EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: home/diska/2005src1099

Report generated Sep 07, 2005; 08:00:20

Unit cell

7845 reflections with 2.91°<theta<27.10° (resolution between 7.00A and 0.78A) were used for unit cell refinement

Symmetry used
in scalepack
p1
a (Angstrom)9.9069 +/- 0.0003
b (Angstrom)12.5182 +/- 0.0004
c (Angstrom)15.4400 +/- 0.0004
alpha (°)102.1218 +/- 0.0017
beta (°)94.7642 +/- 0.0015
gamma (°)101.8131 +/- 0.0013
Volume (A**3)1816.51 +/- 0.09
Mosaicity (°)0.8630 +/- 0.0010

Data collection

Summary

Total number of images collected591
Total exposure time12.2 hours
Data collection exposure time12.2 hours
Data collection wall-clock time13.1 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f363363.0° phi1.000°75 secondsYes
data collections02f33 33.0° omega1.000°75 secondsYes
data collections03f34 34.0° omega1.000°75 secondsYes
data collections04f108108.0° omega1.000°75 secondsYes
data collections05f45 45.0° omega1.000°75 secondsYes
Phi/Chii01f - i08f815 seconds

Scalepack Scaling

Deleted observations

Rejected 240
Zero sigma or profile test   2
Overload or incomplete profile1580
Sigma cutoff  55
High resolution limit  77

Final Data Set

Scale factor range4.91-12.54
Number of 'full' reflections  1857
Number of 'partial' reflections 37511
Total number of integrated reflections 37411
Total number of unique reflections  7999
Data completeness  99.6%
Resolution range7.00-0.78 A
Theta range2.91°-27.10°
Average Intensity   37.1
Average Sigma(I)    2.0
Overall R-merge (linear)  0.098

Sadabs Results

Parameter refinement on 24171 reflections reduced R(int) from 0.1157 to 0.0625

Before rejection, 37501 reflections total and 8035 unique

After rejection, 36890 reflections total and 8033 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    6.4  0.0795   0.784 - 1.178   0.935 - 1.243   1.385   22999   16196
    2   -5.8  0.0851   0.743 - 0.850   0.946 - 1.102   1.353    2046    1381
    3   -5.8  0.0694   0.753 - 0.823   0.996 - 1.109   1.303    2040    1459
    4   -5.8  0.0815   0.805 - 1.018   0.930 - 1.149   1.352    7012    4961
    5   -5.8  0.1756   0.726 - 0.951   0.953 - 1.169   1.607    2793    1379
Ratio of minimum to maximum apparent transmission: 0.748466

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Butler  
  Local Code   ADS30  
  Formula   C34H38N2BrPPdFe  
  Crystal Colour    Orange  
  Crystal Habit    Plate  
  Crystal Size   0.08 x 0.03 x 0.01 (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/