EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2005src1629

Report generated Feb 02, 2006; 11:57:35

Unit cell

9819 reflections with 1.00°<theta<27.48° (resolution between 20.40A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)12.6047 +/- 0.0009
b (Angstrom)12.9795 +/- 0.0010
c (Angstrom)16.0115 +/- 0.0012
alpha (°)90.171 +/- 0.003
beta (°)93.401 +/- 0.004
gamma (°)115.307 +/- 0.004
Volume (A**3)2362.8 +/- 0.3
Mosaicity (°)1.808 +/- 0.003

Data collection

Summary

Total number of images collected412
Total exposure time90.2 minutes
Data collection exposure time88.5 minutes
Data collection wall-clock time160.2 minutes

Experimental Conditions

Wavelength0.71073 A

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Detector
distance		Used in
scaling
cell determinationi01f10 10.0° phi1.000°10 seconds45.00 mmNo
data collections01f279362.7° phi1.300°13 seconds30.20 mmYes
data collections02f27 35.1° omega1.300°13 seconds30.20 mmYes
data collections03f27 35.1° omega1.300°13 seconds30.20 mmYes
data collections04f34 44.2° omega1.300°13 seconds30.20 mmYes
data collections05f35 45.5° omega1.300°13 seconds30.20 mmYes

Scalepack Scaling

Deleted observations

Rejected 310
Zero sigma or profile test  27
Overload or incomplete profile2912
Sigma cutoff 142
High resolution limit   6

Final Data Set

Scale factor range9.70-10.98
Number of 'full' reflections     0
Number of 'partial' reflections 45950
Total number of integrated reflections 41715
Total number of unique reflections 10692
Data completeness  97.5%
Resolution range20.40-0.77 A
Theta range1.00°-27.48°
Average Intensity   14.0
Average Sigma(I)    2.1
Overall R-merge (linear)  0.113

Sadabs Results

Parameter refinement on 19546 reflections reduced R(int) from 0.0902 to 0.0599

Before rejection, 42800 reflections total and 10721 unique

After rejection, 42241 reflections total and 10704 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    6.2  0.1198   0.932 - 1.120   0.920 - 1.311   1.246   30352   15615
    2   -5.6  0.1120   0.666 - 0.720   0.904 - 1.122   1.198    2580    1420
    3   -5.6  0.1175   0.904 - 1.009   0.888 - 1.236   1.274    2554    1351
    4   -5.6  0.1055   0.660 - 0.715   0.891 - 1.178   1.226    3330    1839
    5   -5.6  0.1160   0.634 - 0.703   0.888 - 1.249   1.239    3425    1872

Sadabs Results

Parameter refinement on 12294 reflections reduced R(int) from 0.1063 to 0.0795

Before rejection, 28430 reflections total and 7194 unique

After rejection, 28114 reflections total and 7194 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   -6.2  0.1590   0.768 - 1.016   0.907 - 1.387   1.284   20044    9777
    2    5.6  0.1519   0.776 - 0.853   0.907 - 1.225   1.278    1776     891
    3    5.6  0.1554   0.784 - 0.866   0.908 - 1.264   1.311    1902     963
    4    5.6  0.1995   0.737 - 0.875   0.908 - 1.380   1.305    2191     996
    5    5.6  0.1640   0.773 - 0.873   0.908 - 1.275   1.302    2201    1090
Ratio of minimum to maximum apparent transmission: 0.677126

Metadata

  Group    Service  
  Operator   Mike Hursthouse  
  Sample Owner   Butler  
  Local Code   IAN8  
  Formula   C20H18N2Fe1Ni1Br2  
  Crystal Colour    Orange  
  Crystal Habit    Block  
  Crystal Size   0.25 x 0.2 x 0.15 (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/