EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2005src1337

Report generated Nov 03, 2005; 07:52:56

Unit cell

3321 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p2
a (Angstrom)7.5373 +/- 0.0002
b (Angstrom)7.5225 +/- 0.0002
c (Angstrom)24.7617 +/- 0.0007
alpha (°) 90.000
beta (°) 89.909
gamma (°) 90.000
Volume (A**3)1403.97 +/- 0.07
Mosaicity (°)1.071 +/- 0.002

Data collection

Summary

Total number of images collected693
Total exposure time11.5 hours
Data collection exposure time11.5 hours
Data collection wall-clock time12.4 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance50.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f118141.6° omega1.200°60 secondsYes
data collections02f123147.6° omega1.200°60 secondsYes
data collections03f120144.0° omega1.200°60 secondsYes
data collections04f120144.0° omega1.200°60 secondsYes
data collections05f83 99.6° omega1.200°60 secondsYes
data collections06f121145.2° omega1.200°60 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected 153
Zero sigma or profile test   5
Overload or incomplete profile1362
Sigma cutoff  27
High resolution limit   9

Final Data Set

Scale factor range9.76-16.22
Number of 'full' reflections   851
Number of 'partial' reflections 22003
Total number of integrated reflections 20069
Total number of unique reflections  3446
Data completeness  99.3%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  179.5
Average Sigma(I)    4.1
Overall R-merge (linear)  0.042

Sadabs Results

Parameter refinement on 16865 reflections reduced R(int) from 0.1365 to 0.0367

Before rejection, 21942 reflections total and 3463 unique

After rejection, 21583 reflections total and 3461 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -12.1  0.0396   1.124 - 1.590   0.961 - 1.136   1.583    3264    2618
    2  -21.1  0.0396   1.121 - 1.585   0.951 - 1.108   1.440    3967    3123
    3  -21.1  0.0384   0.630 - 0.793   0.951 - 1.082   1.444    3884    3010
    4  -21.1  0.0363   0.561 - 0.850   0.951 - 1.118   1.438    3870    3054
    5  -21.1  0.0403   0.613 - 0.780   0.975 - 1.094   1.412    2682    2086
    6  -21.1  0.0393   0.944 - 1.546   0.952 - 1.137   1.480    3916    3030
Ratio of minimum to maximum apparent transmission: 0.836506

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. S. S. Turner  
  Local Code   PM006  
  Formula   C44 H24 N10 S4 Cu Fe  
  Crystal Colour    Dark Brown  
  Crystal Habit    Needle  
  Crystal Size   0.24 x 0.03 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    '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/