EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/04alb001r

Report generated May 05, 2004; 13:42:03

Unit cell

7504 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) 11.3392 +/- 0.0002
b (Angstrom) 13.3132 +/- 0.0002
c (Angstrom) 13.9507 +/- 0.0002
alpha (°) 110.4269 +/- 0.0007
beta (°) 98.0608 +/- 0.0007
gamma (°) 115.1735 +/- 0.0008
Volume (A**3) 1679.49 +/- 0.05
Mosaicity (°) 0.4880 +/- 0.0010

Data collection

Summary

Total number of images collected 728
Total exposure time 12.1 hours
Data collection exposure time 12.0 hours
Data collection wall-clock time 13.2 hours

Experimental Conditions

Wavelength 0.71073 A
Crystal to detector distance 35.00 mm

Scans

Type Name # images Total
Rotation		 Per frame
Rotation		 Exposure
per frame		 Used in
scaling
data collection s01f 363 363.0° phi 1.000° 60 seconds 2-363
data collection s02f 33  33.0° omega 1.000° 60 seconds 2-33
data collection s03f 33  33.0° omega 1.000° 60 seconds 2-33
data collection s04f 120 120.0° omega 1.000° 60 seconds 2-120
data collection s05f 55  55.0° omega 1.000° 60 seconds 2-55
data collection s06f 116 116.0° omega 1.000° 60 seconds 2-116
Phi/Chi i01f - i08f 8

30 seconds

Scalepack Scaling

Deleted observations

Rejected  140
Zero sigma or profile test    8
Overload or incomplete profile  900
Sigma cutoff    9
High resolution limit   61

Final Data Set

Scale factor range 8.34-10.47
Number of 'full' reflections  12869
Number of 'partial' reflections  23063
Total number of integrated reflections  33859
Total number of unique reflections   7676
Data completeness   99.9%
Resolution range 7.00-0.77 A
Theta range 2.91°-27.48°
Average Intensity    75.1
Average Sigma(I)     2.4
Overall R-merge (linear)   0.036

Metadata

  Supervisor    Mike Hursthouse  
  Operator    Susanne Huth  
  Sample Owner      
  Local Code    CAG30  
  Formula    C30 H16 N4 S6 F4 Cd I2  
  Crystal Colour    Dark Yellow  
  Crystal Habit    Block  
  Crystal Size    0.16 x 0.12 x 0.08 (mm3) 
  Temperature    120(K) 
  Generator    50 (kV)   85 (mA) 
  Primary Solvent    Chloroform  
  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          ' & \w scans'
_diffrn_detector_area_resol_mean   9.091

_computing_data_collection        
'COLLECT (Hooft, 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 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, 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. SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10

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/