EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

# Summary report for Directory: diska/2007src0203

Report generated Feb 27, 2007; 08:54:41

## Unit cell

23814 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) | 10.2222 +/- 0.0002
b (Angstrom) | 12.4363 +/- 0.0003
c (Angstrom) | 19.6192 +/- 0.0005
alpha (°) | 83.7804 +/- 0.0013
beta (°) | 86.1256 +/- 0.0015
gamma (°) | 77.7912 +/- 0.0013
Volume (A**3) | 2420.80 +/- 0.10
Mosaicity (°) | 0.4340 +/- 0.0010

## Data collection

### Summary

Total number of images collected | 340
Total exposure time | 13.0 hours
Data collection exposure time | 12.9 hours
Data collection wall-clock time | 13.5 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 | 181 | `362.0`° phi | 2.000° | 140 seconds | Yes
data collection | s02f | 17 | `34.0`° omega | 2.000° | 140 seconds | Yes
data collection | s03f | 16 | `32.0`° omega | 2.000° | 140 seconds | Yes
data collection | s04f | 28 | `56.0`° omega | 2.000° | 140 seconds | Yes
data collection | s05f | 60 | `120.0`° omega | 2.000° | 140 seconds | Yes
data collection | s06f | 30 | `60.0`° omega | 2.000° | 140 seconds | Yes
Phi/Chi | i01f - i08f | 8 |  |  | 20 seconds

## Scalepack Scaling

### Deleted observations

Rejected | `897`
Zero sigma or profile test | `324`
Overload or incomplete profile | `820`
Sigma cutoff | `230`
High resolution limit | `57`

### Final Data Set

Scale factor range | 6.00-10.28
Number of 'full' reflections | `32991`
Number of 'partial' reflections | `14997`
Total number of integrated reflections | `45027`
Total number of unique reflections | `11064`
Data completeness | `99.9%`
Resolution range | 7.00-0.77 A
Theta range | 2.91°-27.48°
Average Intensity | `33.3`
Average Sigma(I) | `1.8`
Overall R-merge (linear) | `0.068`

## Sadabs Results

Parameter refinement on 29333 reflections reduced R(int) from 0.0978 to 0.0512

Before rejection, 46264 reflections total and 11106 unique

After rejection, 45290 reflections total and 11102 unique

### Runs

      Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
        1   11.8  0.0628   0.871 - 0.944   0.966 - 1.210   1.245   25330   18045
        2   11.2  0.0760   0.909 - 0.972   0.983 - 1.217   1.305    2191    1490
        3   11.2  0.0864   0.721 - 0.784   0.973 - 1.130   1.389    1410     859
        4   11.2  0.0694   0.899 - 0.951   0.977 - 1.240   1.264    3810    2638
        5   11.2  0.0651   0.865 - 0.952   0.966 - 1.274   1.272    8463    5941
        6   11.2  0.0676   0.909 - 0.971   0.966 - 1.322   1.287    4086    2850

Ratio of minimum to maximum apparent transmission: 0.731017

## Metadata

Group | Service
Operator | Louise Male
Sample Owner | Dr Alan Kennedy
Local Code | CuH6AE1
Formula | C36 H57 S3 N5 O3 Cu1
Crystal Colour | Pale Blue
Crystal Habit | Slab
Crystal Size | 0.16 x 0.16 x 0.06 (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 'graphite'
_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/