EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

# Summary report for Directory: diska/2008src0851

Report generated Jul 23, 2008; 16:43:31

## Unit cell

19008 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used in scalepack | p222
a (Angstrom) | 7.2251 +/- 0.0004
b (Angstrom) | 21.7492 +/- 0.0018
c (Angstrom) | 38.053 +/- 0.003
alpha (°) | 90.000
beta (°) | 90.000
gamma (°) | 90.000
Volume (A**3) | 5979.6 +/- 0.8
Mosaicity (°) | 0.808 +/- 0.002

## Data collection

### Summary

Total number of images collected | 238
Total exposure time | 5.2 hours
Data collection exposure time | 5.1 hours
Data collection wall-clock time | 6.9 hours

### Experimental Conditions

Wavelength | 0.71073 A
Crystal to detector distance | 50.00 mm

### Scans

Type | Name | # images | Total Rotation | Per frame Rotation | Exposure per frame | Used in scaling
--- | --- | --- | --- | --- | --- | ---
data collection | s01f | 88 | `176.0`° phi | 2.000° | 80 seconds | Yes
data collection | s02f | 37 | `74.0`° omega | 2.000° | 80 seconds | Yes
data collection | s03f | 68 | `136.0`° omega | 2.000° | 80 seconds | Yes
data collection | s04f | 37 | `74.0`° omega | 2.000° | 80 seconds | Yes
Phi/Chi | i01f - i08f | 8 |  |  | 15 seconds

## Scalepack Scaling

### Deleted observations

Rejected | `2`
Zero sigma or profile test | `217`
Overload or incomplete profile | `1132`
Sigma cutoff | `685`
High resolution limit | `113`

### Final Data Set

Scale factor | 10.00
Number of 'full' reflections | `12280`
Number of 'partial' reflections | `13572`
Total number of integrated reflections | `19433`
Total number of unique reflections | `6229`
Data completeness | `81.0%`
Resolution range | 7.00-0.77 A
Theta range | 2.91°-27.48°
Average Intensity | `27.8`
Average Sigma(I) | `2.3`
Overall R-merge (linear) | `0.136`

## Sadabs Results

Parameter refinement on 14608 reflections reduced R(int) from 0.1394 to 0.0648

Before rejection, 24359 reflections total and 6540 unique

After rejection, 20343 reflections total and 6404 unique

### Runs

      Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
        1   24.7  0.0795   0.715 - 0.920   0.949 - 1.146   2.057    7399    4699
        2   23.5  0.1638   0.714 - 0.810   0.855 - 1.196   2.282    3406    1353
        3   17.0  0.0757   0.775 - 1.117   0.963 - 1.110   2.069    7081    4577
        4   24.1  0.0761   0.759 - 1.038   0.858 - 1.145   2.148    2457    1522

Ratio of minimum to maximum apparent transmission: 0.715221

## Metadata

Group | Service
Operator | Simon Coles
Sample Owner | Dr A Kennedy
Local Code | FeH6AB1
Formula | C27H33N4O3Fe
Crystal Colour | Red
Crystal Habit | Needle
Crystal Size | 0.2 x 0.01 x 0.01 (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 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/