EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src1297y

Report generated Oct 03, 2007; 07:38:42

Unit cell

20380 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p2
a (Angstrom)6.9077 +/- 0.0008
b (Angstrom)24.201 +/- 0.003
c (Angstrom)7.7428 +/- 0.0007
alpha (°) 90.000
beta (°)100.062 +/- 0.006
gamma (°) 90.000
Volume (A**3)1274.5 +/- 0.2
Mosaicity (°)1.456 +/- 0.004

Data collection

Summary

Total number of images collected353
Total exposure time13.1 hours
Data collection exposure time13.0 hours
Data collection wall-clock time13.3 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance44.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f168252.0° phi1.500°135 secondsYes
data collections02f17 25.5° omega1.500°135 secondsYes
data collections03f45 67.5° omega1.500°135 secondsYes
data collections04f30 45.0° omega1.500°135 secondsYes
data collections05f27 40.5° omega1.500°135 secondsYes
data collections06f58 87.0° omega1.500°135 secondsYes
Phi/Chii01f - i08f860 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Zero sigma or profile test   6
Overload or incomplete profile 494
Sigma cutoff 490
High resolution limit  79

Final Data Set

Scale factor10.00
Number of 'full' reflections    55
Number of 'partial' reflections 11990
Total number of integrated reflections  7989
Total number of unique reflections  2626
Data completeness  87.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   94.0
Average Sigma(I)    4.9
Overall R-merge (linear)  0.257

Sadabs Results

Parameter refinement on 7042 reflections reduced R(int) from 0.1755 to 0.0596

Before rejection, 11610 reflections total and 2994 unique

After rejection, 9775 reflections total and 2950 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   21.4  0.0749   0.929 - 1.955   0.937 - 1.161   2.113    4989    3092
    2   20.8  0.0581   0.601 - 0.774   0.945 - 1.142   2.101     353     231
    3   20.8  0.0943   0.580 - 0.667   0.937 - 1.145   2.223    1177     570
    4   20.8  0.0530   0.489 - 0.569   0.996 - 1.229   2.023     856     568
    5   18.1  0.0755   1.137 - 1.313   0.953 - 1.073   2.065     701     412
    6   20.8  0.0587   0.513 - 0.617   1.011 - 1.141   1.981    1699    1030
Ratio of minimum to maximum apparent transmission: 0.762255

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Prof. C. Springer  
  Local Code   BS037  
  Formula   C13 H9 N4 O2 F1  
  Crystal Colour    Orange  
  Crystal Habit   Stacked Sheet  
  Crystal Size   0.16 x 0.03 x 0.01 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   75 (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/