EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2005src1385

Report generated Nov 09, 2005; 15:04:40

Unit cell

8123 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)10.6212 +/- 0.0003
b (Angstrom)11.6024 +/- 0.0003
c (Angstrom)16.3071 +/- 0.0004
alpha (°)69.7781 +/- 0.0012
beta (°)81.3776 +/- 0.0012
gamma (°)73.0822 +/- 0.0014
Volume (A**3)1801.35 +/- 0.08
Mosaicity (°)0.4640 +/- 0.0010

Data collection

Summary

Total number of images collected347
Total exposure time172.1 minutes
Data collection exposure time170.7 minutes
Data collection wall-clock time214.5 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°30 secondsYes
data collections02f16 32.0° omega2.000°30 secondsYes
data collections03f27 54.0° omega2.000°30 secondsYes
data collections04f28 56.0° omega2.000°30 secondsYes
data collections05f60120.0° omega2.000°30 secondsYes
data collections06f27 54.0° omega2.000°30 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 130
Zero sigma or profile test   2
Overload or incomplete profile 766
Sigma cutoff  14
High resolution limit  86

Final Data Set

Scale factor range8.93-10.65
Number of 'full' reflections 24494
Number of 'partial' reflections 12479
Total number of integrated reflections 36034
Total number of unique reflections  8224
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   37.8
Average Sigma(I)    1.7
Overall R-merge (linear)  0.045

Sadabs Results

Parameter refinement on 25447 reflections reduced R(int) from 0.0544 to 0.0366

Before rejection, 35092 reflections total and 8257 unique

After rejection, 34794 reflections total and 8254 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0425   0.934 - 1.123   0.929 - 1.255   1.237   18941   14464
    2  -11.2  0.0385   0.967 - 1.088   0.929 - 1.098   1.210    1473    1185
    3  -11.2  0.0474   0.708 - 0.761   0.978 - 1.099   1.266    2679    2056
    4  -11.2  0.0414   0.775 - 0.821   0.929 - 1.122   1.226    2765    2171
    5  -11.2  0.0418   0.919 - 1.033   0.958 - 1.116   1.231    6260    4944
    6  -11.2  0.0446   0.940 - 0.989   0.967 - 1.251   1.258    2676    2111
Ratio of minimum to maximum apparent transmission: 0.740149

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. I. R. Butler  
  Local Code   IAN 3  
  Formula   C11 H11 N1 O2 Fe1  
  Crystal Colour    Red  
  Crystal Habit   Cut Slab  
  Crystal Size   0.24 x 0.2 x 0.08 (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/