EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src1070

Report generated Aug 06, 2007; 19:49:58

Unit cell

34900 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)8.29070 +/- 0.00010
b (Angstrom)8.95560 +/- 0.00010
c (Angstrom)15.00720 +/- 0.00010
alpha (°)95.4016 +/- 0.0007
beta (°)95.1097 +/- 0.0007
gamma (°)101.3344 +/- 0.0006
Volume (A**3)1081.05 +/- 0.02
Mosaicity (°)0.4830 +/- 0.0010

Data collection

Summary

Total number of images collected731
Total exposure time16.1 minutes
Data collection exposure time15.9 minutes
Data collection wall-clock time48.0 minutes

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 collections01f102102.0° omega1.000°1 secondsYes
data collections02f102102.0° omega1.000°1 secondsYes
data collections03f95 95.0° omega1.000°1 secondsYes
data collections04f67 67.0° omega1.000°1 secondsYes
data collections05f96 96.0° omega1.000°1 secondsYes
data collections06f93 93.0° omega1.000°1 secondsYes
data collections07f68 68.0° omega1.000°1 secondsYes
data collections08f100100.0° omega1.000°1 secondsYes
Phi/Chii01f - i08f81 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Zero sigma or profile test  29
Overload or incomplete profile1174
Sigma cutoff  68
High resolution limit  48

Final Data Set

Scale factor10.00
Number of 'full' reflections  9308
Number of 'partial' reflections 17086
Total number of integrated reflections 25169
Total number of unique reflections  4957
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  830.5
Average Sigma(I)   13.3
Overall R-merge (linear)  0.059

Sadabs Results

Parameter refinement on 23872 reflections reduced R(int) from 0.0474 to 0.0211

Before rejection, 24853 reflections total and 4974 unique

After rejection, 23788 reflections total and 4971 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    2.8  0.0220   0.947 - 1.164   0.969 - 1.048   2.294    3456    3321
    2   10.2  0.0208   0.944 - 1.254   0.971 - 1.048   2.297    3350    3207
    3   10.4  0.0215   0.829 - 1.068   0.975 - 1.034   2.354    3100    2969
    4   10.2  0.0206   0.931 - 1.098   0.975 - 1.047   2.337    2177    2079
    5   10.2  0.0208   0.754 - 0.911   0.975 - 1.048   2.347    3141    3014
    6   10.2  0.0201   0.837 - 1.044   0.973 - 1.048   2.247    3048    2917
    7   10.2  0.0207   0.988 - 1.203   0.969 - 1.048   2.274    2228    2133
    8   10.2  0.0204   0.768 - 1.021   0.971 - 1.048   2.296    3288    3153
Ratio of minimum to maximum apparent transmission: 0.924418

Metadata

  Group    Service  
  Operator   Richard Stephenson  
  Sample Owner   Prof David Davies  
  Local Code   307-MAG-20-1  
  Formula   C3H6Cl9N7OP6  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.1 x 0.1 x 0.1 (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 2007/2 (Sheldrick, G.M., 2007)'

_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 APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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. (2007). SADABS. Version 2007/2. 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/