EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2005src0348

Report generated Apr 04, 2005; 14:22:53

Unit cell

5349 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)9.2689 +/- 0.0010
b (Angstrom)11.4640 +/- 0.0011
c (Angstrom)11.5741 +/- 0.0011
alpha (°)90.099 +/- 0.006
beta (°)99.362 +/- 0.005
gamma (°)95.134 +/- 0.006
Volume (A**3)1208.4 +/- 0.2
Mosaicity (°)2.514 +/- 0.004

Data collection

Summary

Total number of images collected574
Total exposure time11.9 hours
Data collection exposure time11.8 hours
Data collection wall-clock time12.8 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance40.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f242363.0° phi1.500°75 secondsYes
data collections02f22 33.0° omega1.500°75 secondsYes
data collections03f42 63.0° omega1.500°75 secondsYes
data collections04f85127.5° omega1.500°75 secondsYes
data collections05f83124.5° omega1.500°75 secondsYes
data collections06f43 64.5° omega1.500°75 secondsYes
data collections07f49 73.5° omega1.500°75 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected 397
Zero sigma or profile test  26
Overload or incomplete profile1494
Sigma cutoff  42
High resolution limit 113

Final Data Set

Scale factor range9.24-10.48
Number of 'full' reflections     0
Number of 'partial' reflections 25420
Total number of integrated reflections 22991
Total number of unique reflections  5506
Data completeness  98.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   31.6
Average Sigma(I)    2.7
Overall R-merge (linear)  0.087

Sadabs Results

Parameter refinement on 14142 reflections reduced R(int) from 0.0989 to 0.0613

Before rejection, 24168 reflections total and 5546 unique

After rejection, 23682 reflections total and 5544 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.6  0.0856   0.948 - 1.183   0.914 - 1.248   1.322   10437    6733
    2  -15.0  0.1130   0.546 - 0.584   0.958 - 1.253   1.342     785     468
    3  -15.0  0.0890   0.645 - 0.707   0.966 - 1.333   1.312    1710    1114
    4  -15.0  0.1010   0.753 - 0.854   0.958 - 1.279   1.411    3556    2238
    5  -15.0  0.0982   0.961 - 1.141   0.966 - 1.532   1.340    3497    2171
    6  -15.0  0.1056   0.961 - 1.066   0.974 - 1.103   1.376    1717     999
    7  -15.0  0.0952   0.718 - 0.801   0.966 - 1.291   1.290    1980    1274
Ratio of minimum to maximum apparent transmission: 0.596670

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. R. Bedford  
  Local Code   rmf 378  
  Formula   C40 H54 P2 Cl3 Fe1  
  Crystal Colour    Light Yellow  
  Crystal Habit    Blade  
  Crystal Size   0.33 x 0.17 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/