EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/04src1114

Report generated Dec 02, 2004; 16:41:29

Unit cell

9750 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)11.0377 +/- 0.0003
b (Angstrom)13.2554 +/- 0.0004
c (Angstrom)16.9955 +/- 0.0005
alpha (°)110.0120 +/- 0.0012
beta (°)93.8956 +/- 0.0018
gamma (°)109.8851 +/- 0.0017
Volume (A**3)2148.81 +/- 0.11
Mosaicity (°)0.842 +/- 0.002

Data collection

Summary

Total number of images collected358
Total exposure time119.3 minutes
Data collection exposure time117.9 minutes
Data collection wall-clock time146.3 minutes

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°20 secondsYes
data collections02f16 32.0° omega2.000°20 secondsYes
data collections03f16 32.0° omega2.000°20 secondsYes
data collections04f27 54.0° omega2.000°20 secondsYes
data collections05f56112.0° omega2.000°20 secondsYes
data collections06f27 54.0° omega2.000°20 secondsYes
data collections07f27 54.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 244
Zero sigma or profile test   3
Overload or incomplete profile1874
Sigma cutoff  39
High resolution limit  27

Final Data Set

Scale factor range7.10-14.03
Number of 'full' reflections 20002
Number of 'partial' reflections 26303
Total number of integrated reflections 43839
Total number of unique reflections  9860
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   71.2
Average Sigma(I)    2.7
Overall R-merge (linear)  0.058

Sadabs Results

Parameter refinement on 30078 reflections reduced R(int) from 0.1238 to 0.0475

Before rejection, 42754 reflections total and 9880 unique

After rejection, 42164 reflections total and 9876 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0512   0.816 - 1.271   0.925 - 1.119   1.428   22209   16413
    2  -11.2  0.0547   0.715 - 0.826   0.956 - 1.113   1.380    1745    1258
    3  -11.8  0.0557   0.966 - 1.102   0.925 - 1.077   1.446    1731    1276
    4  -11.2  0.0699   0.769 - 0.920   0.925 - 1.082   1.440    3181    2292
    5  -11.2  0.0494   0.743 - 1.308   0.956 - 1.094   1.321    6957    5306
    6  -11.2  0.0672   0.783 - 0.892   0.955 - 1.154   1.473    3173    2250
    7  -11.2  0.0638   0.522 - 0.689   0.971 - 1.081   1.427    3168    2257
Ratio of minimum to maximum apparent transmission: 0.801924

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. C. J. Matthews  
  Local Code   LJD397Mn  
  Formula   C102 H84 N42 O32 Cl8 Mn4  
  Crystal Colour   Light Orange  
  Crystal Habit    Plate  
  Crystal Size   0.42 x 0.16 x 0.04 (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/