EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2005src0354

Report generated Mar 23, 2005; 08:58:57

Unit cell

4274 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)9.840 +/- 0.003
b (Angstrom)16.132 +/- 0.005
c (Angstrom)17.582 +/- 0.005
alpha (°)67.422 +/- 0.010
beta (°)78.690 +/- 0.017
gamma (°)76.580 +/- 0.017
Volume (A**3)2488.7 +/- 1.3
Mosaicity (°)3.655 +/- 0.008

Data collection

Summary

Total number of images collected351
Total exposure time14.5 hours
Data collection exposure time14.3 hours
Data collection wall-clock time15.5 hours

Experimental Conditions

Wavelength0.71073 A
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 collections03f27 54.0° omega2.000°150 secondsYes
data collections04f28 56.0° omega2.000°150 secondsYes
data collections05f31 62.0° omega2.000°150 secondsYes
data collections06f60120.0° omega2.000°150 secondsYes
Phi/Chii01f - i08f8100 seconds

Scalepack Scaling

Deleted observations

Rejected 354
Zero sigma or profile test5478
Overload or incomplete profile3384
Sigma cutoff2398
Low resolution limit  29
High resolution limit1191

Final Data Set

Scale factor range8.43-10.50
Number of 'full' reflections     0
Number of 'partial' reflections 30282
Total number of integrated reflections 18787
Total number of unique reflections  7424
Data completeness  65.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity    6.5
Average Sigma(I)    2.4
Overall R-merge (linear)  0.155

Sadabs Results

Parameter refinement on 8641 reflections reduced R(int) from 0.1341 to 0.0810

Before rejection, 32221 reflections total and 8937 unique

After rejection, 31008 reflections total and 8899 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.2098   0.928 - 1.165   0.792 - 2.644   1.339   15189    5383
    2  -11.2  0.2517   0.932 - 1.008   0.975 - 1.326   1.293    1486     359
    3  -11.2  0.2476   0.890 - 1.031   0.848 - 1.336   1.309    2871     695
    4  -11.2  0.2499   0.264 - 0.301   0.883 - 1.458   1.329    2526     861
    5  -11.2  0.2282   0.795 - 0.907   0.836 - 1.823   1.313    2833     906
    6  -11.2  0.2579   0.915 - 1.143   0.799 - 1.349   1.362    6103    1647
Ratio of minimum to maximum apparent transmission: 0.299428

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. S. S. Turner  
  Local Code   PM003  
  Formula   C45 H30 N6 S10 Fe1 Zn1  
  Crystal Colour    Red  
  Crystal Habit    Sheet  
  Crystal Size   0.24 x 0.16 x 0.02 (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/