EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2005src0441

Report generated Apr 08, 2005; 08:55:51

Unit cell

6953 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)9.7069 +/- 0.0006
b (Angstrom)10.6005 +/- 0.0007
c (Angstrom)17.7674 +/- 0.0008
alpha (°)76.268 +/- 0.004
beta (°)74.163 +/- 0.004
gamma (°)62.786 +/- 0.003
Volume (A**3)1550.54 +/- 0.16
Mosaicity (°)1.088 +/- 0.003

Data collection

Summary

Total number of images collected367
Total exposure time15.2 hours
Data collection exposure time15.0 hours
Data collection wall-clock time15.6 hours

Experimental Conditions

Wavelength0.71073 A
Cryostat setting120.00K
Crystal to detector distance35.00 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 collections04f54108.0° omega2.000°150 secondsYes
data collections05f28 56.0° omega2.000°150 secondsYes
data collections06f56112.0° omega2.000°150 secondsYes
Phi/Chii01f - i08f880 seconds

Scalepack Scaling

Deleted observations

Rejected 108
Zero sigma or profile test  11
Overload or incomplete profile1140
Sigma cutoff  56
High resolution limit 168

Final Data Set

Scale factor range6.92-12.03
Number of 'full' reflections 10372
Number of 'partial' reflections 23921
Total number of integrated reflections 32350
Total number of unique reflections  7081
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   34.0
Average Sigma(I)    2.4
Overall R-merge (linear)  0.079

Sadabs Results

Parameter refinement on 14845 reflections reduced R(int) from 0.0769 to 0.0461

Before rejection, 32027 reflections total and 7148 unique

After rejection, 31565 reflections total and 7146 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0742   1.017 - 1.364   0.940 - 1.220   1.341   15999    8570
    2  -11.5  0.0967   0.351 - 0.373   0.968 - 1.255   1.368    1265     616
    3  -11.2  0.0773   0.756 - 0.845   0.940 - 1.258   1.344    1996    1058
    4  -11.2  0.0802   0.778 - 0.855   0.942 - 1.182   1.340    4858    2556
    5  -11.2  0.1307   0.399 - 0.438   0.954 - 1.250   1.453    2393    1014
    6  -11.3  0.0789   1.073 - 1.190   0.954 - 1.077   1.358    5054    2667
Ratio of minimum to maximum apparent transmission: 0.747520

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. A. K. Croft  
  Local Code   AG224-2  
  Formula   C17 H13 N2 O4 Br1  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Blade  
  Crystal Size   0.1 x 0.04 x 0.03 (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    '10cm confocal mirrors'
_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/