EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

# Summary report for Directory: diska/2006src1371

Report generated Nov 22, 2006; 17:02:33

## Unit cell

10873 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) | 13.6369 +/- 0.0005
b (Angstrom) | 15.0099 +/- 0.0005
c (Angstrom) | 15.0440 +/- 0.0006
alpha (°) | 89.686 +/- 0.002
beta (°) | 63.7940 +/- 0.0017
gamma (°) | 63.429 +/- 0.002
Volume (A**3) | 2399.19 +/- 0.17
Mosaicity (°) | 1.244 +/- 0.002

## Data collection

### Summary

Total number of images collected | 342
Total exposure time | 158.5 minutes
Data collection exposure time | 157.1 minutes
Data collection wall-clock time | 184.3 minutes

### Experimental Conditions

Wavelength | 0.71073 A
Crystal to detector distance | 31.00 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° | 28 seconds | Yes
data collection | s02f | 17 | `34.0`° omega | 2.000° | 28 seconds | Yes
data collection | s03f | 56 | `112.0`° omega | 2.000° | 28 seconds | Yes
data collection | s04f | 56 | `112.0`° omega | 2.000° | 28 seconds | Yes
data collection | s05f | 24 | `48.0`° omega | 2.000° | 28 seconds | Yes
Phi/Chi | i01f - i08f | 8 |  |  | 10 seconds

## Scalepack Scaling

### Deleted observations

Rejected | `316`
Zero sigma or profile test | `7`
Overload or incomplete profile | `1962`
Sigma cutoff | `265`
High resolution limit | `51`

### Final Data Set

Scale factor range | 9.67-12.34
Number of 'full' reflections | `12921`
Number of 'partial' reflections | `45046`
Total number of integrated reflections | `54854`
Total number of unique reflections | `11059`
Data completeness | `99.7%`
Resolution range | 7.00-0.77 A
Theta range | 2.91°-27.48°
Average Intensity | `30.6`
Average Sigma(I) | `1.8`
Overall R-merge (linear) | `0.081`

## Sadabs Results

Parameter refinement on 30357 reflections reduced R(int) from 0.0974 to 0.0571

Before rejection, 54269 reflections total and 11084 unique

After rejection, 53583 reflections total and 11082 unique

### Runs

      Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
        1    8.3  0.0805   0.844 - 1.149   0.932 - 1.223   1.286   29378   17989
        2   -7.8  0.0808   0.625 - 0.654   0.960 - 1.244   1.241    2435    1464
        3   -7.8  0.0836   0.933 - 1.062   0.927 - 1.240   1.270    9098    5542
        4   -7.8  0.0824   0.726 - 0.824   0.945 - 1.204   1.280    9062    5532
        5   -7.8  0.0816   0.595 - 0.642   0.927 - 1.193   1.323    3610    2207

Ratio of minimum to maximum apparent transmission: 0.745128

## Metadata

Group | Service
Operator | Peter Horton
Sample Owner | Dr. A. Kennedy
Local Code | NiFeH6AE1
Formula | C54 H66 N8 S3 Ni2 Fe1
Crystal Colour | Light Violet
Crystal Habit | Rhombus
Crystal Size | 0.3 x 0.24 x 0.2 (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/