EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

# Summary report for Directory: home/diska/2006src0446

Report generated May 19, 2006; 14:37:52

## Unit cell

1933 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used in scalepack | r3
a (Angstrom) | 12.9828 +/- 0.0004
b (Angstrom) | 12.9828 +/- 0.0004
c (Angstrom) | 26.1691 +/- 0.0010
alpha (°) | 90.000
beta (°) | 90.000
gamma (°) | 120.000
Volume (A**3) | 3819.9 +/- 0.2
Mosaicity (°) | 0.533 +/- 0.002

## Data collection

### Summary

Total number of images collected | 121
Total exposure time | 24.4 minutes
Data collection exposure time | 23.0 minutes
Data collection wall-clock time | 31.9 minutes

### Experimental Conditions

Wavelength | 0.71073 A
Crystal to detector distance | 30.00 mm

### Scans

Type | Name | # images | Total Rotation | Per frame Rotation | Exposure per frame | Used in scaling
--- | --- | --- | --- | --- | --- | ---
data collection | s01f | 65 | `130.0`° phi | 2.000° | 12 seconds | Yes
data collection | s02f | 48 | `96.0`° omega | 2.000° | 12 seconds | Yes
Phi/Chi | i01f - i08f | 8 |  |  | 10 seconds

## Scalepack Scaling

### Deleted observations

Rejected | `48`
Zero sigma or profile test | `1`
Overload or incomplete profile | `378`
Sigma cutoff | `6`
High resolution limit | `1`

### Final Data Set

Scale factor range | 7.74-16.17
Number of 'full' reflections | `6605`
Number of 'partial' reflections | `4088`
Total number of integrated reflections | `10333`
Total number of unique reflections | `1943`
Data completeness | `99.8%`
Resolution range | 7.00-0.77 A
Theta range | 2.91°-27.48°
Average Intensity | `132.4`
Average Sigma(I) | `3.2`
Overall R-merge (linear) | `0.045`

## Sadabs Results

Parameter refinement on 6020 reflections reduced R(int) from 0.1409 to 0.0277

Before rejection, 10050 reflections total and 5312 unique

After rejection, 9916 reflections total and 5301 unique

### Runs

      Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
        1    7.4  0.0299   0.594 - 1.098   0.851 - 1.255   1.375    5636    4464
        2   -6.8  0.0306   0.632 - 1.296   0.877 - 1.071   1.297    4280    3454

Ratio of minimum to maximum apparent transmission: 0.677879

## Metadata

Group | Service
Operator | Peter Horton
Sample Owner | Dr. A. Kennedy
Local Code | REGLIG
Formula | C27 H33 N7
Crystal Colour | Colourless
Crystal Habit | Shard
Crystal Size | 0.36 x 0.26 x 0.09 (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 '10cm confocal mirrors'
_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/