Summary report for Directory: diska/2005slh0248

Report generated Apr 02, 2005; 18:48:36

Unit cell

8008 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) 8.1475 +/- 0.0003

b (Angstrom) 14.0961 +/- 0.0008

c (Angstrom) 16.3605 +/- 0.0009

alpha (°) 90.925 +/- 0.002

beta (°) 99.315 +/- 0.003

gamma (°) 100.887 +/- 0.003

Volume (A**3) 1818.71 +/- 0.16
Mosaicity (°) 0.900 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	8.1475 +/- 0.0003
b (Angstrom)	14.0961 +/- 0.0008
c (Angstrom)	16.3605 +/- 0.0009
alpha (°)	90.925 +/- 0.002
beta (°)	99.315 +/- 0.003
gamma (°)	100.887 +/- 0.003
Volume (A**3)	1818.71 +/- 0.16
Mosaicity (°)	0.900 +/- 0.002

Data collection

Summary

Total number of images collected	301
Total exposure time	199.1 minutes
Data collection exposure time	196.4 minutes
Data collection wall-clock time	220.2 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	181	`362.0`° phi	2.000°	40 seconds	Yes
data collection	s02f	17	`34.0`° omega	2.000°	40 seconds	Yes
data collection	s03f	17	`34.0`° omega	2.000°	40 seconds	Yes
data collection	s04f	55	`110.0`° omega	2.000°	40 seconds	Yes
data collection	s05f	23	`46.0`° omega	2.000°	40 seconds	Yes
Phi/Chi	i01f - i08f	8			20 seconds

Scalepack Scaling

Deleted observations

Rejected	`145`
Zero sigma or profile test	`12`
Overload or incomplete profile	`1200`
Sigma cutoff	`43`
High resolution limit	`95`

Final Data Set

Scale factor range	9.24-12.42
Number of 'full' reflections	`15652`
Number of 'partial' reflections	`23870`
Total number of integrated reflections	`36786`
Total number of unique reflections	`8255`
Data completeness	`99.4%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`12.8`
Average Sigma(I)	`1.1`
Overall R-merge (linear)	`0.090`

Sadabs Results

Parameter refinement on 18903 reflections reduced R(int) from 0.0759 to 0.0507

Before rejection, 37160 reflections total and 8332 unique

After rejection, 36794 reflections total and 8328 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0853   0.768 - 1.026   0.878 - 1.345   1.248   23388   13327
    2   -6.8  0.0907   0.755 - 0.806   0.879 - 1.306   1.255    1917    1108
    3   -6.8  0.0834   0.877 - 0.950   0.872 - 1.285   1.201    1893    1132
    4   -6.8  0.0864   0.943 - 1.036   0.871 - 1.388   1.219    6892    3979
    5   -6.8  0.0911   0.786 - 0.884   0.885 - 1.382   1.232    2704    1496

Ratio of minimum to maximum apparent transmission: 0.627645

Metadata

Group Mike Hursthouse

Operator Susanne Huth

Sample Owner

Local Code CAG 130

Formula C13 H12 N6 I1 Br1

Crystal Colour Orange

Crystal Habit Cut Needle

Crystal Size 0.46 x 0.04 x 0.02 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Susanne Huth
Sample Owner
Local Code	CAG 130
Formula	C13 H12 N6 I1 Br1
Crystal Colour	Orange
Crystal Habit	Cut Needle
Crystal Size	0.46 x 0.04 x 0.02 (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/