EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

# Summary report for Directory: diska/2006src1117

Report generated Nov 01, 2006; 09:23:41

## Unit cell

4377 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) | 8.1247 +/- 0.0002
b (Angstrom) | 17.1558 +/- 0.0004
c (Angstrom) | 13.9097 +/- 0.0003
alpha (°) | 90.000
beta (°) | 105.9609 +/- 0.0014
gamma (°) | 90.000
Volume (A**3) | 1864.07 +/- 0.08
Mosaicity (°) | 0.4750 +/- 0.0010

## Data collection

### Summary

Total number of images collected | 330
Total exposure time | 12.2 hours
Data collection exposure time | 12.1 hours
Data collection wall-clock time | 12.5 hours

### Experimental Conditions

Wavelength | 0.71073 A
Crystal to detector distance | 40.00 mm

### Scans

Type | Name | # images | Total Rotation | Per frame Rotation | Exposure per frame | Used in scaling
--- | --- | --- | --- | --- | --- | ---
data collection | s01f | 152 | `228.0`° phi | 1.500° | 135 seconds | Yes
data collection | s02f | 87 | `130.5`° omega | 1.500° | 135 seconds | Yes
data collection | s03f | 83 | `124.5`° omega | 1.500° | 135 seconds | Yes
Phi/Chi | i01f - i08f | 8 |  |  | 60 seconds

## Scalepack Scaling

### Deleted observations

Rejected | `217`
Overload or incomplete profile | `440`
Sigma cutoff | `34`
High resolution limit | `7`

### Final Data Set

Scale factor range | 7.00-10.99
Number of 'full' reflections | `13054`
Number of 'partial' reflections | `9805`
Total number of integrated reflections | `22222`
Total number of unique reflections | `4428`
Data completeness | `99.9%`
Resolution range | 7.00-0.77 A
Theta range | 2.91°-27.48°
Average Intensity | `86.0`
Average Sigma(I) | `3.1`
Overall R-merge (linear) | `0.070`

## Sadabs Results

Parameter refinement on 15900 reflections reduced R(int) from 0.1806 to 0.0485

Before rejection, 22297 reflections total and 4434 unique

After rejection, 21950 reflections total and 4434 unique

### Runs

      Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
        1   15.6  0.0544   0.983 - 1.533   0.831 - 1.755   1.397   10128    7627
        2  -15.0  0.0644   0.967 - 1.879   0.846 - 1.710   1.368    6066    4383
        3  -15.0  0.0520   0.470 - 0.572   0.831 - 1.362   1.270    5756    4454

Ratio of minimum to maximum apparent transmission: 0.473539

## Metadata

Group | Service
Operator | Peter Horton
Sample Owner | Dr. A. Kennedy
Local Code | ZnAE1
Formula | C36 H54 N4 S4 Br2 Zn1
Crystal Colour | Colourless
Crystal Habit | Shard
Crystal Size | 0.24 x 0.07 x 0.05 (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/