EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2008lsh060

Report generated Oct 06, 2008; 14:59:48

Unit cell

103490 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p222
a (Angstrom)4.76670 +/- 0.00010
b (Angstrom)18.4984 +/- 0.0004
c (Angstrom)18.6318 +/- 0.0004
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1642.88 +/- 0.06
Mosaicity (°)1.2290 +/- 0.0010

Data collection

Summary

Total number of images collected591
Total exposure time12.4 hours
Data collection exposure time12.3 hours
Data collection wall-clock time13.2 hours

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 collections01f191362.9° phi1.900°76 secondsYes
data collections02f18 34.2° omega1.900°76 secondsYes
data collections03f18 34.2° omega1.900°76 secondsYes
data collections04f58110.2° omega1.900°76 secondsYes
data collections05f24 45.6° omega1.900°76 secondsYes
data collections06f54102.6° omega1.900°76 secondsYes
data collections07f56106.4° omega1.900°76 secondsYes
data collections08f25 47.5° omega1.900°76 secondsYes
data collections09f27 51.3° omega1.900°76 secondsYes
data collections10f58110.2° omega1.900°76 secondsYes
data collections11f54102.6° omega1.900°76 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected 101
Zero sigma or profile test   4
Overload or incomplete profile1944
Sigma cutoff 145
High resolution limit  18

Final Data Set

Scale factor10.00
Number of 'full' reflections 13379
Number of 'partial' reflections 53612
Total number of integrated reflections 57823
Total number of unique reflections  2233
Data completeness  99.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  119.4
Average Sigma(I)    1.6
Overall R-merge (linear)  0.056

Sadabs Results

Estimated minimum and maximum transmission: 0.6434 0.7456

Metadata

  Group      
  Operator   Susanne Huth  
  Sample Owner     
  Local Code     
  Formula   C8 H8 Cl1 N1 O1  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Fragment  
  Crystal Size   0.24 x 0.24 x 0.1 (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/