigma(I)    1.4
Overall R-merge (linear)  0.106

Sadabs Results

Parameter refinement on 13702 reflections reduced R(int) from 0.4970 to 0.1002

Before rejection, 27188 reflections total and 3419 unique

After rejection, 20068 reflections total and 3286 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.1629   0.948 - 1.333   0.930 - 1.325   1.463    9910    4591
    2   -7.8  0.1514   0.240 - 0.318   0.899 - 1.198   1.433     852     506
    3   -7.8  0.1627   0.295 - 0.774   0.898 - 1.355   1.479    3208    1620
    4   -7.8  0.1817   1.012 - 1.218   0.903 - 1.297   1.462    3352    1561
    5   -7.8  0.1723   0.767 - 1.180   0.914 - 1.177   1.528    2746    1379
Ratio of minimum to maximum apparent transmission: 0.662511

Metadata

  Group    Martin Grossel  
  Operator   Jonathan Cheeswright  
  Sample Owner     
  Local Code   06jec001  
  Formula   C25 H25 N O4  
  Crystal Colour   Clear Colourless  
  Crystal Habit    Needle  
  Crystal Size   0.7 x 0.16 x 0.16 (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/