EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src0001

Report generated Jan 06, 2009; 11:06:23

Unit cell

17992 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)10.0998 +/- 0.0002
b (Angstrom)10.2807 +/- 0.0002
c (Angstrom)11.7549 +/- 0.0003
alpha (°)100.0672 +/- 0.0015
beta (°)100.4291 +/- 0.0014
gamma (°)103.2160 +/- 0.0016
Volume (A**3)1138.41 +/- 0.05
Mosaicity (°)0.5040 +/- 0.0010

Data collection

Summary

Total number of images collected370
Total exposure time38.7 minutes
Data collection exposure time38.1 minutes
Data collection wall-clock time54.6 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 collections01f51102.0° omega2.000°6 secondsYes
data collections02f44 88.0° omega2.000°6 secondsYes
data collections03f51102.0° omega2.000°6 secondsYes
data collections04f46 92.0° omega2.000°6 secondsYes
data collections05f48 96.0° omega2.000°6 secondsYes
data collections06f23 46.0° omega2.000°6 secondsYes
data collections07f48 96.0° omega2.000°6 secondsYes
data collections08f51102.0° omega2.000°6 secondsYes
Phi/Chii01f - i08f84 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Zero sigma or profile test   7
Overload or incomplete profile 676
Sigma cutoff 198
High resolution limit  83

Final Data Set

Scale factor10.00
Number of 'full' reflections 17651
Number of 'partial' reflections 10236
Total number of integrated reflections 26727
Total number of unique reflections  5203
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   73.1
Average Sigma(I)    1.7
Overall R-merge (linear)  0.159

Sadabs Results

Parameter refinement on 20553 reflections reduced R(int) from 0.0988 to 0.0436

Before rejection, 26018 reflections total and 5246 unique

After rejection, 23230 reflections total and 5234 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    4.3  0.0412   0.818 - 1.007   0.991 - 1.059   2.096    3395    2702
    2    7.5  0.0436   0.704 - 1.117   0.988 - 1.050   2.096    2843    2227
    3   10.2  0.0437   0.997 - 1.274   0.991 - 1.042   2.207    3297    2482
    4   10.2  0.0466   0.786 - 1.007   0.990 - 1.060   2.168    2921    2186
    5   10.2  0.0512   0.690 - 0.999   0.996 - 1.058   2.211    3061    2284
    6   10.2  0.0423   0.664 - 0.803   0.990 - 1.046   2.149    1388    1119
    7   10.2  0.0419   0.698 - 0.873   0.991 - 1.069   2.113    3081    2436
    8   10.2  0.0385   0.599 - 1.065   0.988 - 1.044   2.054    3244    2603
Ratio of minimum to maximum apparent transmission: 0.924455

Metadata

  Group    Service  
  Operator   Sam Callear  
  Sample Owner   Dr J Spencer  
  Local Code   bc29  
  Formula   C22H35BN2O4  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.19 x 0.1 x 0.03 (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/